Fracture in Steel

FRACTURE
CEik2ACTERISTICS
AND
MEGiANISNfiIN CASTSTEEL
NIGEL HOWARD
CROFT M.A.
f
(Cantab. )
Thesis submitted in fulfilment

of the requirements for the
degree of Doctor of Philosophy,
at the Department of ;Metallurgy,
University of Sheffield.
E cE BER, 1981.
For Joe
(i)-
AND NEQHANIStiS
CHARACTERISTICS
FRACTURE
IN CAST STEEL
Nigel
By
Howard Croft,
M.A.
(Cantab. )
SYNOPSIS
The current
practices
foundry industry
of the UK steel
described and a review has been made of the fracture

in
steel
which
commonly
occur
and mechanisms
has been placed on intergranular
embrittlement
by segregation
effects,
and precipitation
The problem of A1N-induced intergranular

examined using experimental
fracture
Directional
solidified.
into
liquid
The
using various
optical
The plates
the adjacent
at a late
nucleate
austenite
and
of two forms of A1N
form) has been confirmed.
at a later
are precipitated
plates
(I. F. ) has been
work has shown that the dendritic
solidification
forms in the residual
the
material.
and the existence
form and a dendritic
(a plate-like
phenomena caused
0.30C-1.50bh castings with varying
has been studied
techniques
optical
Emphasis
castings.
and in particular
Al and N contents, and commercially-produced
electron
characteristics
has been considered.
role of alinniniwn nitride
mechanism of fracture
have been
A1N
The
stage of solidification.
stage when the casting

at the grain boundaries
grains with an orientation
is fully
and grow
relationship
of the form
(0001)//
The effects
{111}Y
<1010>A1N//
of some processing
have been examined.

a slow cooling
rate.
<110>Y
variables
on the susceptibility
IF is favoured by a high Al and N content

The state
to IF
Tand
found
of heat treatment was also
(ii)
-
to be important,
with quenched and lightly-tempered
more susceptible
to IF.
A model has been proposed which is based
on a comparison of the relative

and intergranular
strength
explain
yield
A programme of mechanical testing

techniques and conditions
quite
effect
(Si).
has shown that different

the severity
of intergranular
on the initiation
are considered.
with
temperature.
testing
of IF observed
decrease
embrittlement,
value of the crack opening
The C.O. D. at maximumload,
is decreased and the implications

practices
This can be used to
behaviour with testing
can influence
in Charpy impact energy as a result
displacement
cleavage strength
Although there maybe a considerable
significantly.
there is little
strength,
of a casting.
in fracture
the variation
samples being
), however,
max
regard to engineering design
CONTENTS
Page
CHAPTER
1
INTRODUCTION
2
CHAPTER
INDUSTRY- CURRENT
THE STEEL FOUNDRY
PRACTICES 6
2.1
Introduction
2.2
Steelmaking
2.2.1
Induction
2.2.2
Electric
2.3
Control
2.3.1
Oxygen
14
2.3.2
Nitrogen
17
2.3.3
Hydrogen
19
2.4
Solidification
2.4.1
Grain Structure
2.4.2
Solute Redistribution
CHAPTER3
Practice,
Arc Practice
11
of Gas Content
12
Behaviour
21
21
During Solidification
22
FRACTURENIECHANISINS
IN CAST STEEL
26
3.1
Introduction
26
3.2
Ductile
Fracture
27
3.3
Brittle
Cleavage Fracture
30
3.3.1
Theoretical
3.3.2
Fractographic
3.4
Brittle
3.4.1
Segregation Effects
Treatments
30
Aspects of Cleavage
Intergranular
Fracture
33
34
38
. =e y
3.4.1.1
Temper Embrittlement
40
3.4.1.2
Hot Tearing
44
3.4.2
Precipitation
3.4.2.1
Aluminium
3".4.2.2
Sulphide Precipitation
Effects
Nitride
Precipitation
47
49
'S1
Page
3.4.2.3
Niobium Carbide Precipitation
53
3.4.2.4
Vanadium Carbide
54
3.4.2.5
Boride and Carboboride Precipitation
54
ALUMINIUM NITRIDE IN CAST STEELS
56
4.1
Introduction
56
4.2
Detection,
CHAPTER4
Precipitation
Observation
of AIN
"
and Indentification
56
4.2.1
Chemical
4.2.2
Metallographic
4.2.3
Other Techniques
4.3
A1N as a Cause of Intergranular
4.3.1
Effect
of Heat Treatment
62
4.3.2
Effect
of Chemical Composition
63
4.4
The Solubility
4.4.1
In Austenite
67
4.4.2
In Liquid
69
4.4.3
Solute Interactions
69
4.5
Precipitation
70
4.5.1
Temperature
of Precipitation
70
4.5.2
Precipitate
Morphology
72
4.6
Other PhenomenaAttributable
Precipitation.
4.6.1
Grain Growth Inhibition
73
4.6.2
Impaired Hot Ductility
74
4.6.2.1
Ingot Panel Cracking
74
4.6.2.2
Surface Break-up During Hot Working
75
CHAPTER5
5.1
Methods of Detection
56
Techniques
58
59
Fracture
of A1N in Steel
67
Steel
of A1N
EXPERIIENTAL WORK
Introduction
60
to ALV
73
76
4
76.
Page
of Experimental
Melts
77
5.2
Production
5.3
Chemical Analysis
79
5.4
Heat Treatment
79
5.5
Mechanical Testing
80
5.5.1
Hardness Measurements
80
5.5.2
Three Point
80
5.5.3
Tensile
5.5.4
Impact Testing
81
5.5.5
Fracture Toughness Testing
83
5.6
Metallographic
Techniques
85
5.6.1
Macroscopic
85
5.6.2
Optical
85
5.6.3
Scanning Electron
5.6.4
Transmission
5.6.5
Electron
5.6.5.1
Specimen Preparation
88
5.6.5.2
Analysis
89
5.7
Directional
5.7.1
Details
5.7.2
The Solidification
5.7.3
Measurement of the Temperature Gradient
91
5.7.4
A Typical
92
5.7.5
Specimen Examination
93
5.8
Industrial
93
CHAPTER6
6.1
Bend Testing
Testing
80
Microscopy
Microscopy
Electron
86
Microscopy
Probe Microanalysis
Solidification
86
88
Technique
of the Specimen Assembly

Apparatus
90
90
91
Procedure
Examinations
94
RESULTS
The Mechanism of AIN-induced
Intergranular
94
Fracture
6.2
AIM Precipitation
6.2.1
Plate-like
AiM
97
9`'
Page
101
6.2.2
Dendritic
AIN
6.2.2.1
Results of the Directional
6.2.2.2
Metallographic
6.3
Effects
6.3.1
Aluminium and Nitrogen
6.3.2
Carbon Content
104
6.3.3
Pouring Temperature
104
6.3.4
Heat Treatment
105
6.4
The Results of Mechanical Testing
107
6.4.1
Tensile
6.4.2
Impact Testing
6.4.2.1
The Effect
6.4.2.2
Effect
6.4.2.3
The Effect
6.4.3
Fracture
Solidification
Work 101
102
Observations
102
of Processing Variables
102
Contents
107
Testing
108
of I. F. on Impact Properties
of Testing
109
Temperature
of Matrix
108
111
Hardness
111
Toughness Testing
DISCUSSION
115
7.1
Introduction
115
7.2
The Mechanism of I. F.
115
7.3
A1N Precipitation
119
7.3.1
Dendritic
120
7.3.2
Plate-like
7.4
The Effect of Processing Variables

Susceptibility
to I. F.
7.4.1
7.4.2
Carbon Content
127
7.4.3
Pouring Temperature and Cooling Rate
128
7.4.4
Heat Treatment
129
7.5
The Effect
7
Q-LAPTER
7.5.1
7.5.2
Tensile
A1N
123
A1N
on the
Contents
of I. F. on Mechanical Properties
Properties
Impact Properties
125
125
131
131
132
Page
134
Toughness
7.5.3
Fracture
7.5.3.1
CODfor Crack Initiation
7.5.3.2
COD at maximum load
7.5.3.3
CHAPTER8
(Si)
134
max)
6u and 6
Commentary on c5 Si,
,
max
135
136
138
CONCLUSIONS
ACKNOWLEDGEMENTS
REFERENCES
Toughness Testing
Al
APPENDIX 1
Fracture
APPENDIX 2
Report
to Foundry
'A'
A6
APPENDIX 3
Report
to Foundry
'B'
A14
APPENDIX 4
The Measurement of 'extinction'

angles in the SEM
APPENDIX 5
Calculation
of the Microsegregation
Characteristics
Solidification
TABLES
FIGURES
of Al and N during
AZO
A22
TEXT
-1-
Chapter
Introduction
The casting
to provide
route continues
economic method of producing

in spite
forming
and fabrication.
Steel
mining
and mineral
power generating
iron
processing,
industry
Complex geometry and difficulties
earth
there is direct
and the
1979).
in hot working often
from a forging
competition
economic grounds casting
on purely
industry.
plant
that some components can only be made by casting,

often
have a
moving equipment,
and steel
(Reynolds,
of metal
engineering
plant,
usually
the more favourable,
quality
of the cast product with
and
components
in particular
castings
used in chemical
versatile
in the fields
in the mechanical
number of applications
They are widely
engineering
certain
developments
of many recent
a uniquely
directly
dictate
but very
Although
route.
to final
shape is
doubt is often expressed about the

regard to internal
integrity
and surface quality.

Reynolds (1979) suggests that
with a correctly
heat-treated
of mechanical properties
carbon and alloy
content
in comparable
wrought
Alloy
compositions
mechanical
cast structure.
Indeed, a wide range
of the steel,
These properties
is
inherently
(Nakajima
materials
but
et al,
it
to cater
of
than
The
1977).
of random defects.
and detection
are available
the
and the heat treatment
tend to be more isotropic
the incidence
requirements,
wrong
can be achieved simply by varying
the casting.
main problem
there is nothing
for
is necessary
most physical
to ensure
that
and
the
-2-
will
castings
imperfections
perform as specified,
during the casting process.
arise
which often
of linear
the techniques
In recent years,
inspection
design
and
as
a
used
increasingly
manufacture of pressure vessels
with greater
confidence,
(Selby,
unimportant
is imperative
ductile-brittle
and the avoidance of overthat
it
the mode of failure

Clearly
under
it would be totally
were to be used at temperatures below the

Equally
transition.
important,
fracture
mechanism at a given temperature,
lowering
of the toughness.
One such problem which is occasionally

low alloy
steel
is often
referred
castings
is usually
in a
fracture
(I. F. ) which
as "Rock Candy" fracture.
for a number of premature failures
and the rejection
foundry as a result
and result
encountered in carbon and
is intergranular
to more pictorially
This has been responsible
however, is the
phenomena which may change the
need to avoid other embrittlement
fracture
in the adoption
can result
to design a component using room temperature
toughness data if
in service
making
castings,
of any discontinuities
this
can be predicted.
conditions
inappropriate
Whilst
1979).
it
specification,
Such
and to ignore any defects which are
design criteria
of more realistic
service
to large steel
to assess the significance
possible
in the
tool
and welded assemblies.
are now being applied
techniques
fracture
elastic
mechanics have been
fracture
mechanics and general yielding
it
having due regard for the
from
large
tonnages
within
of
of cracking
in the mould.
encountered at temperatures
the
Intergranular
ductile
the
above
to
-3(cleavage)
brittle
of the upper shelf
factor
resulting
toughness.
Although there are many
causes, investigations
contributory
in a dramatic reduction
transition,
to be the precipitation
in the past have, shown a major
grain boundaries of the steel.
austenite
can occur around these precipitates,
Preferential
the fracture
as-cast boundaries.
This behaviour
of coarse, shiny facets
on the fracture
(1962) has identified
a plate-like
little
form.
by the presence
surface.
(1960) and Wright and
the presence of two morphologies
on the fracture
of aluminium nitride
the original
is characterised
Previous work by Woodfine and Quarrell

Quarrell
by subsequent heat
appears to follow
still
failure
and even though a new
system of grains may have been established

treatment,
on the prior
Since this
a dendritic
surface,
and
time, however, there has been
fundamental research on the phenomenon, and despite
numerous ad-hoc investigations

intergranular
fracture
of commercial failures,
is still
a cause of serious
concern among
foundrymen.
The aim of this
research is therefore
to adopt a more basic
Approach to the problem by examining the precipitation

in experimentally
this
and commercially
to the fracture
steels,
and relating
A steel
of nominal composition
to intergranular
have shown this

fracture.
0.30%C, 1.500h
(BS 3100 A5/6)

work, since previous
to be particularly
Initially,
melted
mechanisms observed.
has been used as a basis for the experimental

investigations
behaviour
experimental
susceptible
castings were
-4'aluminium and nitrogen
made with varying
to different
subjected
heat treatments
Fracture
hardness levels.
In parallel
this
with
work, examinations were made
which had failed
Subsequent work was aimed at defining
Directional
control
greater
over processing
information
and the
precipitates
out,
and the results
obtained by fracture
way, the practical
parameters.
of T. F. on mechanical properties
the effects
impact tests were carried
the
techniques were used to
solidification
In order to quantify
In this
in an inter-
temperature of the two morphologies
of the precipitation
observed.
more clearly
of the aluminium nitride
crystallography
exert
electron
manner.
granular
details
a range of
from bend specimens were
surfaces
produced castings
of commercially
to obtain
and were
and in the scanning and transmission
examined optically
microscopes.
contents,
compared to
toughness (C. O.D. ) testing.
implications
of intergranular
fracture
could be assessed.
Chapter 2 gives a general outline
use in the UK steel
of the steelmaking
formdry industry
emphasis on the gas content
associated
research in its
to place the current
Chapter 3 is a review of the various

which a steel
current
can fail
theories
discussed briefly,
today with particular

with each.
industrial
fracture
tuendernormal service
of ductile
and brittle
and the conditions
methods in
This is intended
context.
mechanisms by
conditions.
(cleavage)
The
fracture
are
intergranular
which
under
-5fracture
Several particular
can occur are considered.

in more detail.
T. F. are described
The role of aluminium nitride
in causing T. F. is discussed in
Chapter 4 which also gives details

precipitation
causes of
of AIN.
of the solubility
and
Other phenomena which are attributable
to AiM are mentioned.

Chapter 5 describes
current
research,
the experimental
most of which are well
only considered briefly.

mechanical testing
directional
Chapters 6,7
respectively.
techniques
(tensile,
These include
used in the
established
electron
impact and fracture
and are
metallography,
toughness) and
solidification.
and 8 give the results,
discussion
and conclusions,
-6Chapter 2
The Steel Foundry Industry
2.1
Current
Practices
-
Introduction
Before embarking on a review of the scientific
literature
to the fracture
to survey briefly
light
is pertinent
that the ideal
solution
in the UK.
castings
research in context,
place the current
some of the technological
dictate
it
methods employed to produce steel
the various
This will
of cast steel,
relevant
high-
and will
and economic limitations
which often
problem cannot be
to a scientific
implemented in practice.
The business of the steel
carbon, low alloy
plain
areas of application
are available
foundry industry
and high alloy
is the production
steel
which are suited
General
castings.
are shown in Fig . 2.1.
of
Casting processes
to the production
of virtually
any
size component from a few grams to over two hundred tonnes,
and in
any quantity,
from a "one-off"
In 1978, British
of castings
foundries
to many millions.
produced approximately
worth over 225m before finish
employed over 20,000 people.
250,000 tonnes
machining,
This compares with
and
a total
production
of 13M tonnes p. a.,
7M tonnes,
the USA 1.6M tonnes and Japan 0.6M tonnes.
world
of which the USSRproduces almost

(Jackson,
1979).
2.2
Steelmaking
In the UK, liquid

electric
steel
for making castings
arc and induction
AOD are currently
furnaces,
being introduced
is melted mainly by
although
for special
techniques
such as
applications.
-7-
foundries
Figures for 1977 (Jackson, 1979) show that in British

369,500 tonnes of liquid
109,500 tonnes by induction
route,
by other techniques
this
steel were produced by the arc furnace

furnaces and 20,500 tonnes
(mainly cupolas and convertors).
by
75%
that
almost
weight of all
means
furnace
arc
practice,
using
made
it
the use of electric
arc steelmaking
induction
practice,
since the latter
producing
small quantities.
UK furnace useage for 1978.
castings
produced are
should not be concluded that

is more widespread than
is used extensively
This is highlighted
for
by a summary of
(Table 2.1).
Number of furnaces of different

in use.
Table 2.1
Although
capacities
currently
Arc furnaces
<St
61
Induction
In addition,
These figures
It
10-20t
20-30t
20
15
43
TOTAL
>30t
103
furnaces
<O.5t
67
but will
5-10t
0.5-1t
96
1-2t
26
13 converter-type
209
furnaces were also in operation.
have remained fairly
be
doubt
affected
no
TOTAL
>2t
20
constant
for the last
by recent closures
few years,
in the industry.
is apparent from these data that not every foundry will
for
to
castings
orders
accept
equipped
of all
furnaces
there
seven
are
only
example,
in operation
having a capacity
of 20 tonnes or more.
30 tonne casting would therefore
weights.
be
For
in the UK
A customer requiring
be limited
in his choice of
-8but it
foundry,
to
a
approach
by utilising
can produce large castings
Practice
Induction
Despite the relatively

the induction
route,
the combined melting
furnaces.
of a number of smaller
capacity
2.2.1
should be emphasised that most foundries
foundry industry,
produced by this
small tonnages of steel
furnace is widely used throughout
and there are currently
the
more than twice as
furnaces as arc furnaces in operation.
many induction
Induction
furnaces are less expensive than arc furnaces to buy and install,
and their
smaller
(usually
sizes
suited
for service
regular
intervals.
where casting
all
furnace bodies,
switched into
the lining
is to occur at short,
One large advantage is that

it
for a foundry
to have
each one reserved for specific
steels,
steels,
one generator.
This avoids contamination
in successive melts and obviates
This is particularly
furnace is normally
most of the alloys
being retained
in the final
melt.
the furnace charge is therefore

alloy
important,
since the induction
contained
Careful
unit,
in the initial
selection
with
charge
of scrap for
to avoid exceeding the
crucial,
specifications.
For example, in a series
of experiments
Hubbard (1975) a small induction
meant that
the nitrogen
0.010$ in the initial
reported
by Holt and
furnace was used to remelt the
same charge three times in succession.

boil
elements from
considered to be a dead melting

or impurities
from
the need to make a
"wash heat" to remove traces of unwanted alloying

the furnace.
but
is possible
producing many grades of alloy

several
less than 2 tonnes) are ideally
The absence of a carbon
content of the steel
charge material
increased from
to 0.017% after
the third
-9-
This resulted
remelting.
in porosity
in the finished
one of the many problems which may be encountered
which highlights
by the continuous
of internal
recycling
foundry scrap with
induction
furnace practice.
Induction
furnaces may be used with either
basic
(MgO) lining,
is its
associated
The main advantage of a silica
low cost, which for a comparable life
that of a basic lining.

necessity
an acid (Si02) or
having its
each practice
disadvantages.
and
advantages
lining
that basic induction
is about half
However, other considerations
to use scrap low in sulphur

steelmaking
is more commonin the UK.
practice
the charge for a basic furnace,
shot blasted
to remove any adherent sand, which will

the furnace lining.
form a slag and attack

however, sand is left
siliceous
intact
Some foundries
actually
known to add a quantity
oxidised
or sand-free
induction
the scrap is usually

otherwise
In acid practice,
will
react with
in the charge and lessen the attack
lining.
once a'molten
it
so that
such as the
and phosphorus have meant
In preparing
oxide present
casting,
any iron
of the
employing an acid practice
of sand to the charge when highly
scrap is used.
heel has forced in the bottom of the furnace,
furnace becomes an ideal
of scrap such as swarf.
unit
This is carried
for melting
atmosphere where oxidation
can occur.
compared to other air melting

practice,
furnaces.
the
small pieces
out almost immediately
is
the
there
the
surface
melt
of
and
no preheating
under
In dead melting
are
This results
in the
in high yields
(Hubbard, 1972).
the scrap is charged into
the furnace
10
together
the other non-oxidisable
with all
have
these
melted out,
when
bring
into
the steel
Final
additions
and tapped as quickly
are made to
as possible.
is carried
with aluminium)
out either
or both.
in the ladle,
for some reason the melt has to be held at elevated
for any length of time,
the gas content of the steel
rapidly
a molten heel for efficient
has to retain
To overcome this
tapping one cast,
furnace normally
there
power utilisation,
problem, the temperature
is kept as low as possible
increase
to occur during each successive
is a tendency for gas pick-up

tapping.
temperature
will
because
the induction
and
(see Section 2.3),
and
additions,
The melt is then superheated
specification.
(usually
deoxidation
in the furnace,
If
the oxidisable
temperature
to the required
alloying
at all
times,
of the melt
and immediately
after
the cold charge for the next melt is added to
the furnace.
Although it
has so far been assured that
a dead melting
Hubbard (1971) report

carbon boil
melt.
is not entirely
this
unit,
that
it
by the addition
is possible
correct.
furnace is
Holt and
to promote a controlled
of small quantities
of ore to the
This is advantageous in that the scrap in the base charge
does not need to be so carefully

and silicon
flush
the induction
selected,
removal can now be achieved.
since carbon, manganese

The boil
also serves to
out unwanted gases, and promotes much lower nitrogen

(Fig.
hydrogen levels.
2.2).
Hubbard (1972) does not consider

to be a feasible
proposition
there have recently
and
the use of vacuum induction
for general foundry melting,
been introduced
several
furnaces
but
designs
furnace
new
11
for
operation
allow
which
has been reviewed by Holt,
of steel
the composition
thereby obviating
castings
production
Hubbard and Jackson (1973).
far
as the steelmaker
as
main advantage
slags,
arc furnace is
of the modem electric
documented, and in the context
to refine
lowering
Arc Practice
Electric
The design and operation

well
further
However, these are not in widespread use.
the gas content.

2.2.2
under reduced pressure,
of the liquid
The
is concerned is the ability

metal by using appropriate
the need for stringent
selection
of
charge materials.
The most versatile
unit
furnace which, with

or reducing),
scrap and still

composition.
the use of suitably
makes it
to very low levels.
is the basic lined
available
Hence the steelmaker
is the necessity
has
restricted
which
although acid lined
low phosphorus,
composed slags
with
the required
furnaces are widely
runners),
scrap (turnings,
etc).,
to add some form of recarburiser

crushed electrodes
high carbon content
boil
to proceed.
in Britain,
used in the USA, where
charges are more readily
and in some cases, ore.
chemical
to remove phosphorus and sulphur
The charge to the arc furnace is normally

mix of light
(oxidising
can use poor quality
the use of an acid practice
low sulphur
arc
to remove phosphorus and sulphur
possible
produce a casting
It
electric
available.
made up from a suitable
heavy scrap (feeder heads,

Prior
to charging,
such as anthracite,
it
is usual
coke or
to the furnace bottom to ensure a sufficiently

at melt-out.
This allows an adequate carbon
12
It has long been recognised
is generally
and it
steel,
(Holt,
dissolved
two schools of thought as to when the boil
of about 0.10%, and then recarburise

to "catch"
prefer
to be exercised
The first
to problems due to overoxidation
The recent introduction
control
but can give rise
(see Section 2.3.1).

but results
controlled,
techniques
for analysing
(the
"checkpoint"
the
content
of
melt
carbon
type liquidus
apparatus)
arrest
"catch-carbon"
2.3
of rapid
has resulted
the fact
state
effects
that
casting.
the high solubility

with
at the liquidus.
be rejected
for the
and structural
This is a consequence of
of many gases in the liquid
decreasing
temperature,
Any gases present
during solidification,
measures are taken, will

For this
the
can have extremely
steel
on the mechanical properties
decreases steadily
therefore
gases in liquid
of the solidified
very sharply
easier.
of Gas Content
The presence of dissolved
integrity
popularity
in more
technique.
Control
deleterious
in greater
Others
required
making subsequent deoxidation
oxygen contents,
predictable
little
period,
of the-bath
is less easily
level.
below the level
method requires
over the decarburisation
The second technique
should be terminated.
to the required
or just
the carbon at,
by the specification.
gases to acceptable
the bath to give a carbon content
to oxidise
prefer
content of
There are, however,
Stephenson and Jackson, 1971).
Some foundries
is the
a carbon drop of 0.30%
agreed that
to remove these harmful
is sufficient
levels
the hydrogen and nitrogen
in controlling
factor
prime
carbon boil
that a vigorous
give rise
in the melt will
and unless preventative
to porosity
reason, numerous investigations
and drops
in the casting.
have been carried
out
13
-
the control
over many years regarding
of the gases
and effects
during
steelmaking.
encountered
commonly
Jackson (1975) found it
convenient
The monatomic (inert)
ii)
The elemental
iv)
gases.
(e.
g. 02, N2, H2).
gases
diatomic
gases (e. g. CO).
The compound diatomic
iii)
The triatomic
Of these,
gases.
the most crucial
with regard to steelmaking
gases, and in particular
diatomic
the more important
four groups:
gases into
i)
to divide
insolubility
temperatures
at all
since their
out undesirable
example of this
is the ladle
1965).
degassing of steel
hydrogen
the
and nitrogen
can
reduce
which
The solution
by Sievert
by its
stirring
of diatomic
have to dissociate
using argon,
contents quite
effect.
gases in liquid
(1929), who took into
A typical
homogeneity of temperature
and also promote greater
and composition
virtual
allows them to be used to flush
(Fast,
from
the
melt
gases
significantly,
and hydrogen.
oxygen, nitrogen
The monatomic gases are, however, useful
are the
steel
was first
account the fact
before they can dissolve
that
proposed
such gases
in the melt to form
monatomic solutions.
For the reaction
G2
2G (metal)
2
K=[CC-G]
where
[G3
K is the equilibriin
is the activity
CG2] is the activity
constant
in
the melt.
atoms
of gas
diatomic
the
of
gas above the melt.
14
Assuming ideal
C11
G3
K'
then
directly:
law follows
Sievert's
and that Henry's law holds,
gas behaviour,
where PGZ is
PG,.
the partial
of gas
pressure
above the melt.

Because of this
remove completely
vacuum steelmaking
facilities
foundry industry,
dissolved
gas will
are not widely
always be present
be evolved during solidification.
elements which will

inclusions,
2.3.1
in the
steel,
and will
the aim of the
of blowholes or porosity
by the addition
in the
of alloying
any excess gas to produce solid
combine with
in a suitably
such as oxides or nitrides,
innocuous form.
Oxygen
oxygen plays a very important

and can influence
steel,
is
vital
carbon
oxygen and
a positive
disadvantage
and the evolution
manifest
as blowholes
or semi-killed
Although
during
the reaction
the steelmaking
between
it
process,
is
of steel
of carbon monoxide gas is often
in the finished
are always fully

steels
of the cast product quite
during the solidification
castings
castings
during the manufacture of
role
the quality
(Jackson, 1975).
significantly
steel
in the liquid
Clearly,
This is best effected
casting.
available
that
the presence of any such gases does
in the formation
not result
2.2.1)
has to be accepted that some
and so it
foundryman is to ensure that
to
during
gases such as oxygen and nitrogen
It has already been noted (Section
steelmaking.
steel
is extremely difficult
it
square root relation,
killed
product.
For this
reason,
before pouring, and rimming
are never produced.
Although Carney C1953) has shown oxygen to have quite
high
15
-
iron,
in liquid
solubility
Figure 2.3 shows the carbon/oxygen equilibrium
arc practice
and subsequent deoxidation

too far,
is allowed to progress
will
become dissolved
final
rise
yields
in electric
then excessive amounts of oxygen
of deoxidants,
at all
This can give
and leads to a tendency for
the steel
in an attempt to avoid
(Wilson,
costs.
and the
1981).
Jackson (1975) advocates the use of the "catch-carbon"

to overcome this
problem.
carbon content just

of the melt will
more predictable.
By terminating
below the specified
be lower,
the boil
If
of the melt.
be high and variable.
the foundryman to "over-kill"

blowhole formation
This has a
as the carbon content decreases,
oxygen content will

to erratic
at 1540C and
of the carbon boil
to the control
relevance
particular
of carbon monoxide.
pressures
partial
various
to
prior
mainly by the carbon content of the melt.
is controlled
deoxidation
in steel
the solubility
technique
the carbon boil

level,
the oxygen content
and subsequent deoxidation
The use of this
technique
at a
behaviour
generally
means
that an excess of carbon has to be added to the furnace charge

to allow an adequate boil
Deoxidation
of the steel
weak deoxidants
to proceed.
is normally
to the furnace
achieved by the addition
(silicon
and manganese, as Fe-Si
or Fe-Mn), augmented by the use of a stronger

ladle,.
for this
to prevent pinhole
latter
because of its
deoxidant
Aluminium is widely
in the
used
in
bars,
form
99%
Al
the
purpose
of
rods or
pure
relatively
elements such as titanium

are reluctant
porosity.
of
low cost and availability

and zirconium.
to use titanium
Many steel
for deoxidation
compared to
foundries
on the grounds that
16
it
a "dirty"
produces
is generally
levels
variable
although
of recovery
of deleterious
the formation
inclusions,
or even pin-hole
The usual
morphology
(angular)
is type III
satisfactory,
can sometimes result
II
type
of impact
loss
an associated
with
The use of aluminium
strength.
low.
steel
in
manganese sulphide
porosity
when yields
of sulphide
inclusions
which are associated
are particularly
in steel
castings
a low oxygen
with
content.
A major problem may, however,
of the deoxidant
quantities
the aluminium
this
circumstances
boundaries
during
cause severe
this
which
will
embrittlement.
that
in recent
used for
and can
The conditions
in greater
deoxidation
years,
has been rising,
excess of 0.10% are not uncommon.

in the uncertainty
furnace,
under
depth in
dead-melted
of the state
induction
deoxidation
addition
of oxidation
furnace
than a heavily
the amount of aluminium

and aluminium
The reason for
of prediction
and the unilateral
regardless
for
grain
of the casting,
cooling
be considered
any nitrogen
Under certain
nitride.
on the as-cast
will
has been noted
to lie
stoichiometric
to combine with
precipitate
intergranular
for
3 and 4.
Chapters
It
free
to form aluminium
the initial
occurs
Under these circumstances,
are used.
the oxygen is
in the steel
present
when excessive
is added beyond the level
which
with
combination
be encountered
is thought
this
of oxygen content
of a fixed
of the bath.
heat will
require
blown electric-arc
in
contents
in the
amount of aluminium
Clearly
less
aluminium
melt.
172.3.2
Nitrogen
The absorption
operations
and refining
years,
by iron
of nitrogen
century,
nineteenth
of intensive
Indeed this
contents which is frequently

in use today.
vary slightly
with
investigation.
The
(1879) determined contents of
when Allen
melted steels
for many
demonstrated in the late
in steel was first
0.005% to 0.015oN by chemical methods.

of nitrogen
during melting
alloys
has been recognised as important
and has been the subject
presence of nitrogen
and its
observed for most air
The actual nitrogen
the different
is the range
steelmaking
content does
methods in use and
Speith and Vom Ende (1959) and Kuhn and Detrez (1962) have made
surveys of the nitrogen
expected from each method.
levels
Table 2.2 shows that the highest
nitrogen
contents
with processes where there is extensive
associated
between the molten metal and the atmosphere.

the melt from scrap additions,
into
introduced
is usually
ferro-alloys
Pehlke and Elliott

in pure iron
contact
Any nitrogen
pig iron and
small in comparison (Jackson,
quite
(1960) quote a solubility
solubility
varies
with
1975).
of 0.045 wt%N
at 1600C and one atmosphere pressure
in which this
Fig.
are normally
temperature
and the way
is shown in
2.4.
In liquid
steel,
the solubility
the presence of alloying

of nitrogen.
Strong nitride
such as vanadium and niobium increase

(Fig.
markedly
In practice,
2.5) while
elements also influences
the solubility
carbon and silicon
the amount of nitrogen
forming elements
quite
reduce it
slightly.
in
liquid
found
commonly
steel
18
is much less than the solubility
is kinetic,
reason for this
since it
in the atmosphere to dissociate

into
1962).
The
is necessary for nitrogen
before it
In the arc furnace,
the melt.
(Wright,
limit.
can be incorporated
metal is usually
the liquid
from the atmosphere by a slag cover, making nitrogen
protected
difficult.
absorption
Induction
from slag cover in this

boil,
a carbon
this
benefit
melted casts rarely
way and together
with
the absence of
lead to very high nitrogen
can often
levels
being encountered.
In certain
grades of steel where the nitrogen
deliberately
increased
(Cottrell,
is
content
1975a), nitrogen
additions
are
made using cracked ammonia, calcium cyanamide, or manganese

which overcomes the kinetic
nitride,
the dissociation
(Blake and Jordan,
reported
during
of molecular
the arc melting
is a result
that this
Nitrogen
with
has been
1971) that under some circumstances
of iron,
the absorption
law.
of the high local
arc (5000-6000K) dissociating

the kinetic
Indeed it
nitrogen.
by Sievert's
exceed that predicted
problems associated
of nitrogen
can
The authors suggest

temperatures
the nitrogen
near the
and eliminating
barrier.
is well
known to form a number of nitrides
at temperatures within
the ferrite
range.
with
iron
Paranjpe et al,
(1950) determined the phase diagram for the iron-nitrogen

system below 900C and found the existence
phases.
In steels,
however, it
of these phases since nitrogen

alloying
elements present
of five
is unusual to find
usually
distinct
evidence
combines with
to form a more stable
other
nitride.
19
Pearson and Ende (1953) collected
and their
most metal nitrides

Figure 2.6.
the thermodynamic data for
results
are summarised in
The order of decreasing stability
is:
of the nitrides
ZrN, TiN, AJN, BN, Si3N41 VN, Cr2N, CrN and Fe4N. The nitrides
formed by zirconium
and titanium
very low solubility
of their
assumed that
if
are the most stable,
in austenite
a sufficient
quantity
no other metal nitrides
present,
Under normal circumstances,
used extensively
and ferrite,
be formed (Wright,
in a steel
for deoxidation.
excess aluminium to form solid

distribution
casting,
1962).
of the casting
since it
is
Thus most of the nitrogen

will
combine with
The morphology and
precipitates.
of these precipitates
the properties
can be
of these two elements is
from the melt during solidification
rejected
it
however, aluminium is the most
former present
stable nitride
will
and because
can have a profound effect
as will
on
be discussed in subsequent
Chapters.
2.3.3
H dy
rogen
The major effect
of hydrogen in steel
castings
to form gaseous pores during solidification

decrease in solubility
on transition
(1981) point
This mobility
diffusion
casting
of hairline
These
state.
but,
with nitrogen
high mobility
can also result
of hydrogen to grain boundaries

and the formation
of the
even at
in the
of the solidified
cracks.
In steelmaking,
the major source of hydrogen is from water vapour present

atmosphere, although
contributions
as
out, hydrogen is the more
dangerous of the two gases because of its

moderate temperatures.
tendency
as a result
to the solid
pores can often be formed in conjunction

Svensson and Fredriksson
is its
from the moisture
in the
content of
20
elements cannot be discounted
and alloying
refractories
(Jackson,
1975).
With the exception
of dead melted induction
bath
of steel
a
of
content
the hydrogen
heats,
is determined by the balance between
the rate at which the water vapour dissociates
and the rate
bath
by
from
is
hydrogen
the
the action
purged
at which
During the boil,
carbon boil.
falls
Hence double-slag
period.
levels
a subsequent increase
to prevent
than single
is
during the reducing
melts tend to have higher hydrogen
slag heats because of the longer time spent

Figure 2.7 shows typical
under reducing conditions.

in hydrogen content
generally
2-3ppm, but in air melted casts it
to approximately
impossible
the hydrogen level
of the
variations
for a 31, tonne arc furnace heat (Stephenson,
1974).
Air-melted
casts usually
gives rise
to problems in smaller
the surface
contain
inside
the hydrogen is retained
not possible
alloying
and costly
critical
it
diffusion
to
however, most of
and can only be
Since it
annealing.
with
is
other
is often necessary to use vacuum treatment

components.
to reduce the hydrogen level

and problems with porosity
eliminated.
the casting
where diffusion
to combine the hydrogen chemically
elements,
for large,
castings
In heavy sections,
is possible.
removed by lengthy
3-6ppm of hydrogen which rarely
(Jackson,
In this way, it
is possible
of the melt to approximately

and hairline
1975).
cracking
lppm
are largely
21
Behaviour
Solidification
2.4
Grain Structure
2.4.1
The classical
is shown in Fig.
intermediate
2.8 which depicts
by material
composition,
temperature
pouring
The
equiaxed zone.
of these zones are determined
proportions
and processing
of a casting
zone, the
the outer chill
colurimar zone and the central
grain size and relative

largely
of the grain structure
representation
variables
such as alloy
(Davies
and mould properties,
and Garland, 1975).

a)
The chill
dendrites
at the mould wall
caused by pouring
as a result
and convection.
in the melt
(Bower and Flemings,
The columnar zone is produced by a competitive
mechanism of the chill

This region exhibits
crystals
strong
since the columnar crystals

the <100> directions,
growth (Hellawell
normally
show a preferred
1962).
1967).
growth
interface.
of mechanical properties
which are the directions
extends until
become obstructed
at the solid/liquid
anisotropy
and Herbert,
of
of thermal undercooling,
zone depends on turbulence
and the size of this
b)
from the copious nucleation
zone arises
orientation
along
of dendritic
The columnar region
the growth of the columnar crystals
by the presence of equiaxed crystals
has
in the
centre of the casting.

c)
The equiaxed zone
producing
i)
There are three major mechanisms for
equiaxed crystals:
isolated
heterogeneous nucleation
events in the melt
(Chalmers, 1963).
ii)
fragmentation
et al,
1966).
(Jackson
the
columnar
growing
zone
of
22
iii)
nucleation
(Southin,
All
at the free surface of the casting

1967).
three sources normally
degrees, and it
to varying
crystals
processing
variables
facilitates
control
equiaxed grain
to influence
known that as steels
and macroscopic scale.
enhanced by the introduction
there is always some
solidify
elements on a microscopic
There have been several
theoretical
models proposed over a number of years to describe

of alloy
composition
as solidification
from assuming equilibrium
complexity
models where complete solute

1974).
(Flemings,
All
mixing
are derived
is macroscopically
interface
A schematic representation
approximation
freezing
not strictly
is incorporated.
the solid/liquid
distribution
speed.
predicted
but the
each model in detail,
to the solidification
of a steel
takes place in the solid.
alloying
to
2.9.
tnze of course, but solid
for most substitutional
These vary in
and moves at constant
is obtained by assuming complete mixing of solute

diffusion
that
no
and
the variation
conditions
in the liquid
of the solute
is not intended to describe
simplest
proceeds.
assuming that
planar
by each model is shown in Fig.

It
or by
of the growing dendrites.
of solute
redistribution
concurrent
For example,
During Solidification
Solute Redistribution
is well
of
such as TiC or FeTi in steel,
encouraging dynamic fragmentation
It
is the manipulation
cast structure.
is often
of heterogeneous nucleants
2.4.2
of equiaxed
these mechanisms that
of the final
formation
to the origin
contribute
state
casting
in the liquid
The latter
diffusion
elements are several
is
coefficients
orders of
23
-
magnitude smaller
than in the liquid
in the solid
redistribution
elements and where back diffusion
of solute
be ignored.
can usually
The
which are interstitial
are carbon and nitrogen,
exceptions
and the effects
in the solid
may be
significant.
For the unidirectional
Co, the composition
composition
liquid
interface
of a bar of initial
solidification
is given by
Cs = Cok (1 - fS)k-l
(2.1)
fs
is
fraction
the
where
solid
k is the equilibrium
partition
be rewritten
This can alternatively
(CL) and the fraction
composition
coefficient.
in terms of the liquid
liquid
(fL)
CL = Co fLk-1
since
(2.2)
Cs = kCL and
fs + fL =1
These equations have been derived by Scheil

(1952) and are referred
to curve (c) in Fig.
is large,
and providing
will
to as the Scheil
2.9.
there is little
solidification
proceeds,
Initially,
overall
reached.
In practice
castings,
but considerable
this
Equations,
becomes solute
temperature
microsegregation
S
does
P
can
and
and
occur.
as
such
but as
enriched
k is constant,
extreme is rarely
to the situation
corresponding
change in composition,
coefficient
an invariant
(1942) and Pfann
when the volume of liquid
so the liquid
the partition
remain until
approximation
(Cs) at the solid/
of the solid
some liquid
(e. g. a eutectic)
achieved in steel
of alloying
elements
Perhaps the closest
described
is
be
the
would
above
24
of an interdendritic
formation
inadequate amounts of manganese.
grossly
containing
Not only can microsegregation

concentrations,
lead to differential
including
flow.
density
1970;
this
of liquid
of pouring
to just
and
Flemings and
block casting which
completely,
Table 2.3 shows the
in the feeder head from the start
analysis
before
1968;
which
is not inconsiderable.
In the extreme case of a 200 tonne anvil
variation
differences
Bridge and Beech, 1980).
macrosegregation
took over 80 hours to solidify
contributory
enriched liquid
(Flemings et al,
Mehrebian et al,
In large castings
There are several
movements of solute
fluid
solute
can be compoundedwith the influence
in the casting.
causes of macrosegregation,
Nereo, 1968;
in high local
result
but the effect
of macrosegregation
interdendritic
in a steel
Fe-FeS eutectic
final
(Wilson,
solidification
1981).
Table 2.3
Variation
in liquid
metal analysis
from start
to finish
pouring
of a 200 tome casting.
Liquid
Composition
C*
Si
Mn
Al
Ti
Initial
0.12
0.40
1.16
0.016 0.012 0.020
0.042 0.01
Final
0.37
0.56
1.17
0.060 0.032 0.003
0.018 0.02
* exacerbated by the effects
of arc feeding.
25
Thus it
can be concluded that although the nominal base composition
of a casting
may be in accordance with

in the structure
inhomogeneities
macro-segregation
significantly
a specification,
arising
can mean that material
through the casting
section.
from microproperties
and
vary
26
3
Chapter
Mechanisms in Cast Steel
Fracture
3.1
Introduction
Mechanics based design philosophy
The aim of a Fracture
inherent
replace the degree of uncertainty
fracture
measure of the material's

Using this
it
parameter,
of any defects
is possible
and to avoid the use of excessive

1977).
and Wright,
factorily
However, this
and the fracture
can be predicted,
design must be representative

The single
most important
mode of steels
triaxiality
with greater
factors
under service
mechanism.
parameter which determines
narrow temperature
range, and this
conditions
steel
over a
with
a change
cleavage to dull
crystalline
of the effect
fibrous
on impact
3.1. a.
it
is desirable
to operate under
of high impact energy, and many specifications

now include
the requirement
impact energy at a specified

BS 1504,1976).
temperature
This can usually

of alloying
of
there is usually
fracture
is associated
castings
the addition
the fracture
rate and state
In mild steels,
from low- to high-energy
For most applications
conditions
toughness data used for the
of this
also play a part.
energy is shown ,in Fig.
(Jackson
can only be achieved satis-
a sharp transition
fracture.
confidence,
of safety
is temperature, although strain
in mechanism from bright
1973a).
to assess the significance
the mechanism of failure
if
(Knott,
resistance
in the material
present
in conventional
parameter which is a direct
by a quantitative
design factors
is to
elements
t
for
for a minimum
(BS 3100,1976:
be achieved quite
readily
such as manganese to the
by
27
steel
impact
transition
lower
the
which
of the heat treatment
1972), or by modification
inherently
tougher microstructure.
Although
temperature has an overall
castings
to produce an
on the fracture
effect
in
steel
can
occur
phenomena
mechanism, other embrittling
in a lowering
which result
of the fracture
These are particularly
The aim of this

ductile
in steel
embrittlement
in steel
fracture
some of the factors
detail
3.2
(1962) is shown in Fig.
Chapter is to review briefly
and brittle
based on the
An example, taken from the work of
failure.
of
mode
expected
Wright and Quarrell
since they
any design calculations
invalidate
can completely
important,
toughness
be ductile
the
steel would otherwise
temperatures
where
at
and tough.
(Reed-Hill,
temperature,
3.1. b.
the mechanisms of
and to examine in greater

to intergranular
which can give rise
castings.
Fracture
Ductile
ductile
for
mechanism
accepted
The generally
void nucleation
at inclusions
fracture
is one of
followed
or second phase particles
by the growth and coalescence of these voids to give, final

failure
(Thompson and Weihrauch, 1976).
typical
dull
fibrous
appearance of the fracture
which the voids are manifest

The concept of void nucleation
by Tipper
(1949) and Puttick
samples prior
in the light
This results
to final
microscope,
failure
in the
surface,
on
as dimples.
by inclusions
(1950).
was first
By unloading
proposed
tensile
longitudinal
examining
and
sections
they were able to observe the close

ao
-A
28
of voids and inclusions.
association
Further
indirect
support
for this
mechanism came from Crussard et al (1956), who
reported
that an increase
resulted
in inferior
in the inclusion
Charpy upper shelf
changing the impact transition

Later,
pure iron
surfaces
inclusion
temperature.
size and distribution
of inclusion
only FeO inclusions.
containing
in the scanning electron
in electrolytically
By examining fracture
microscope (S. E. M.) they found
diameter of 0. lpu to be capable of nucleating
a minimum inclusion
a void,
energies without
work by Kunio et al (1977) investigated
more quantitative
the effects
content of steel
and determined a linear
between the
relationship
diameter and the dimple size observed (Fig.
It was noted that voids were initiated

FeO/matrix boundary.
In general,
3.2).
by the separation
of the
however, void nucleation
depends very much on the nature of the bonding at a matrixparticle

in steel,
interface.
this
For inclusions
bonding is weak and voids can be initiated
grow at very low plastic
will
contrast
to this,
are relatively
precipitates
strains
bonded to the matrix,
strongly
by the high localised
loops at the "poles"

that
the ductile
fracture
is these inclusions
fibrous
fracture
and nitrides
formed by vacancy
stresses
of cast steels
It
is therefore
will
large sulphides
(Figs.
In
and Ashby (1966)
and oxides,
3.3 to 3.5).
of these inclusions
clear
be dominated by
which are most frequently
surfaces
size and distribution
1973J.
and
voids can only be
of the particles.
the presence of relatively

it
(Knott,
such as carbides
showed that under such circumstances

initiated
such as oxides and sulphides
and
observed on
Control
of the
can have a considerable
29
effect
ductility
on the tensile
as shown by the work
of steel,
(1971).
Mclvor
Holmes
Gladman,
and
of
3.6 demonstrates
Fig.
the improvements which can be achieved by reducing the volume

of inclusions,
fraction
matrix
and also shows the effect
bonding discussed earlier,
sulphides
of inclusion/
by comparing results
for
and carbides.
Although macro inclusions
play an important
role
they do not generally
the fracture
strain,
the fracture
process (Broek, 1973).
in determining
details
control
In particular
of
they cannot
account for the spacing and size of the small voids or dimples
which are frequently
may not contain
(1960) first
observed on the fracture
inclusions
recognised
but that
not coalesce,
at all.
surface,
(Crussard et al,
1956).
that voids at macro inclusions

they can be linked
and which
Rogers
need
by sheets of very
small voids which form in the shear bands between the macro
This essentially
inclusions.
shear on a microscopic
process is presented
The intervention
scopic level
fracture,
in Fig.
is that
evidence of the
shearing mechanism at a macrothe formation
as shear lips
or as slant
of
3.7 (Cox, 1973).
prevents
and is manifest
reason for this
the intervention
scale and photographic
of a ductile
usually
type fracture,
represents
fracture
of a fully
on a "cup and cone"
on bend specimens.
as void coalescence occurs,
sample geometry changes to that
fibrous
of an internally
The
the
cracked
specimen, and a shearing mechanism is favoured near the

surface.
As a result,
dimples in this
region,
markings are observed.
the fracture
surface may show elongated
and areas with
relatively
few surface
30
Cleavage
Brittle
3.3
Treatments
Theoretical
3.3.1
the mechanism of cleavage involves
In steels,
low ductilities.
with
associated
The tendency for this
rate and a triaxial
cleavage fracture
tensile
uniaxial
stress
mode of
but
As a
state.
is only encountered in slowly strained

during deformation
specimens of mild steel
at
(-100K), whereas in notched impact specimens
very low temperatures

it
and is usually
is increased not only by a decrease in temperature,
high
by
strain
a
also
result,
the transgranular
{100}
along
planes,
of the b. c. c. matrix
fracture
failure
Fracture
may become apparent near room temperature
(Armstrong,
1977).
Several models have been proposed to account for the nucleation

brittle
a
of
cleavage crack,
they have essentially
in detail,
they differ
and whilst
the same foundations.
basis of Low's work of 1954 on mild steel

always precedes fracture
some yielding
to produce a cleavage crack nucleus),

by Stroh (1957), Cottrell
all
of a slip
representation
pile-up
highly
applied
acting
tensile
(since yield
that
is necessary
and the models proposed
band or twin by an obstacle
process is shown in Fig.
of dislocations
concentrated
became clear
or a grain boundary.
such as a second phase particle

of this
it
On the
(1958), Petch (1958) and Smith (1966)
the blocking
involve
slightly
in a grain
stress
stress
3.8, where a
of diameter d produces a
band.
An
to a shear stress
'C
at each end of the slip
a will
A typical
give rise
band, where r
by
Since
slip proceeds
-a/2.
movement, this shear stress is opposed by a friction
on the slip
dislocation
stress -ri which includes

resistance
of the lattice
contributions
to slip
from the inherent
(the Peierls-Nabarro
force),
31
and from clusters
from small precipitates
band as a freely
the slip
treating
deformation,
is attained
value of stress
to occur when a critical
in the adjacent
between the stress
derived a relationship
QF = Qi + kF d'z
grain,
required
a cleavage crack (aF) and the grain size
to the local
of this
grain size and yield
(d):
tensile
stress
equation
stress will
be noted,
conditions
under which a crack,
Their results
indicated
nucleus would result
that
Smith and Barnby
that cleavage fracture
It was-predicted
that
ti
the important
is the effective
= *Cy -'Ci
shear stress
energy of the system,
in causing cleavage
(`Ceff), where
S
d"2
I>,
=
is the applied
(3.2)
required
from
to spread yield
to grain.
represents
the resistance
of the grain
K, is a constant which is related

js
However, this
analysis
fails
to slip.
to the shear stress
to explain
is high,
the value of (Cy -t
i)
state.
why cleavage fractures
predominate at low temperatures where,. although

stress
would spread.
is nucleation-controlled.
stress
shear stress
the
in length of the
in a decrease in total
thereby implying
fractures
by considering
once nucleated,
any increase
between
since the two
(1967), however, extended the Stroh analysis
grain
to
required
to the Petch relation
are based on the same principles.
derivations
ry
to nucleate
the second grain.
The similarity
Leff
Stroh (1957)
(3.1)
kF
is related
where
fracture
By
crack under bode II
slipping
fracture
and considering
atoms.
of solute
the yield
is not significantly
32
-
from its
different
The experimental
room temperature value.
of Hahn et al (1959) suggest that cleavage fracture
results
be growth controlled
temperature
a certain
within
because of the presence of a significant

micro-cracks
nucleation
is not the rate controlling
strong dependence on the applied
regime
number of grains
fracture.
after
containing
must
This implies
step.
tensile
that
There is also a
which is not
stress,
accounted for in the Stroh analysis.

theory of brittle
The Cottrell
fracture
is based on a dislocation
for
allows
growth of the crack to be the
which
mechanism
factor
controlling
the cleavage crack is nucleated
theory,
dislocations
of two partial
to form a sessile
in iron
an easy nucleation
process.
1958).
(Cottrell,
In this
by providing
on intersecting
edge dislocation,
by the interaction
{101} slip
according
planes
to the
reaction
7
[111
(101)
+ 7
This therefore
[111]
(101)
the first
provides
3.9) and Knott
(see Fig.
into
a
wedge
of
(001)
stage of crack nucleation,

the model to the driving
the cleavage plane.
for the propagation
Cottrell
of this
(1958) determined the criterion
crack nucleus to be
(3.3)
d-
32
(1973b) likens
By energy considerations,
aF
'
10013
Y
where c
is the stress
required
u is the shear modulus

y is a surface energy term
for fracture
33
Hence this
model emphasises the role of tensile

the effect
explains
stress,
Cd-I) in a similar
of grain size
and
way to the
Stroh analysis.
It
that hardening,
is also predicted
the grain
size,
promote cleavage fracture
will
value of the tensile

Hence the Cottrell
contain
stress
by raising
the
point.
for homogeneous
model appears satisfactory
carbides
for example.
However, most steels
in one form or another which, being very brittle,
can provide
easy sites
of cracking
nucleated
for cleavage crack nucleation.

at pearlitic
3.10.
into
account the effect
in
proposed a model which takes
of carbides,
to be associated
An example
is presented
cementite
Smith (1966) therefore
Fig.
stresses
at the yield
samples of iron,
polycrystalline
other than by decreasing
and predicts
low fracture
the presence of coarse carbides.
with
This is in good agreement with
the experimental
results
of
McMahonand Cohen (1965).

3.3.2
Aspects of Cleavage
Fractographic
Cleavage fractures,
once nucleated,
the resulting
fracture
(Fig.
Microscopically,
3.11).
a series
of ridges
markings".
represent
a difference
highly
the surface
Low (1959) considered

in height
from the fact
crystallographic
plane,
and
facets
reflecting
of the facets
may show
arranged in the form

these markings to
between the steps on the cleavage
and subsequent fractographic
The steps result

single
exhibits
or steps which are often
of "river
facet,
surface
propagate very rapidly
that
work has confirmed

instead
of following
this.
a
the cleavage crack can be broken
up by the presence of discontinuities
in the crystal
structure,
34
planes (Gilman, 1956).
and may proceed along several parallel

These eventually
front
steps as the crack
agreed from fractographic
the crack propagates in the direction
evidence that
markings (Herzberg,
appearance of river
the effects
is generally
and it
proceeds,
of the river
merge to form fewer larger
1976).
An example of the
markings is given in Fig.
boundary.
high
a
angle
grain
of
has
from
right
advanced
crack
planar
to left
the crack plane has been forced to splinter

process as the crack front
of "flow"
3.12, which shows

As the largely
across the boundary,
in an accommodation
searches out suitable
cleavage planes
in the new grain.

Other discontinuities
of river
which may also contribute
include
markings
dislocations
screw
and
interphase
interfaces,
to the formation
inclusions
which cut across the cleavage plane
(Gilman, 1956).
Although most cleavage fractures
on the fracture
details
appearance,
by the microstructure
features
this
is the fracture
quasi-cleavage.
3.4
Brittle
of the steel,
complex.
in which few well
and the failure

(Fig.
influenced
and the
A good example of
defined
tempered
cleavage facets
mode is best described
as
3.13).
Intergranular
The two most commonfailure

fibrous
are often
of an untempered or lightly
structure,
can be identified,
the same general
surface
and composition
observed may be quite
martensitic
exhibit
Fracture
mechanisms in cast steels,
and cleavage fractures
namely
which occur in a transgranular
manner, suggest that under normal circumstances,
boundaries
grain
35
are not an inherent
dating
observations
source of weakness.
However, numerous
from the nineteenth
century bear witness
that grain boundaries are easily
to the fact
particles
or precipitate
that alter
grain boundary
the localised
(Hondros and McLean, 1976).
chemistry.
The reduced performance of engineering
through intergranular
alloys
has been observed in a wide range of metallurgical
failure
and in the case of steels
situations,
give rise
fracture
to intergranular
(1978).
and Banerji
into
classified
some of the factors
which
have been reviewed by Briant
These are presented
in Fig.
3.14, and can be
four general categories:
The presence of certain
i)
to
by the presence of elements
principally
embrittlement,
serious
susceptible
elements which have segregated
to the grain boundary without
any detectable
phase
precipitation.
The presence of discrete
ii)
grain boundary phases or
precipitates.
iii)
The action
of certain
iv)
The action
of stresses
the embrittling
It
and (ii)
at high temperatures.
applied
(in which case
can be more severe) , but only categories

be reviewed here.
effect
will
is generally
accepted that
the intergranular
be along the highest
in steels
will
present,
(Briant
boundaries,
environments.
may act alone or in combination,
These factors
(i)
corrosive
and Banerji,
or in their
fracture
path
angle grain boundaries
1978).
These may be the austenite
absence, martensite
ferrite
packet or
36
In some circumstances
boundaries.
boundary which may be coincident

boundary
can provide
grain
and this
propagation,
even a particle/matrix
a previously
with
a favourable
situation
existing
route for crack
be discussed later.
will
Hondros and McLean (1976) have examined the susceptibility
cohesion,
in terms of the grain boundary
fracture
metals to intergranular
approach is given here.
and a summary of their
By considering
on two surfaces
of
curve for the atoms
a schematic stress/separation
formed in a fracture
process (Fig.
3.15),
it
be seen that the cohesion is measured by the maximumstress

beyond which fracture
Because, to a first
and a.
can
am
should occur.
approximation,
both y (the surface energy)
to E (the Youngs Modulus),
are proportional
then
QmaY
a comparison of grain boundary cohesions by
This facilitates
examination
of the appropriate
For an intergranular
fracture
macroscopic surface
along a high angle grain boundary,
the work done in forming two new surfaces

fracture
energy of
(3.4)
ys is the surface energy of the exposed boundary

1b is the surface
energy of the pre-existing
By comparing the cohesive strength

the cleavage
obtain
(the surface
is
by
given
1b*)
Yb* =2YS-Yb
where
energies.
strength
of the grain boundary ab with
of the matrix,
a measure of susceptibility
boundary
aclo it
is possible
for intergranular
to
fracture.
37
proceeds by the parting
Since cleavage usually
planes'{hkl},
crystallographic
act
cc Ycl*
then
C3.5)
Yhkl
=2
of two low index
is
the surface
Yct*
where
energy of cleavage fracture
is energy of the freshly
created surfaces.
cohesion at a grain boundary compared with
Hence the relative
that at any other cleavage plane is

Yb*
Yct*
2YS -
Yb
(3.6)
2Y1
Using the data of Mills
et al (1973) and Hondros and Stuart
(1968)
for a Fe-3%Si alloy
(the only ferrous
data are available)
Hondros and McLean (1976) compiled a table
cohesive energies
system for which experimental

of
(Table 3.1).
Table 3.1
Cohesive Energies for
Intergranular
and Cleavage Fracture
in Fe-3%Si (Hondros and McLean, 1976)
Fracture Path
Energy (mJ/m2)
Y(om)
Intergranular
(Average Plane)
1754(average)
y*
cl
yb
462
Yb*
3047
Yb*
0.87
Ycl
Since cleavage normally

it
is clear
the lattice
difference
(100)
Cleavage
(110)
(111)
1670
1745
1848
3340
3490
3696
0.91
0.87
0.82
occurs by the separation
{100}
of
planes,
intergranular
cohesion is less than

(iYc,
cohesion for these planes*
= 0.91 , the
-*
that
although
is so marginal
it
does not normally
have any
38
on the fracture
effect
process.
It
is usually
discrete
species
or
presence of segregated
only in the
precipitate
particles
energies of cohesion become appreciably
that the relative

different.
These two situations
detail.
Segregation Effects
3.4.1
In comparison with
the situation
there is theoretically
failure
granular
well
now be discussed in greater
will
known that
only a marginal
for Fe-3%Si, where

for inter-
expectation
to {100} type cleavage,
in preference
it
is
the presence of small amounts of residual
elements can promote unequivocal

(Briant
and Banerji,
related
to cast steels
pertinent
described
1978).
will
intergranular
fracture,
Some of the specific

be considered
later,
phenomena
but first
it
is
the mechanism by which embrittlement
to consider
occurs.
There have been numerous observations
the segregation
of residual
ment, and a quantitative

(1973).
facial
corresponding
of segregation
indication
Although
it
to use the grain boundary cohesion as a

stress
in absolute
terms, this
of the tendency for intergranular
when compared to the cohesion of a suitable

planes.
on inter-
some idea of the
changes in grain boundary cohesion.
measure. of fracture
a useful
model was proposed by Seah and Hondros
and were able to obtain
would be inappropriate
between
elements and grain boundary embrittle-
They considered the effects

energies,
on the relationship
model gives
failure
set of cleavage
39
-
Gibbs
by
the
adsorption
given
dy =-
is
(3.7)
RTT'd (loge X)
dX, and r is the associated

bulk
solute
small
of
The effect
alloy
form
the
takes
which
isotherm,
is
dy
the energy change corresponding
where
interval
binary
energy for a dilute
The change in interfacial
to a bulk composition
interfacial
concentrations
enrichment.
on the surface
energy (which is of the same order of magnitude as the grain
systems.
This again can be used only as a guide to the effects
of the residual
since an absolute value of the surface
elements,
inherent
depend on the segregation
energy will
function
is
in
turn
a
which
intergranular
fracture
were able to obtain

with segregation
of the segregant on the two
between the cohesion of a boundary
a ratio
Hondros and McLean (1976)
surfaces,
and that of a clean boundary (ab*).
(ob(s)*)
Y-brS_
in the system,
heat treatment.
of prior
By assuming equal partitioning
Qb(S)
for a number of alloy
3.16
boundary energy) is shown in Fig.
2Ys
m-x
m-x
yb
-
(3.8)
2Ys - Yb
to the alloy
(metal-solute
X).
where the suffix
m-x refers
The experimental
data of Hondros and McLean (1970) suggest
that the minimum value of the surface

Ysm-x(
)xI
in
general,
and
ys,
for grain boundary energies,

these approximations
Yb(s)*
becomes
Yb*
: 0.5.
energy is given by
the same situation
i. e. ybm-x (min) #hhb.
in equation
(3.8)
the relative
applies
Using
cohesion
40
Despite the crude approximations
the experimental
agrees well with
used in this
observations
Hqndros (1973), who used Auger spectroscopy

measurement of the segregation,
the cohesion ratio
This
Yb*
YC1*
of
values
since
above,
a direct
to obtain
value of
and obtained a similar
cohesion for cleavage fracture,
'Yb(s)
Yct *
Yb*
Yb (s) *X
T*
(see Table
are 0.8-0.9
the cohesion
be even lower than the value
boundary
will
segregated
at a
predicted
of Seah and
using the Gibbs equation.
lattice
Compared with
model, the result
and typical
Yct*
3.1).
Yb s*z0.4
Ycl*
gives
Under these circumstances,
an intergranular
mode of failure
would
be expected.
3.4.1.1
(T. E. )
This phenomenon has been studied

cast low alloy
relating
steels,
to steel
The segregation
in steel
but only a brief
castings
will
of residual
in both wrought and
resumd of the work
be presented here.
impurities
to the grain boundaries
can occur at any stage of the heat treatment
which the steel

although
extensively
is subjected
the embrittlements
(Banerji
and Briant,
loss of ductility.
lead to intergranular
1980) and
from segregation
resulting
stages of thermal exposure are manifest

ways, they all
cycle to
in slightly
cracking
at various
different
and the associated
41
N
are from groups IV-VI
The most commongrain boundary embrittleis
(Briant
in steels.
impurities
as trace
(see Table 3.2) which are often found
table
of the periodic
1978).
and Banerji,
Table 3.2
CommonGrain Boundary Embrittlers
Va
IVa
Group
Si
PS
Ge
As
Se
Sn
Sb
Te
research into
Historically,
has been divided

a)
VIa
into
the problem of temper embrittlement
two regimes.
One-step Temper Embrittlement
ment as it
is often known, occurs mainly in high strength
quenched and tempered steels,

tempered for short
where the martensite
times at low temperatures
hardness of such steels

temperature
(O. S. T. E. ), or 350C embrittle-
increases,
decrease in fracture
exhibits
of this
been known for many years,
the actual
recently,
remained speculative.
(1979 a, b, c) has shown that

segregation
as the tempering
an anomalous
type of embrittlement
have
mechanism responsible
Work by Briant
in low alloy
steels
has,
and Banerji
substantial
of P, S and N can occur during austenitisation.
however,
alloying
most cases,
aluminium are present
sulphur
The
energy when tempered in the range 250-350C.
Although the characteristics
until
(<400C).
decreases monotonically
yet the steel
has been
and nitrogen
In
elements such as manganese and
in the steel
respectively,
and form stable
compounds with
but phosphorus is usually
in
SHEFFIELD
UNIVERSITY
42
in the austenite
solution
in its
boundaries
and is free to segregate to the grain

form.
elemental
impurity
is. the most deleterious
reason, phosphorus
element with respect
crack nucleating
-a
to O.S. T. E.
alone is not sufficient
However, phosphorus segregation

cause temper embrittlement
For this
to
is first
site
required.
At tempering temperatures
transforms
the structure
(Lenient et al,
prior
of around 350C, the c-carbide
austenite
1954).
to give a thin plate-like

Those plates
grain boundaries
to nucleate
a brittle
the
with
(which are already weakened by

effective
intergranular
McMahon (1975) has shown that the formation

exacerbate the effects
cementite
which are coincident
the segregated phosphorus) can provide

barriers
in
additional
crack.
Moreover,
of cementite
of phosphorus segregation
slip
can
by solute
rejection
along the grain boundaries.

Thus there are two factors
neither
is
sufficient
which
of
in isolation.
purity
which combine to give O. S. T. E.,
steel
isation,
At higher
For example Banerji

which exhibited
and even after
embrittlement
to promote intergranular
et al (1978) examined a high
little
segregation
during austenit-
tempering in the susceptible
region,
no
was observed.
tempering temperatures
be vulnerable
fracture
(>400C) the steel will
to, one-step temper embrittlement,
coarsen and lose their
effectiveness
no longer
since the carbides
as crack nucleating
sites.
43
b)
in toughness
transition
temperature
are isothermally
steels
is
when a steel
slowly
days to cool
after
be rapidly
cannot
castings
The same effect
is particularly
This
temperatures.
take
cooled
observed
range
be observed
may also
tempering
at relatively
important
in practice
quenched and their
cores may
to room temperature.
by the addition
is retarded
as molybdenum, titanium
However, after
more potent
of alloying
elements such
or boron.
prolonged exposure to the ageing temperature,
other
such as Sb and Sn may also segregate to
embrittlers
the grain boundaries
and within
induce
intergranular
to
can occur
al,
cause
to the grain boundaries unless its
segregates readily
diffusion
high
since
As in O.S. T. E., phosphorus is again the main contributory

since it
low-
when tempered
aged in the temperature
(McMahon, 1975).
375-560C
large
is often
that
to the
in the ductile-brittle
and increase
decrease
alloy
(T. S. T. E. ) refers
Two-step
100-200hrs.
brittle
sufficient
fracture
segregation
(Mulford
et
1976).
The actual
fully
mechanism of crack nucleation
understood.
in T. S. T. E. is not yet
Kameda and McMahon (1980) observed a crack
have
to
nucleated
appeared
which
at the interface
inclusion,
matrix
and a non-metallic
Clarke
(1981) suggests that
but recent work by Wirth
fine needle-like
unidentified
compound may be responsible.
precipitates
have been observed at the prior
boundaries
of embrittled
conclusive,
and further
austenite
grain
are by no means
are warranted.
and
of an
precipitates
Although these
En3OA, the results

investigations
between the
44
It is,
therefore,
treatment
of large steel
possibility,
the first
In order to minimise this
castings.
obvious approach is to produce the cleanest
with minimum impurity
steels
and economic limits
are practical
temper
to occur during the heat
processes are liable
embrittlement
possible
that both one-step and two-step
clear
However, there
contents.
to which this
can be achieved,
and so the other approach is to attempt to minimise the segregation

elements to the grain boundaries.
of impurity
been noted that Mo additions

but the effect
fracture
depends not only on the Mo:P ratio,
of the Mo. A similar
effect.
and nitrides,
Seah et al (1979) showed beneficial
in
controlling
elements
earth
3.4.1.2
Hot Tearing
Although
hot
included
serious
strictly
than an intergranular
rather
here since
defects
it
encountered
3.17 and 3.18.
of rareproblems
of RE-oxysulphides which
phenomenon,
it
is
one of the most common and
in steel
arising
an interdendritic
speaking,
embrittlement
represents
The nature of the fracture

Figs.
effects
energies.
is,
tearing
thus negating
T. S. T. E., but additional
were encountered owing to the formation

reduced the upper shelf
but also
problem is also encountered
forms carbides
with Ti, which readily

its
the
which determines the
on the carbon content of the steel

solubility
Consequently,
as carbides.
of Mo in suppressing phosphorus induced inter-
effectiveness
granular
phosphorus segregation,
on the presence of the large Mo atoms in
relies
not precipitated
solution,
can retard
It has already
castings
(riiddleton,
1966).
from a hot tear is shown in
45
It
accepted that hot tearing
is now generally
range before the steel
solidification
Certain
features
characteristic
been known for some time,
is completely
solid.
process have
of the tearing
to the hot cracking
and are relevant
of other cast metals besides steel
the
occurs within
(Clyne, 1976).
These are:
i)
The stresses
which lead to crack formation
from the freezing
contraction
to be constant within
(Kondic,
mainly
which can be assumed
of the metal,
the normal range of steel
compositions.
1968).
Cracking occurs in the solid/liquid
ii)
originate
the fraction
is large.
solidified
two-phase region when
(Bishop, Ackerlind
and Pellini,
1958).
The interdendritic
iii)
the cracking
region are extremely
of a casting
ability
(Metz and Flemings,

Details
distribution
cohesion and liquid
to withstand
important
in
in determining
the thermal contraction
the
stresses
1970).
for strain
of the processes available
accommodation may
be found in Clyne (1976).

above, it
From the considerations

factors
a)
which promote hot tearing
Mould restraints
(cores,
design) which accentuate

b)
inserts
The presence of a temperature
of interdendritic
remainder of the casting
liquid
that
or the inherent
gradient
along the casting
solidification
is complete.
casting
stresses.
This region will

after
two of the main
are
the contraction
"hot
a
spot".
generates
which
film
is clear
still
contain
of the
-46An example combining (a) and (b) would be a casting

thick
by already solidified,
members which are restrained
quicker
cooling
areas.
techniques have been employed to study the
Various experimental
hot tearing
but the most quantitative
susceptibility,
the use of a "dog-bone"
involves
in aluminium alloys,
cracking
in steel.
is possible
measure of the area of cracking

and Xcr =1
uncracked casting,
studied binary
for a completely
and silicon
observations
an
broken sample.
Shin (1981)
The most pronounced

and phosphorus
regions
during
also proved to be deleterious,
but both
were rendered harmless by the addition
of
This is in agreement with previous
by Middleton
that in commercial steels,
(1966).
However, it
the effects
elements on cracking
the potency of each element.
is recognised
of a combination
susceptibility
since there may well be solute
influence
a quantitative
P, Si and C and also
to the interdendritic
Silicon
manganese to the melt.
clear,
to calculate
were shown to be from sulphur
which segregate strongly

solidification.
method of
(Xcr) such that Xcr =0 for
of Fe with S, %,
alloys
on hot tearing
alloying
resistance
Fe-Mi-S and Fe-Nh-Si systems.
the ternary
sulphur
of compositional
to examining commercial low C steels,
In addition
3.19).
but has been
the effects
Using the electrical
Clyne and Davies (1975) it
effects
(Fig.
shaped casting
adapted by Shin (1981) to evaluate

variables
method
devised by Clyne and Davies (1975) to study
This was initially

solidification
containing
of
is by no means
interactions
which
47
3.4.2
Effects
Precipitation
There are many examples of intergranular
failure
by the presence of grain boundary precipitates,

will
be discussed later
in this
being initiated
some of which
section.
Plateau et al (1960) proposed a mechanism for brittle

fractures
granular
which propagate in a semi-ductile
due to the presence of precipitates.

cracks are nucleated
decohesion
by
at their
or
by the linking
propagation
the fracture
ductile
manner
He suggested that micro-
by fracture
either
inter-
interface
of the precipitates
the matrix.
with
of these microcracks
Crack
results
in
having the dimpled appearance characteristic
failure
on a microscopic
time being confined
scale,
while
to the immediate vicinity
of
at the same
of the grain
boundary.
Hondros and McLean (1976) have considered
boundary cohesion is affected
Schematically,
yb and ym_p are the energies

particle
by the presence of hard particles.

is shown in Fig.
the situation
interfaces
the way in which grain
of the metal/metal
3.20, where
and metal/
and ys and yp are the average surface
energies of the metal and the particle.

The cohesion at the particle/matrix
interface
compared to the
boundary
is
by
cohesion
given
grain
Ys + Yb - Ym_p
Ym p
2Ys - Yb
The term ym
is referred
b*
p*
interfacial
the
of
values
(3.9)
to as the work of adhesion.
Although
energy have been measured experimentally
48
(1971) measured
for only a few systems, Navara and Easterling

the work of adhesion for alumina particles
angle between a decohered particle
the contact
data, Hondros and McLean (1976) calculated
Using their
Y*Fe-Al
and the matrix
anneal.
an equilibrium
after
in iron by examining
203
0.22, which shows the extremely
Yb*
strength
interface
Fe-A1203
the
of
original
grain boundary,
compared to that of the
and therefore
fracture
interface.
is likely
proceed by the separation
of this
tendency of a precipitate
to promote an intergranular
will
low
depend on both the nature of its
In general,
to
the
failure
bonding to the matrix
and
the morphology of the precipitate.

once again,
it
must be emphasised that
fail
It
strength.
at stresses
predicted
of cohesion
is only used as a comparative measure of the
of the interface
fracture
the strength
is well
up to several
theoretically
known that most materials
can
orders of magnitude below those

of localised
as a result
stress
concent-
rations.
The concept of a slip
particle
band intersecting
a hard non-deformable
to produce a crack nucleus has been introduced
Smith (1966).
The high stresses
a slip
band may either
matrix
interface
result
which build
by
up at the head of
in the decohesion of the particle/
or may be sufficient
through the particle.
Such a crack,
the most energetically
favourable
to generate a shear crack

once nucleated,
route,
will
which is likely
boundaries.
the
weakened
grain
already
along
follow
to be
49
of intergranular
instances
Some specific
castings
caused by precipitation
3.4.2.1
Aluminium Nitride
fracture
Precipitation
fracture
into
many investigations
now be discussed.
phenomenawill
This is considered by many to be the single

of intergranular
in steel
most important
the phenomenon over a number of years.
occurs and realistic
have not been unequivocally

granular
failures
continue
discussed in greater
of the mechanism
ways of avoiding
in Chapter 4.
morphology is characterised
facets
coarse
angular
of
which are closely
presence
the as-cast
be
to occur and the topic will
detail
it
Consequently inter-
established.
the fracture
Macroscopically,
cause
and there have been
castings
Despite the abundance of work, however, details

by which embrittlement
in steel
grain boundaries
related
despite
of the casting,
by the
to
the fact
that these boundaries may have been replaced by a new system of

boundaries
grain
temper-embrittled
and often
relief
from features
After
graphic
metallic
steels,
could
samples (Fig.
appear dull,
Unlike
the case of
3.14) the facets
with occasional
show some
bright
reflections
on the surface.
the initial
granular
during heat treatment.
by Jolivet
observations
fracture
could be caused by the "deposition
constituents
positive
varied
steel
and showed that
of metallo-
occurred in aluminium-killed
evidence that aluminium nitride
be a cause came from Lorig

the aluminium
inter-
such as cementite or some other non-
phase" and frequently

the first
(1942) that
and nitrogen
a high
level
and Elsea
contents
(1947).
These authors
of a 0.30%C, 1.6009n
of these elements
in conjunction
50
with
rate increased
a slow cooling
to inter-
the susceptibility
fracture.
granular
A1N was identified
as the cause by X-ray analysis
from
the steel
separated
In the steels
electrolytically.
high aluminium and nitrogen
containing
of residues
it was possible
a grain boundary network of precipitates
in the optical
These appeared as needles growing into
the austenite
microscope.
grains
to the boundary.
adjacent
(1952) proposed a mechanism for intergranular
Lorig
to observe
failure
whereby the crack propagates between these needles in a

manner near to the grain boundary.
transgranular
this
in the fracture
results
though microscopically
series
investigation
in the transmission
from the fracture
extracted
by electron
diffraction,
resulted
reflections
were associated
as A1N
morphologies.
with
surface which gave rise
when viewed optically.
in microductile
identified
and
although no attempts were made to
the plates
on the fracture
Wright and
These were plates
the reasons for the two different
was found that
techniques
forms of A1N on replicas
both of which could be positively
dendrites,
bright
surface.
3.21.
process was made
microscope (TEM).
(1962) observed two idiomorphic
Quarrell
to the grain
is shown in Fig.
of the fracture
electron
appearance,
has occurred by a
by the development of microfractographic
possible
facets
crack propagation
?'fore detailed
explain
having an intergranular
of steps between the A1N needles adjacent
boundary.
Macroscopically,
failure
occurring
flat,
It
featureless
to the occasional
The dendritic
form
round the precipitate
51
-
boundary.
to
the
grain
near
C1965).
Altmami
al
et
work of
the later
(1952) described
Although Lorig
the fracture
by
Wright
Quarrell
and
observed
spacing
(-gum) and these precipitates
in the optical
microscope.
The important
properties
of the matrix,
coincident
with
fine
concept revealed by
the micro-
depend to a large extent
since the fracture
on the
path is not exactly
the boundary.
Sulphide Precipitation
3.4.2.2
aluminium nitride
erbrittlement
this
precipitation,
in
IF
steel
of
commoncause
a)
arm
appear as needles
which appears intergranular,
mechanisms of crack propagation
After
the dendrite
was extremely
would therefore
round
is that although grain boundary A1N gives
these investigations
to a fracture
as occurring
should be remembered that
it
AIN,
of
"needles"
rise
was supported by
This observation
castings,
is the second most

to the
and may contribute
in several ways.
Type II hiS Precipitates
It is well
steel
known that the morphology of NhS inclusions
is determined mainly by the oxygen content

Linder normal circumstances
Charles 1972,1973).
been
deoxidised
have
which
Type III
(angular)
with
MnS inclusions.
is added or segregation
local
thoroughly
oxygen contents,
If,
(Baker and
steel
may be encountered
(Jackson 1977).
these can initiate
pseudo-intergranular
and reduce the upper shelf
castings
aluminium contain
however, insufficient
of aluminium has given rise

then the dendritic
in
Al
to high
Type II MS inclusions
Since they occur in sheets,
energy quite
fracture
in a casting
significantly.
52
In order to avoid the formation
to ensure that
This provides
of type II NhS, it
Al is added to promote type III
sufficient
sulphides.
yet another motive for the tendency to add excessive
in
turn result
which
may
aluminium,
of
amounts
in intergranular
from A1N embrittlement.
fracture
b)
is necessary
Overheating
This phenomenon occurs in both cast and wrought steels
grain boundaries
austenite
of MnS at the
the secondary precipitation
with
associated
In wrought steels,
of the primary
this
during cooling
normally
sulphides
from high temperature.
occurs after
by a high temperature
the dissolution
austenitising
but Brannnar et al (1959) and Baker and Harrison
treatment,
(1975) have shown that a similar

of large steel
the slow cooling
can take place during
effect
castings
after
Examination of a 0.15%C, 3%Ni investment
containing
0.02S and 0.009oP revealed

surface with extensive
nucleated by very small

Harrison,
1975).
(0.5=)
Additionally,
is
solidification
complete.
fracture
and is
casting
a matt intergranular
arrays of fine
particles
equiaxed dimples
of NhS
(Baker and
towards the centre of the casting
smooth facets were observed which were found to be associated

intergranular
films
of iron phosphide (FeP not Fe3P).
A mechanism was proposed for the precipitation

in Fig.
rise
regions
of iron phosphide at the intersections
austenite
boundaries.
grain
austenite
region,
contain
process (as shown
interdendritic
3.22) wherein the solute-rich
to a film
with
On subsequent cooling
with
give
the
through the
those areas on the grain boundary which do not
the phosphide act as sites
secondary sulphides.
Thus, as Fig.
for
the precipitation
of the
3.22 shows, there is a
53
-
to
from NnS-induced IF at the surface of the casting
transition
FeP-induced IF at the centre.

c)
Other Sulphides
large intergranular
Leger and Guillaume (1979) have identified

precipitates
0.10%Al together
These sulphides
containing
content of 0.31%.
more "shiny".
in appearance to A1N-induced
However, most commercial steel
much higher manganese contents
castings
contain
for this
reason the sulphides
and
but the
micro section,
on a polished
were similar
IF, though slightly
than 0.31%, and

MIS.
are almost exclusively
under normal circumstances
is unlikely
casting
were much coarser than AIN precipitates
fractures
Therefore
low 1
with an abnormally
could be seen clearly

resulting
MnS in a steel
of AlS and Al-rich
of AMS
the precipitation
to be a problem.
Niobium Carbide Precipitation
3.4.2.3
Hannerz et al (1968) and Gibson (1979) have reported

of intergranular
failure
in large
steel
castings
instances
which were
to the presence of niobium carbide precipitates
attributed
the as-cast
boundaries.
grain
The casting
examined by Harnerz et al was a crankshaft
diesel
engine with
an as-cast
composition
examination
revealed
embrittled
facets)
surfaces
(a dull
and large plates
diffraction
(Fig.
3.23).
be
to
controlled
process
and knowing the cooling
for a naval
weight of 20 tonnes, and a nominal
of 0.22%C, 0.76%Mn and 0.068%Nb.

features
at
similar
Fractographic
to those observed on A1N-
background interspersed
of NbC were identified

By considering
shiny
by electron
the precipitation
by the rate of diffusion

rate of the casting
with
of niobium,
the authors
54
-
calculated
was found that
treatment
clearly
impractical
at temperatures
is
1400C
which
or
above
of
on a commercial scale.
the presence of coarse filamentary
Gibson (1979) reported
of a large node steel
fracture
intergranular
on the partially
precipitates
only by
could be redissolved
the precipitate
solution
to be ,.2O00. It
of the precipitate
the thickness
casting
NbC
surface
0.13%C, 1.30oMn, 0.055%V
containing
and 0.025 oNb.

In both these instances,
the separation
Section 3.4.2,
3.4.2.4
appears to have been caused by
fracture
than by the fracture
rather
as suggested in
interface
of the particle/matrix
of the precipitates.
Vanadium Carbide Precipitation
This has been identified
as a possible
Brook (1976) who observed dendritic

fracture
the
on
surface
cause of IF by Barnard and
vanadium carbide precipitates
of a 2%Ni-Cr-Mo-V ingot,
42
Cr-Mo-V
in
(1973)
tonne
Spiess
casting.
a
and
case, the precipitate
forms
intergranular
of
other
with
as
Nevertheless,
the effect
so for the investigation

other precipitates,
namely aluminium nitride
3.4.2.5
Boride and Carboboride Precipitation
A minor cause of intergranular

Mahmoud(1974), who reported
/
embrittlement.
and manganese
to exacerbate the problem.
sulphide
precipitates
impaired as
by Barnard and Brook, where
were also present
carboboride
form.
This was particularly
was significant.
reported
In the latter
in a massive plate-like
case were the mechanical properties
In neither
seriously
was present
and by Naumann
and
fracture
was investigated
by
the presence of small globular

boride
a massive semi-continuous
55
film
at the prior
containing
0.002-0.006% boron.
intergranular
while
to that associated
Ion microprobe analysis

a complex chemistry,
approximately
by the carboboride
in a much smoother fracture
resulted
castings
The former promoted a dimpled
with voids initiated
fracture
the latter
similar
austenite
boundaries
of steel
grain
appearance
with temper embrittlement.
showed both forms of precipitate
the carboboride
having a composition
to have
of
(Fe0.91 M0.1)20-22 000.1, B0.9)
being based on Fe2B, with-other
boride
the
and
5-6
elements. replacing Fe in
solution.
In order to minimise the effects
of these two constituents,
boron
that
since
optimum
contents
was suggested
for hardenability
in
0.001-0.003%
(the
hardenability
the
range
are
purposes
boron) excessive additions
relies
on soluble
effect
be
avoided.
should
and
it
have little
effect
beneficial
56
Chapter 4
in Cast Steels
Aluminium Nitride
4.1
Introduction
The influence
of steel
has only been fully
time,
of this
Since
fracture,
grain
break-up and ingot panel cracking,
between JUN and these features
size control,
and a correlation
is now generally
This chapter examines the techniques
out to
on the mechanisms of
precipitate
phenomena such as intergranular

forging
since a method for its
amount of work has been carried
a considerable
determine the effect
appreciated
and properties
was developed by Beeghly (1949).
chemical determination
that
on the structure
available
accepted.
for the observation
of AlN and discusses some of the consequences of
and detection
A1N precipitation
with
respect
to the structure
and properties
of cast steels.
4.2
Observation
Detection,
The structure
(similar
and Identification
is close packed hexagonal
to ZnO) with
lattice
of A1N
parameters a=b=3.11J,
c=4.99..
It melts at 2200C and 4 atmospheres pressure,
dissociates
at pressures
water and more rapidly

decomposition
as
by mineral
products.
of JUN from the matrix

metallographic
below this.
A1N is hydrolised
slowly by
acids to form alumina and ammonia
This means that during
(either
but
for chemical analysis
the extraction
or for
purposes) care must be taken to ensure the
reagents used are anhydrous.

4.2.1
Chemical Methods of Detection
The most widely

content of steel
used method for determining
the aluminium nitride
has been that developed by Beeghly in 1949.
57
This
the dissolution
involves
(typically
mixture
ester/halogen
residue
by a distillation
Beeghly
that
in steel
to determine
extensively
Woodfine
and Quarrell
attempted
to define
granular
other
factors
technique
Several
and Jackson
as Swinburn and Melia
of other
being
However,
below which
not
(1970) have pointed
and may be included
consequence, the validity

criterion
is seriously
in question.
that a more accurate description

to say that it
ester/halogen
for the determination

obre recently,
based on this
of the Beeghly method would be
but soluble
of nitrogen
which are insoluble

in sodium hydroxide
dissociation
total
temperatures.
content of the steel,
calculate
nitride.
This work has further
(used
method has been developed
temperature of the various
nitrogen
in the
in the residue).
by Baker et al (19 79) to determine the mobile nitrogen

at different
As a
Swinburn and Melia suggest
a hydrogen extraction
a sample of steel
Other
in the ester-
in the analysis.
determines the nitrides

solution,
but
to IF,
the Beeghly method
out,
of some predictions
inter-
do many
only
such as Si3N4 and SiN are also insoluble
halogen solution,
including
authors
cannot be assumed to separate A1N alone from the matrix.

nitrides
used
and Bradshaw (1970)
minimum "%oNas A1N" values
have an influence
by
claims
by the presence
the "%N as AIN'.
could be avoided.
fracture
in the
of nitrogen
in this
resulted
(1960)
acetate)
The original
procedure.
the method was unaffected
elements
alloying
bromine/methyl
and the determination
by filtration
followed
in an anhydrous
of the matrix
it
nitrides
content of
Knowing the
present and the
is then possible
to
present as each individual

inadequacies
of
the
emphasised
58
the Beeghly method, since it was found that manganese-silicon
in the bromine/methyl
may also remain undissolved
nitride
acetate
solution.
However, in a great number of instances where there is no
interference
from other nitrides,
the Beeghly method is valid,
it would be wrong to cast doubt on all
and
based on this
correlations
technique.
4.2.2
Techniques
Metallographic
of A1N can be extremely
Grain boundary precipitates

viewed in a metallographic
and as Woodfine and Quarrell
section,
the inability
fine when
to detect
a grain boundary phase
(1960) pointed
out,
in the optical
microscope cannot be taken to imply its
For example, in one sample whose fracture

no metallographic
steel
was 80% intergranular,
evidence of JUN could be found, even though the

indicated
Beeghly method of analysis
0.005%N as A1N.
only when the aluminium and nitrogen
usually
absence.
are high (-0.15%Al,
contents
It
is
of the
be
A1N
that
can
resolved
-0.015%N)
optically.
When viewed unetched and in reflected
in
dark
colour,
grey
appears
using polarised
Lorig
light,
but it
light
aluminium nitride
can be seen more easily
under which it
is strongly
(1947)
Elsea
and Woodfine and Quarrell
and
of picric
acid in alcohol
boundary MN, particularly
when a wetting
that an etchant
zephiran chloride
It was not until
anisotropic.
(1960) found
highlighted
the grain
reagent such as
was also used.

1962 that direct
by
Wright
A1N
was
made
of
observation
and identification
(1962) using microfractographic
59
in the T. E. M.
This involved
surface of a thin
carbon film
techniques
fracture
Intergranular
fracture
precipitates,
which had been extracted
replication.
Selected area electron
alcohol.
surfaces were found to be covered by A1N

onto the carbon during
diffraction
techniques were
the AIN, and the measured spacings agreed

ASTMdata.
moderately well with published

deviations
that the slight

have resulted
onto the
which was subsequently
of 5% bromine in ethyl
removed using a solution
used to identify
the deposition
Baker (1962) suggested
(5%) from the published
spacings may
from the presence of other elements in solution
in
the AiN.
The development of the SEMwith energy dispersive
also been useful
for
the examination
and IF caused by AIN precipitation

characteristic
4.2.3
use as tools
can be identified
probe microanalysis
by its
surfaces
are not readily
contained
to identify
visible.
on intergranular
analysis
a complex form of A1N which
small amounts of Fe, Mn, Si,

However, the limited
and the complex experimental
since it
for quantitative
microsections
Mahnwud (1974) used ion microprobe

fracture
(e. p. m.a. ) have
for examining A1N precipitates,
and the precipitates
analysis
little
fractures,
Other Techniques
is necessary to use polished
solution.
of intergranular
has
appearance in the SEM (see Chapter 6).
Techniques such as electron

limited
analysis
Cr, Ca and Ti in solid

of this
availability
requirements
mean that
technique
the method is
used.
A novel technique
ti
for detecting
AIN in steel
castings
devised
was
60
by Steck (1969) who claimed to be able to differentiate
embrittled
and good castings
by ultrasonic
found that
if
probe was positioned
the ultrasonic
to the columnar grains

additional
the prior
It was
testing.
perpendicular
there would be an
of the casting,
of the beam due to the presence of A1N at
attenuation
grain boundaries.
austenite
between
for any grain boundary network,
This of course would be true

for A1N.
and not just
suggests the technique may also be able to detect
Steck
the presence of
large amounts of Type II %S inclusions.

4.3
A1N as a Cause of Intergranular
The term "Rock Candy" fracture
Fracture
is widely
foundry industry
to imply intergranular
the precipitation
of aluminium nitride.
involved
the ambiguities
term will
austenite
in a descriptive
boundaries
will
grain
term of this
kind,
the
had an unusually
magnifications
at the prior
be designated "IF".
A1N as a possible
defective
they
examined
a
when
fracture
caused by
However, because of
caused by A1N precipitation
Elsea (1947) identified
in the optical
the original
Lorig
and
cause of intergranular
commercial casting
high aluminium and nitrogen
content.
which
At high
microscope (>1000x) they were able
to observe chains of non-metallic

follow
embrittlement
the steel
be avoided in the remainder of this work and interfracture
granular
used within
particles
which appeared to
columnar grain boundaries
around which
had occurred.
fracture
Using experimentally
melted casts of base composition
1.60$bn, 0.50%Cr, 0.35Ib,

contents
and after
heat treatment
broken by slow three point

I
they varied
bending.
0.30%C,
the aluminium and nitrogen
(quench and temper) samples were

Although it
was not possible
61
to analyse individual
castings
for Al and N, a clear
between the amount of Al added during deoxidation

and the degree of intergranular
0-281b/ton*)
Increasing
the fractures
(0.40%).
With Al additions
of A1N in the melt.
to the precipitation
this
random form which acted as a nucleus for
This was in a coarse,

subsequent solid
was noted.
Later work by Woodfine and Quarrell
decreased.
(1960) attributed
fracture
from
(0.89%), however, the percentage IF on
than 20lb/ton
greater
(varied
in an increased
the amount of Al added resulted
tendency for IF up to about 81b/ton
correlation
state precipitation
and prevented the formation
of a grain boundary network.

Lorig
and Elsea also noted a correlation
content and the cooling
of %IF with
For a given Al
rate of the casting.
content,
the amount of IF observed increased with
nitrogen
content and decreasing
cooling
the nitrogen
rate,
increasing
both of which
tend to promote A1N precipitation.

Fig. 4.1 presents
important
variables
corresponding
likely
a sumrunaryof the effects

(oAl,
to points
to be susceptible
Since the actual

nomenclature will
%Nand cooling
of these three
rate).
above and to the right

to IF at the cooling
Compositions
of each curve are
rate represented.
Al contents were not analysed,

be retained:
100%
assuming
recovery.
%0.05oA1,
as a guide,
this
lib/ton
62
Lorig
from single
test
"safe"
was quite
layer
of AMNof critical
at the grain boundaries.
and Elsea's
A1N thickness
This required
Effect
for different
Wright and Quarrell

strength
to fail
(1962) explained
to estimate
the
at various
between 150OCand650C to obtain
different
strength)
is low.
strength
Wright
(1962)
temperatures
strength
at room temperature.
failure
more favourable
a relatively
tempered a 0.27%C, 1.06 Yn steel
ductile
from
was observed
or were as-cast.
is increased by heat
strength
do
they
than
when the matrix
route
performed mechanical tests
in an intergranular
and the grain boundary (see
of the matrix
When the matrix
which had been
in terms of the
this
the grain boundaries provide
(lower matrix
of the
of Heat Treatment
had
been
those
than
which
normalised
manner
treatment
when a
Al and N levels.
hardened and tempered were more likely
Chapter 3.4).
measurements
an integration
It was noted by Lorig and Elsea (1947) that castings
relative
similar
is precipitated
thickness
rate over a range of temperatures
precipitation
4.3.1
Lorig
The model was based on IF occurring
good.
continuous
model to predict
nature of some of his
the questionable
the agreement with
approximations
total
to be sure of avoiding
Al and N levels
Hannerz (1968) used a theoretical
despite
and
curves
They cannot be
and showed only trends.
results
used to predict
IF.
however, that the curves were obtained
and Elsea stressed,
levels,
and
A transition
at high tempering temperatures
to an intergranular
to the lower tempering temperatures

At the lowest tempering temperatures
mode corresponding
(higher
a point
fracture
became
the
predominant
cleavage
matrix
strength).
was reached where
mechanism in the
63
steels.
martensitic
The concept of removing IF by a high temperature solution

by
Lorig
was considered
(0.07%) and 31b/ton
l1lb/ton
containing
and Elsea (1947).
They homogenised samples

(0.15%) of aluminium for
2 hours at 1260C and found that by rapid cooling

in the first
was eliminated
at 1260C followed
in fracture
temperature
resulted
established
austenite
from the prior
being dissolved
Rapid cooling
whilst
grains.
in its
resulted
boundaries.
austenite
assuming that
Harris
but all
general conclusions,
treatment.
temperature.
of this
4.3.2
austenite
that
grain boundaries.
in solid
retention
the A1N was
solution,
to occur at the new
and Chandley (1962) came to the same

these authors can be criticised
removed by such a heat
A1N grain
depend on the Al and N contents
which in turn dictate
This will
for
of the
the solubility
be discussed further
in Section 4.4
Chapter.
Effect
The effects
for
This implied
the success in dissolving-the
Clearly
in question,
round the newly
occurring
IF can be universally
boundary network will

steel
from the solution
allowed precipitation
slow cooling
solution
by water quenching was sufficient
IF, and that slow cooling
to eliminate
IF
case, and reduced in the second.
0.06%Al and 0.016%N, and found that
containing
treatment
in oil,
(1960) repeated some of this work on a
Woodfine and Quarrell

steel
treatment
of Chemical Composition
of aluminium and nitrogen
contents
IF have already been discussed in Section 4.3.

,.
64
(1962) examined the influence
Wright and Quarrell
of carbon,
manganese, sulphur
and phosphorus on mechanical properties.
low carbon content
(0.12%) was found to favour a fibrous
fracture
high carbon contents were associated
mechanism, whilst
with cleavage failure.
It was only at intermediate
intergranular
that
carbon
fracture
(Section
matrix
failure
and a higher
is hard and brittle
fracture
strength
can again be interpreted
fibrous/intergranular
and reduction
Although little
effect
mode. A corresponding
of ductility
and Quarrell's
high
in
quality
whereas
observed.
to a mixed
increase
in tensile
was noted.
on fracture
behaviour,
and Wright
a paradox which had confused
for a number of years.

(often
from 0.50%
of phosphorus content was observed,
work resolved
Bessemer steels
effect
(1962) found that
mode changed from fibrous
influence
had
marked
a
sulphur
researchers
in terms of its
the manganese content of a 0.30%C steel

the fracture
to 2.14 n,
Wright and Quarrell
properties.
by increasing
frequently
In cases where the
predominates.
to IF, and this
strength
C, lower
(high C, or untempered) cleavage
Manganese was also found to have an effect
on matrix
favours
(higher
matrix
tends to promote IF.
tempering temperature)
matrix
low strength
(low carbon cf high tempering temperature)
ductile
of
of tempering
in that a relatively
4.3.1),
levels
was encountered.
This is in some ways analogous to the effects

temperature
This was the fact
high in nitrogen)
armour plate
rarely
steels
Wright and Quarrell's
that
exhibited
IF,
the phenomenon was

results
showed that
65
-
a high sulphur
content
could promote a premature ductile
This was the case with Bessemer steels.
the armour plate
intragranular
making
clean,
failure
boundary
grain
void nucleation
titanium
and zirconium
aluminium nitride
nitride
without
(1960) showed that both titanium
rise
giving
However, whereas titanium
aluminium for
on the grain boundaries.
additions
in
the presence of aluminium,
even
zirconium.
to replace
were found to prevent

this
IF
was not the case for
given by Woodfine and Quarrell
The explanation
was
decreases
of the oxides and nitrides
that since the stability
and
to IF, since both form stable
which do not precipitate
nitrides
and avoid
has been considered by several workers.
could be used successfully
deoxidation
and
forming elements such as
to combine with nitrogen
formation
Woodfine and Quarrell

zirconium
more difficult
more favourable.
correspondingly
The use of more powerful
In contrast,
low in sulphur and very
were invariably
steels
inclusions
at the sulphide
because of the ease of void nucleation

present.
failure
in the order Zr02, A1203, Ti021 ZrN, TiN, A1N, combined titanium
and aluminium additions
combined zirconium
formation
Baliktay
tend to give A1203 and TiN, whereas
and aluminium additions
of Zr021 leaving
the aluminium free to form A1N.
(1976) and Honer and Baliktay
that provided
in the
result
the deoxidants
(1978c) have pointed
are added in the correct
(i. e. Al added before Ti or Zr) a combined addition

beneficial.
be
can
elements
several
reducing
large
foundries
the occurrences
Indeed this
practice
sequence
of these
is adopted in
in the UK and has been successful

of IF
(Wilson,
1981).
out
in
However, many
66
foundries
smaller
access to vacuum degassing facilities
without
for deoxidation
have found that
the use of titanium
a 'dirty'
with poor upper shelf
steel
and are therefore
in
toughness properties,
to change their
reluctant
results
(Jackson,
practice.
1980).
Lorig and Elsea (1947) and Fremont
effect
(1962) found a beneficial

to IF, which they
of molybdenum on the susceptibility

to the retardation
attributed
and aluminium diffusion
of nitrogen
by the large Mo atoms in the matrix,
thus hindering
AMN
precipitation.
The effect
the literature,
refine
it
although
the primary
(unspecified)
quantities
because of the formation

It can also be anticipated
strength
will
strength
ratio,
Alloying
on properties
factors
(Lorig
elements can also influence

by their
Solute element interactions

Section 4.4.
grain
that elements which increase
size
effect
of this
the matrix
the grain boundary:
matrix
may outweigh this
also forms a stable nitride
of small
of NbC precipitates.
An example is boron which,
effect
For example Fremunt
which gave a fine
of niobium,
although other
strength,
in
reduce the susceptibility
of IF by the addition
promote IF by decreasing
contribution.
beneficial
will
the grain boundary area.
(1962) noted a suppression
defined
is to be expected that elements which
grain structure
to IF by increasing
matrix
elements is not clearly
of other alloying
despite
increasing
the
and can have a
and Elsea,
1947).
the precipitation
tenperature
on the solubility
product.
nature will
be considered
in
67
-
of AIN in Steel
The Solubility
4.4
4.4.1
In Austenite
investigations
Although several
y-iron
of the solubility
(Sieverts
have been reported
Fukusima 1939), the first
equilibrated
contents
with nitrogen
For a given temperature,
of the work to determine
was by Darken et al (1951).
workers determined the nitrogen

steels
1931 and 1938, Iwase and
extension
of AMNin steel
the solubility
nitrogen
found to be independent of the aluminium level
This rise was explained
Fig. 4.2).
formation
content
of A1N, and the solubility
determined from the position
of the absolute
content was
up to a critical
(See
rose abruptly.
as being due to the

product
(Ks) could be
against
The
the reciprocal
and gave the following
temperature
above 1000C.
of the break in the curve.
values of Ks thus found were plotted
These
of aluminium-killed
gas at temperatures
the equilibrium
amount, whereupon the nitrogen
in
of nitrogen
empirical
relationship:
7400
[MRN3
log10
1.95
Numerous subsequent investigations*

similar
slopes,
but with
Pickering
have predicted
equations with
lower values of the constant
See, for example, Leslie

Pehlke and Elliot
(4.1)
(1960)
et al (1954), Pearson and Ende (1953) ,

Erasmus and blech (1964),
,
and Gladman (1967), Hner and Baliktay
(1961).
Knig
et
al
and
Thus,
teen.
Irvine,
(1978a)
68
-
equation
(4.1)
represents
an upper limit
To take these factors
log10 Kapp _
into
account,
-6770
T
they predicted
an "apparent
(4.2)
technique were discounted by
as a reason for the discrepancies

since it
product,
solubility
conditions.
1.03
Inadequacies in the analysis

et al
of equilibrium
(Kapp), given by
product"
solubility
Leslie
et al (1954) in terms of
by Leslie
and the slow attainment
segregation
This,
is interesting
However, it
investigations,
in certain
derived
_
Table 4.1 presents
(4.1)
subsequent
and it
the
has
the Beeghly method
describes
together-with
their
data
own results
product
for a
given by
(4.3)
+ 1.48
some of the empirical
the solubility
been assumed.
the solubility
a "mean" solubility
7500
NA1N.
of the %Nas A1N (see Section 4.2.1).
(1967) collated
and using this,
[Al][N]
log10
circumstances
than has previously
Gladman and Pickering
0.1%C steel,
all
determinations,
be
that equation
could
product more closely
available
since Nsol = Ntotal-
to note that unlike
in overestimations
it
in an
the work of Darken et al did not utilise
been
shown that
since
Therefore
product,
Beeghly method for the solubility
can result
the Beeghly
they reasoned, would result
in solubility
apparent increase
in measured
that
was considered
technique would tend to underestimate

present as A1N.
of
The reasons for the differences
AMNwhich can be expected.

have been interpreted
to the solubility
equations
together
with
69
the relative
0. l%Al and 0.0l-, N.
containing
for a steel
temperature predicted
solution
It
can be seen that this
temperature
by
is
by
200C,
no means obvious when
as
which
as
much
can vary
the data are presented
A more satisfactory
as in Fig. 4.3.
graphically
that used by Gladman and Mclvor (1972).

contents
aluminium and nitrogen
Fig.
a given temperature.
of a steel
the
which are soluble
account the higher
at
solubility
aluminium contents
encountered in cast steels.
frequently
In Liquid
Steel
state has not been thoroughly
The solubility
of AMNin the liquid
investigated,
but Honer and Baliktay
(1978a) found a similar
dependence to that obtained
temperature
austenite
This relates
4.4 shows an example of this
diagram extended to take into
4.4.2
data is
the solubility
method of presenting
(see Fig.
4.3).
0.8oNh they obtained
for the solubility
For a GS-60 steel
the following
relation
containing
in
0.40%C,
in the range
1550-1750C
CA13M
log10
2.37
+
-88490
Solute Interactions
4.4.3
The presence of alloying

alter
the solubility
actions.
steel
(4.4)
The effects
elements in austenite
of AIN quite
significantly
on the solubility
have been shown schematically
or liquid
by solute
of nitrogen
in Fig.
steel
inter-
in liquid
2.5, and interaction
can
70
-
have been evaluated by a number of workers. *
coefficients
The effects
but what data are available
been determined extensively,

listed
of Al have not
elements on the solubility
of alloying
are
in Tables 4.2 and 4.3.
in liquid
These give values of eN" and eM"

logfN
for
%x -} 0
and in austenite, where eN" =
0
steel
fN is the activity
positive
for N.
coefficient
Elements with
thus tend to decrease the
interaction
coefficient
correlation
has been established
solubility.
A useful
in situations
(1968) for nitrogen

in austenite
is not known.
is an empirical
in liquid
iron
relation
by Nbri and Ichise
where the interaction
This makes use of the fact
between interaction
and in austenite,
which can be represented

(4.5)
(160000)-0.016
(1000C)=3.1
eNX
eNX
(4.6)
thus:
Temperature of Precipitation
Under isothermal
conditions,
of precipitation
from supersaturated
the precipitation
high
is
temperatures,
slow
at
rate
mediate temperatures
(C-curve behaviour).
there
of AIN
Precipitation
4.5.1
that
parameters of nitrogen
(16000Q
(1200C)=1.9
eN"
eNX
-0.005
4.5
coefficient
solid
of A1N is typical
solutions
in that
the
reaches a maximum at inter-
and decreases again at lower temperatures

Leslie
et al (1954) determined the maximum
For example, Pehlke and Elliott
(1960), Schenck et al (1958),
Schumann and Kunze (1967) , Uda and Pehlke (1974), Maekawa and
(1968),
(1964),
Gomersall
(1959),
Pehlke
Evans and
et al
Nakagawa
Leewis and Maclean (1979), Wada and Pehlke (1978).
71
-
has
been
800C,
be
this
to
since
about
and
at
rate
.
precipitation
by other
confirmed
Wertebach
(1964),
However,
workers
(Wiester
and Hoff
(1958)).
precipitation
phenomena in cast
precipitation
does not
since
castings
Secondly,
steels
cool
usually
(low)
by
them.
ones examined
these elements
present
and hence the A1N will
contents
to 0.10%A1,0.010oN)
of any micro-
effects
exist,
Therefore
place
rate
contents
to
to the
in the amounts of
temperature,
at a correspondingly
cooling.
for
the aluminium
in a casting
and nitrogen
(typically
up
at which a component becomes
the temperature
This
ignores
also
the
of Al and N which may
or macro-segregation
which would tend to increase
in enriched
hours or even days.
the solubility
may be in excess of 1350C.
insoluble
conditions,
and nitrogen
to precipitate
to be encountered
likely
Firstly,
two reasons.
any increase
4.4 shows that
to Fig.
Reference
for
et al can only be applied
increase
begin
to explain
such results
over several
aluminium
will
Takei et al
under isothermal
slowly
Clearly
during
temperature
steels
of Leslie
similar
to apply
take place
the results
with
higher
et al
would be inappropriate
it
(1957),
the precipitation
temperature
areas.
it
can be expected
that
in the upper range of the austenite

is slow enough.
Kowalowka (1978)
precipitation
suggest
that
may take place
As described earlier,
in the liquid
Indeed,
Barron
for
of A1N may take
precipitation
region,
(1974)
if
the cooling
and lojecki
and
high Al and N contents
in the liquid
the precipitation
during
solidification.
form
in
A1N
a
random
of
has been cited by Woodfine and Quarrell
(1960) to
72
-
why castings
explain
do not
with very high Al contents often
show IF.
4.5.2
Morphology
Precipitate
Lorig and Elsea (1947) were the first
forms, although the low resolving
idiomorphic
in
two
occur
microscope they used meant that
of the optical
to distinguish
between the two.
clearly
A1N on fracture
when they identified
(Figs.
and dendrites,
distinguish
to
was made
into
growing
the grains with
techniques
in the form of
However, no attempt
between the precipitation
at the original
between the arms.
surfaces
conditions
under
It was found that the majority
were of the dendritic
of the precipitates
have nucleated
Wright and Quarrell
4.5 and 4.6).
had
these
occurred.
of
each
which
power
they were unable
the problem by using microfractographic
(1962) resolved
plates
to suggest that AIN could
kind,
and appeared to
grain boundaries,
austenitic
a crystallographic
In most cases, the dendrites
relationship
appeared
asynnnetric, with secondary arms growing from only one side of the
arm.
primary
Thus it
was implied
in
the solid
taking
place
was
to be possible
in certain
annealing
(Bainbridge,
(Stickler
and Vinckier,
the extensive
It
is,
therefore,
dendritic
1961 and Wilson,
unclear
precipitates
that precipitation
precipitation
this
during
1972) and for some carbides
of small,
typical
arrays
Although
state.
Cu and Ti alloys
in the formation
resulted
that dendritic
isothermal
in steel
1971) these systems
ill-defined
dendrites
and not
of the AIR precipitate.
at what stage of primary
form.
has been shown
cooling
the
Most workers seem to have assumed
occurs in the solid
state,
because this
is the-
73
from steels
experience
where only small amounts of Al are added

It has already been shown, however, that
for grain refinement.

solution
found in cast steels

the effects
higher,
are considerably
of microsegregation,
precipitation
The dendrites
of AUN are much finer
(Stachura,
the fracture
surfaces
(Fig.
This compares to typical
like
form of the mitride
fractographs
that
arm
the morphology
clearly
show regions where it

between dendritic
merely to result
of the arms of certain

and it
dendrite
1976).
Indeed Stachura (1980) considers
particles.
precipitates
(1962) gives X -1um
and
grain boundary on which the particles
of the austenite
to distinguish
difficult
spacing on
is determined by the substructure
of the A1N precipitates
Some of their
to promote
1969,1971,1977).
solidification
Altmann et al (1965) were of the opinion
grow.
a=
of Wright and Quarrell
(Edvardson
20-200pm
et al,
of
spacings
orientation
with
than the solidification
and measurement of the dendrite
4.5).
and together
may be sufficient
this
structure,
to be
for the amounts of JUN likely
temperatures
favourably
may be that
is
and platethe plate-like
from growth and coarsening
orientated
dendritic
there is no clear
distinction
between the two forms.

4.6
Other PhenomenaAttributable
4.6.1
Grain Growth Inhibition
In a pure metal,
where the grain
temperature.
grain
growth is a thermally
size developed is a function
Grain boundary mobility
by the presence of a fine,

Halley
to A1N Precipitation
(1946) noted that
activated
process
of time and
may be reduced significantly
randomly dispersed precipitate.

the additon
of 0.03%A1 to steel
increased
74
the temperature
is found with
effect
of A. N.
to the precipitation
this was attributed

A similar
(G. C.T. ), and
at which grain coarsening occurred
but whereas further
the GGT, with
(1957) suggested that
this was because at higher Al contents A1N precipitates

and in a coarser dispersion,
temperatures
making it
at higher
less effective
the grain boundaries.
at pinning
Thus Al is frequently
fine
a
promotes
boundaries
added to wrought steels
in amounts<0.04%oA1
of AIN during cooling.
dispersion
to form a fine
4.6.2
4.7),
aluminium a subsequent
and Leslie
Rickett
decrease was noted.
(Fig.
and zirconium
of these elements beyond 0.03%
additions
continued to increase
titanium
grain size by pinning
This then
the austenite
grain
effectively.
Impaired Hot Ductility
This is normally
in two different
manifest
has been cited
precipitation
ways, and A1N
as a cause of both.
(Reynolds and
Gladman, 1979).
Ingot Panel Cracking
4.6.2.1
These longitudinal
steel
ingots
and steels
too frequently
cracks all
during cooling
or on charging
to the soaking pits,
in the range 0.4-0.7%C are particularly
(Nagger, 1975).
Irvine
and Pickering
intergranular,
is
path
crack
boundaries,
and it
of internal
thermal stresses
ingot
appear in Al-treated
the prior
cracking
set up during
in the range 600-800C.
A1N
precipitates
at
crack
a
(1957) showed that
following
is thought that
susceptible
austenite
grain
occurs as a result
the cooling
These may be sufficient
in the prior
the
austenite
of the
to nucleate
grain
75
boundaries.
This crack can then readily

ferrite
pro-eutectoid
network.
Desai (1959) found that the hot tensile
of uncracked
can be achieved by the addition
of ingot panel cracking
of
to ingots which are to be cooled through the susceptible
titanium
temperature
range, and by ensuring
that
ingots which are to be

furnace before the
at once are charged to the reheating
temperature
falls
range (Jackson, 1978).
this
within
Surface Break-up During Hot Working
4.6.2.2
This can occur during either

has been associated
with
identification
case
each
a lowering
or rolling
operations
of hot ductility
of the high temperature
structure
in making direct
which transforms
However, recent work by Funnell
on an austenitic
alloy
role
away from developing
There will
ductility.
has shown the mobility
to play an important
able to migrate
obviously
the initial
grain
and Davies (1978)
of the grain
since the boundaries must be

cavities
be a critical
boundary
migration
grain
which
size above
to be a function
In
of the mechanism by which A1N affects
during cooling.
boundaries
and
caused
1979).
has been hindered by difficulties
hot ductility
observations
forging
(Erasmus, 1964 and Funnell,
by AIN precipitation
likely
and that
were associated with higher Al and N contents.
the latter
rolled
ductility
at 600-700C than for cracked ingots,
ingots was greater
Control
propagate through the
to promote good
AiN particle
can occur and this
of the volume fraction
of precipitate,
size and the stored energy of deformation.
is
76
Chapter 5
Experimental
5.1
Work
Introduction
The aims of the experimental

information
program w were to obtain more detailed
the mechanism of AMN-induced T. F.,
regarding
the AMNprecipitation
for the two forms of
phenomena responsible
precipitate
observed by Wright and Quarrell
the effects
of T. F. on mechanical properties.
chosen for the experimental
The steel
0.30%C, 1.50 Nh.
containing
for general applications
track
assembly items,
is widely
where shock resistance,

in thin
section
used in industry
strength
castings
and
such as
mine car wheels and earth moving equipment.
It has also been shown to be particularly

problems associated
(1962) and to examine
work was BS 3100 A5/6 (1976)
This alloy
are important
wear resistance
to study
with
I. F. (Lorig
susceptible
and Elsea,
1947;
to cracking
Wright
and
1962).
Quarrell,
10kg induction
Initially,
melted castings
which were high in Al
and N were used to study the mechanism of I. F. in samples which

were broken by slow three-point
variables
processing
treatment
control
such as pouring
determined.
also
were
solidification
bending.
temperature
Subsequently,
work was undertaken.
of solidification
The effects
of some
and heat
directional
This facilitated
closer
parameters and the samples produced
were used to examine the A1N precipitation
phenomenon in more
detail.
Quantitative
information
regarding
the effects
of I. F. on
77
-
mechanical properties
toughness (C. O.D. ) data for embrittled
and fracture
and non-
steels.
embrittled
this work are already well-
The techniques used throughout

developed, and therefore
5.2
Production
All
the steels
have been described only briefly.

Melts
of Experimental
used in this work were air-induction
one of the three practices
melted using
below.
outlined
Practice
Melting
Charpy impact
was obtained using tensile,
frequency induction
12kg Radyne variable
unit:
furnace.
MgO
Lining:
'Armco' iron punchings
Base charge:
Alloying
additions:
white iron
(4.2%C)
Si metal
Mn flake
5% N/Mi flake
Al rod (99% purity)
75m square C02/sand moulds, nominal capacity
bbulds :
Exothermic powder:
Melting
Foseco 'Feedex 3'

The base charge was melted at 28kWpower, and
details:
when fully
10kg
molten,
the additions
in
that order.
made
were
manganese
of white iron,
silicon
When the desired
and
casting
temperature was achieved (measured using a Pt/Pt-13%Ph thermocouple)

the additions
by
immersion into
N2/Mn
Al
were
made
of
and
The melt was poured directly
into
exothermic powder was transferred

immediately
after
casting.
the mould and after

to a sand pit
the bath.
adding the
buried
and
This gave a slower cooling
rate than
78
have been attainable,
would otherwise
formation
casting
of A1N.
The cooling
thereby promoting the
rate at the centre of a typical
was monitored using a Pt/Pt-13%Rh thermocouple connected
to a 'Servoscribe'
chart
recorder
and was found to have a mean
value of 0.1C sec-1 in the range 1100C-800C.
Castings were
over a period of -.24hrs
allowed to cool to room temperature
before being removed from the moulds.

Practice
belting
unit:
Lining:
70kg Birlec
medium frequency induction
MgO
'Armcol iron billet
Base Charge:
and punchings
As for Practice
Alloying
additions:
Moulds:
12.5kg C02/sand keel blocks
details:
As for Practice
was poured into
a preheated ladle
An allowance of 30C was made for

bath and ladle.
'A'
Foseco 'Feedex 3'
Exothermic powder:
Melting
furnace.
'A',
except that
containing
the melt
the Al additions.
the temperature
Each 55kg melt produced sufficient
drop between
molten steel
for four keel blocks.

Practice
Melting
unit:
Lining:
furnace located
at SCRATA.
Low carbon 'coffin'
scrap
MgO
Base charge:
Alloying
180kg APV Paralec medium frequency induction
additions:
White iron,
FeSi, High C-Febh, 5%N-FeMn,
Al bar C98%Al)
bbulds :
100irmisquare C02/sand moulds
Exotherrii. c powder:
Melting
details:
Foseco 'Ferrux
As for Practice
16'
'B'.
79
-
5.3, Chemical Analysis

Full
body
from
the
the
casting
taken
of
samples
Carbon and sulphur
feeder head).
positions
minimise the effects

Full
details
were determined by
levels
across the section
technique
for analysis
Drillings
content
nitrogen
vacuum fusion
by the Feichtinger
LECO
gas analyser.
a
using
or
at various
(i. e. not from the
(LECO). The total
oxygen combustion techniques

was measured either
out on
of each cast was carried
analysis
spectrographic
were taken
of the casting
to
of segregation.
of each casting
used in this work can be found in
Table 5.1.
5.4
a)
Heat Treatment
The castings
furnace after
in a muffle
treatments
to typical
were subjected
where necessary.
and sectioning,
samples were water quenched after
commercial heat
removal of the feeder heads
Care was taken to ensure that

tempering treatments
to avoid
temper embrittlement.
b)
High temperature heat treatments
wound vacuum resistance

or oxidation
solution
furnaces
of the surface.
treated
present
by Lorig
to avoid excessive
Samples from selected
for times between ihr
1350C before being either

The aim of this
were performed in platinum-
part
casts were
and 24hrs at 1250C and
water quenched or furnace cooled.
A1N
determine
the
to
the
whether
was
work
of
be
re-dissolved
could
castings
Q,ua.R2l,
(1960).
(1947)
Woodfine
Elsea
and
and
in embrittled
decarburisation
as reported
80
5.5
Mechanical Testing
5.5.1
Hardness Measurements
Vickers pyramidal
diamond hardness measurements were made on

ground on 600-grade
freshly
had
been
samples whose surface
cases, the hardness recorded was the average
In all
emery paper.
impressions.
three
separate
of
5.5.2
Three-point
In the preliminary
Bend Testing
it
subsequent
occasions
on
some
and
work
fracture
determine
the
to
was necessary
for extensive
Samples of approximately
sample preparation.
25mmx 150mmwere cold sawn from the appropriate

heat treated
layers
as necessary.
by a linishing
After
operation,
castings
removing any surface
testing
machine.
they were placed in a desiccator
25mmx
and
oxide
the samples were saw-notched
to a depth of -.5mmand broken by slow three point

Denison hydraulic
the requirement
mode without
Immediately
bending in a
after
fracture,
to await fractographic
examination.
5.5.3
Tensile
Testing
Room temperature
tensile
tests
were carried
(1971)
2
Part
18
BS
using cylindrical
with
cross sectional
area and gauge length
servo-hydraulic
testing
out in accordance
samples of 150mm2
5.65vSo on a Dartec
machine under displacement
In the case of the square castings,

from
the columnar regions
machined
the tensile
control.
samples were
to minimise the effects
of
porosity.
Low temperature
tests were performed on the same equipment fitted
with an environmental
chamber.
Cooling was effected
using a
81
fine
spray of liquid
fan.
an electric
to within
nitrogen,
In this
circulated
way, the temperature was held constant
+3C for 20 minutes prior
High temperature
tensile
the chamber by
within
testing
to testing.
out in accordance
was carried
with BS 3688 Part 1 (1963) using samples with a cross sectional

area of 100mm2. These were soaked for 30 minutes in a resistanceheated environmental
+2C) prior
automatically
chamber at temperature
Load/extension
to testing.
using the read-out
(measured to within
curves were plotted
from a Baldwin high temperature
extensometer.
5.5.4
Impact Testing
The main progrannne of mechanical testing
Samples were cold sawn from the columnar
V-notch impact test.

regions of test
orientation
castings
prior
to heat treatment.
of the samples is shown in Fig.
seen that the notches were positioned

proceed parallel
finish
The
5.1 and it
can be
to allow fracture
to the long axis of the columnar grains.
this way any orientation

After
employed the Charpy
effects
using the techniques
In
were minimised.
machining the samples were tested
BS 131 Part 2 (1972).
to
The soaking temperatures
in accordance with
were attained
shown in Table 5.2 and a soaking time of
15 minutes at temperature was used throughout.
82
Table '5.2
The media used to obtain
for Charpy samples.
soaking temperatures
Medium
Temperature Range
Liquid
-196C
Nitrogen
-164C to -60C
Isopentane/liquid
20C
to
-60C
Methyl alcohol/solid
20C to 150C
Thermostatically
bath
Air muffle
>150C
nitrogen
C02
controlled
oil
furnace
Clearly
least
the method used for the high temperature

accurate
in terms of temperature
it was the fracture
during
regime
value of impact
Hence the variations
the transfer
was the
but in this
control,
mechanism and not the absolute
importance.
was
of
which
energy
temperature arising
tests
in
of the sample from the
furnace to the Charpy machine could be tolerated.

Because of the complex nature of some of the fracture
measurements of the
I. F. were made by photographing
specimens, cutting
out the appropriate
balance.
accurate
The effects
photographic
% I. F. projected
areas and weighing on an
of density
however, that
this
onto a two dimensional
account the effects
introduced
the broken
differences
of the
paper were measured and were found to be negligible.
It should be noted,
into
surfaces,
because of this
of surface
technique measures the

surface
relief.
are considered
and does not take
The inaccuracies
to be small.
83
5.5.5
Toughness Testing
Fracture
Samples of the 0.300-1.5ONh steel
For each case, steels
condition.
and an uaembrittled
for lhr,
J. Q. ) and the normalised
cooled).
Because of the excessive

Kic results
were tested
(950C for l11hrs, W.Q.; 600C
in the quenched and tempered state
to obtain valid
in an embrittled
were tested
state
(950C for lhr,
size requirements
for this
air
necessary
(Appendix la),
material,
the fracture
toughness parameter measured was the crack opening
displacement
(C. O.D. ).
it was intended to use small keel block castings
Initially,
by Practice
(Section
'B'
fast
of the relatively
5.2) throughout
cooling
it was not possible
keels,
rates
this work, but because
in the body of these small
to produce a fully
intergranular
fracture,
even with high aluminium and nitrogen
46/5-7).
Consequently,
surfaces
at room temperature
Note that
5.2.
colwmar
fully
intergranular
in the heat treated
Pre-fatiguing
the square castings
to minimise the effects
regions
of the test
servo-hydraulic
chamber.
(Fig.
Testing
testing
5.3).
fracture
condition.
is shown in
were sampled. from the

of porosity.
specimens was carried
(1979)
BS-5762
using an Amsler vibrophore
with
dynamometer.
2t
a
(Casts
Because of the significantly
of the samples taken from the castings
The position
Fig.
'C'.
these exhibited
rate,
contents
four 100mmsquare ingots high in Al and
N were produced using Practice

slower cooling
made
out in accordance
machine fitted
with
took place at SCRATAusing the Dartec
machine fitted
This utilised
with
a fine
an environmental
thermostatically,,
84
controlled
spray of liquid
circulated
and a heating
testing,
low temperature
nitrogen
the fan) for high temperature
by a fan for the
element (again assisted
In this way the temperature
testing.
from -190C to +150C, calibrated
could be varied
by
to an accuracy
of +3C.
During the tests,
displacement
the machine was operated automatically
control
at a ram speed of 0.033mms-1.
was monitored using the double clip
(1980).
Fig.
Crack opening
gauge (DCG) technique
has been described by Veerman and Muller

(1977) and El-Soudani
in
which
(1972), Selby and Danson
This is shown schematically
in
5.4.
Two simultaneous
(a)
load vs clip
(b)
clip
gauge displacement
gauge displacement
were obtained
By considering
that if
of
plots
(Vl) vs clip
edges.
COD, then the
magnitudes of the two clip

at each set of knife-edges
between the apparent centre of rotation

In the initial
elastically
loaded regime,
is stationary
V1 vs V2 is obtained.
However, the development of a plastic
effective
(V2)
can be seen
the centre of rotation
or a crack tip
and
of the specimen must also move forward.
since the displacement
depends on the distance
5.4) it
moves forward at a constant
is a change in the relative
knife
the
and
gauge displacement
the geometry of the system (Fig.
apparent centre of rotation
gauge signals,
by BS 5447)
for each test.
the crack front
The result
(as required
opening displacement
and a straight
constitutes
crack length which gives rise
centre of rotation.
This is manifest
line
plot
of
zone
a change in the
to a movement of the apparent
on the V1/V2 plot
as a
85
-
fraction
becomes a larger
of V2 as a result
events in the fracture
Significant
the DCG plot
and related
displacement
curve.
on the fracture
By correlating
Metallographic
by grinding,
to calculate
appropriate
in Appendix lb.
Techniques
the cast structure,
and etching was carried

solution.
ammoniumchloride
using a neutral
out in acidic
depositing
higher
concentrations
remained for up to 8 hours.
15%HC1,where it
dendritic
structure
etching
characteristics
Optical
After
samples were machined flat
of the casting
copper
a layer
the sample was transferred
solution,
progressively
containing
of copper
into
baths
of HC1, up to
In this way, the
is revealed by the differential
of microsegregated
regions.
Microscopy
Samples were prepared in the usual way, by polishing

finer
features
with
Macroscopic
In order to reveal
5.6.2
on the load/
position
these points
it was possible
the CODdata is presented
5.6.1
process were determined on
to the relative
surface
of the crack movement.
An example of the complete procedure for obtaining
CODvalues.
5.6
since the displacement Vl
towards the Vl axis,
displacement
on successively
grades of emery papers and diamond wheels to a finish
In cases where the metallographic

heat
treatment
of
of 0.25um.
work was to check the effects
on the microstructure,
a solution
of 2% Nital
was used as the etchant.

However, when the object
at the prior
austenite
was to observe the precipitates

grain boundaries
of the commonly available
it
of AMN
was found that none
by
Lorig
those
suggested
etchants nor
86
(1960) and Mahmoud(1974)
Quarrell
Woodfine
(1947),
Elsea
and
and
highlighted
they
merely
since
was suitable,
features
present
was to hinder
the microstructural
Indeed, the tendency
at the time of examination.
The most satisfactory
of the A1N.
observations
technique for cases where the AIN was thick
enough to be resolved
finish
with a suspension of
to a 0.05um
was to polish
optically
high
in
to
magnification.
unetched
at
examine
water and
y-A1203
The initial
of JN on each sample was often
observation
but once a line
had been observed, the whole of the
of precipitates
merely by following
be traversed
sample could readily
difficult,
the network
boundary
particles.
of grain
The instrwnent
fitted
Microscopy
Scanning Electron
5.6.3
with
used primarily
examination
backscattered
dispersive
LINK
energy
a
of fracture
electron
imaging and contrast
of the technique
Transmission
fracture
mode for the

such as
enhancement were
goniometer specimen stage,
adopted will
be presented
surfaces.
in Section 6.2.1.
Microscopy
replicas
taken from intergranular
because
SEM
the
of.
to
work
supplement
surfaces was used
the improved resolution

identify
This was
to examine the angular relationships
Electron
Examination of extraction
PSEM500
microsections.
value was the eucentric
between some of the features
5.6.4
system.
but other techniques
surfaces,
which was used extensively
Details
analysis
at 25kV in the secondary electron
employed to observe polished

Of particular
this work was a Philips
used throughout
A1N precipitates
of this
technique,
by electron
and the ability
diffraction.
to t,
87
used for the majority
The instrument
of the work was a Philips
51301 TEN operated at 100kV, but at a late

a Philips
EM400T fitted
a STEMattachment and EDAXanalysis
with
became available.
facilities
out using this
A limited
Two-stage extraction
by two methods
replicas.
This technique was used in situations
'Fonnvar'
wetting
the fracture
Formvar was placed on the fracture
to be stripped
the film
unit.
The plastic
replica
surface
and coated with
in an Edwards carbon
was then cut into
small squares,
2mm
x
-2mm
in size which were placed on 200-mesh copper grids with

layer
By suspending these grids
uppermost.
bath
of acetone, the plastic
a
of
period
of several
hours leaving
the
surface with acetone,
had hardened sufficiently
away from the fracture
evaporation
size and softened
and allowed to assume its
of carbon (-20nm thick)
layer
a thin
2-3 hours,
After
topography.
A piece of 100um
sheet was cut to an appropriate
After
in acetone.
where severe degradation
surface was to be avoided.
of the fracture
thick
amount of work was carried
equipment.
Samples were prepared for examination

(a)
stage of the project
just
was dissolved
the carbon
above the surface

away slowly
behind the carbon replica
over a
on the
copper grid.
(b)
Direct
carbon extraction.
Although the technique

good quality
it
does result
attack
replicas
of direct
with
the efficient
in a degradation
by the acid.
extraction
was found to produce
extraction
of the fracture
of precipitates,
surface
due to
88
Within
minutes of fracturing,
thirty
20nm thick
of carbon approximately
onto the fracture
directly
evaporated
was
an Edwards carbon evaporation

5x
a layer
in
surface
operated at a pressure of
unit
10-5 Torr.
of the area of interest,
With the exception

with
'Lacomit'
compound to prevent
stopping-off
It was then marked into
extraction.
using a solution
of 5% bromine in anhydrous ethyl
in
methylated
washed
and
water
boundary
from an embrittled
in 2% Nital
and disks
network,
emery paper
perchloric
5.6.5
followed
acid
Electron
5.6.5.1
using
were spark
by mechanically
Probe Microanalysis
from the
wheel.
of the prior
by a ferrite
machined
from
polishing
'Tenupol'
on
of
10%
unit.
(EPMA)
Specimen Preparation
Samples were mounted in a conducting bakelite

to the procedures outlined
features.
were
11-2nm thick
in a solution
in a Struers
alcohol
taken
the position
by electro-polishing
attempts
a diamond cutting
which were delineated
diameter
in
-3mm
in ethyl
foils
Slices
samples.
revealed
These were thinned
these areas.
surfaces,
in thin
casting
solution
boundaries
grain
austenite
of fracture
of as-cast
regions
the sample in distilled
in the microscope.
the A1N precipitates
made to observe
for
alcohol
before being caught on a
spirit
to the examination
In addition
off
for examination
200-mesh copper grid
Etching
small squares with a scalpel.
The carbon was floated
2-10 minutes.
were cut
any unwanted
of the sample was etched away through the carbon layer
The matrix
grain
the sample was coated
in Section
Regions of interest
within
5.6.2
resin
and subjected
to observe the required
the specimens were selected
89
-
indentation
by
marked
and
on a Leitz
microhardness tester
using
a 400g load.
The samples were then repolished
etchant
finish
the
and
by polishing
5.6.5.2
to remove all
signs of the
necessary for microanalysis
was reached
on 0.05}un y -A'203'
Analysis
The experiments were carried

using standard techniques
out on a Cambridge Microscan Mk 5,
and an accelerating
In order to measure the extent

experimentally
of microsegregation
melted 75mmsquare castings,
was used and the output

pen chart recorder.
potential
of 15kV.
of Al in the
a scan speed of 0.16iuns-1
from the ratemeter was recorded on a three-
Prior
to and after
each specimen was analysed,
20-second counts were taken on an aluminium standard,
and at the
background
Al count was made.
scan
a
end of each
The count rates of each scan were converted
aluminium using a 'Sheffield
corrects
for atomic number, absorption
The instrument
analysis
and fluorescence
effects.
mode for the qualitative
found in some of the heat treated
Using a low atomic number detector
analyse for nitrogen,

SEMfacility
computer program, which
was also used in the 'spot'
of JUN precipitates
samples.
it was possible
to
which is not detected by the energy dispersive
because of atomic number limitations.
low peak/background ratios

used.
Frame Three'
to weight percent
encountered,
counting
Because of the
times of 200s were
-9a5.7
The technique of directional

closer
exercise
control
mechanism.
was used in order to
solidification
parameters and to
of solidification
a more detailed
facilitate
(D. S. ) Technique
Solidification
Directional
investigation
Small samples of material
of the A1N precipitation

were remelted under an inert
atmosphere of argon and could be quenched from high temperatures.

In this way it
originating
from the fully

regions
resolidified
The two compositions
in one sample structures
to obtain
was possible
liquid,
partially
of the steel.
selected
for this
part
of the work were cast
4282 (0.08%oAl, 0.014%N) which was not susceptible

cast 4283 (0.17oA1,0.017oN)
samples approximately
by the progressive
and fully
solid
to I. F., and
Cylindrical
which was susceptible.
200m long and 5m in diameter were prepared
extrusion,
cold swageing and grinding
of the
75mmsquare castings.
5.7.1
Details
of the specimen assembly
Each sample was ground on a linishing

into
wheel until
it
could be inserted
a 400imnlong Degussit Alumina tube of 8mmo. d.,
was closed at one end.
5mmi. d. which
This tube was then fixed with
cement to a 360mmlength
'Autostik'
of 6mmo. d. , 5mmi. d. stainless
steel
tubing which had one end reduced to 4.9mm o. d. to accommodate the

tube.
The top end of the tube was screwed into
by
flexible
connected
a
was
which
steel
a brass holder
wire to the driving
This was capable of speeds between 0.005mms-1 and 5nuns-l.

of a port
maintained
in the stainless
steel
unit.
By means
tube an atmosphere of argon was
over the specimen during each experiment.
is
in
Fig.
the
specimen
assembly
shown
of
view
5.5.
A schematic
91
-
Apparatus
The Solidification
5.7.2
designed by
The apparatus used in the present work was originally

(1976) to study the solidification
Eruslu
steel,
stainless
(1981).
Bridge
and was later

Fig.
sequence of austenitic
by Pereira
modified
5.6 gives a general view of the equipment.
A Radyne 10kW high frequency power unit with

was used to provide
keep oxidation
service
heads providing
A graphite
16mmi. d. was placed inside

5.5) and aligned with
(see Fig.
To facilitate
stabiliser
In order to
tube was secured around the
to a minimum, a silica
atmosphere of argon.
25mmo. d.,
a voltage
the heat necessary for melting.
specimen assembly with

inert
(1979) and
coolant
and an
of length
susceptor
the cast alumina insulator
the work coil.
easy quenching the vertical
method of growth was
be
dropped
to
specimens
allowed
under gravity
chosen which
an agitated
releasing
5.7.3
time,
into
the
head was opened and the specimen was quenched by
the supporting
wire for the specimen assembly.
Measurement of the Temperature Gradient
Experiments were carried

partially
At an appropriate
quench tank of water.
bottom service
200mm,
slit
along its
out using a dummyspecimen which had been

length
to incorporate
a thermocouple.
A 0.2mm Pt/Pt-13%Rh thermocouple threaded through 1.2mn o. d.

twin bore recrystallised
alumina tubing was used for this
The thermocouple bead was protected

length,
1.8mm o. d. single
by inserting
bore recrystallised
fired
CC60
alumina
cement
using
sealed
was
found, however, that even with
thermocouples at temperatures
it
into
purpose.
a 5mn
alumina tube which

at 1500C.
these precautions,
It was
the life
of the
in excess of 1550C was very short
92
owing to attack
the temperature
evaluate
directly
gradients
but these were
owing to the premature failure
unsuccessful
The technique which was finally
thermocouple was stable,
at a temperature where the
coil
and to measure the temperature
for the power inputs
The thermocouple life
of the thermocouples.
used was to determine the position
induction
hot
the
the
of
zone
of
point
Several attempts were made to
by the molten metal.
used in the actual
was sufficient
at that
quenching experiments.
for this
to be carried
out
satisfactorily.
In this way
during
was measured, and an approximate temperature
the tests
could be calculated
gradient
examinations
metallographic
attained
on the basis of subsequent

of the test
piece.
Procedure
A Typical
5.7.4
the maximumtemperature
Having placed the specimen assembly into

dried
high
and
sealed
purity
was
system
the silica
tube,
the
argon was allowed to
flow through the furnace for twenty minutes in order to replace

Before the power was supplied,
the air within
the system.
drive
specimen
unit was switched on and the specimen assembly
positioned
solid/liquid
at least
so that
the
50mmof the sample would be below the
interface.
The furnace was switched on and the specimen allowed to heat up

to avoid refractory
slowly
final
input
power
starting
cracking.
of 0.89kIV normally
This heating
lasted
process to a
about an hour.
Before
the run, the specimen was held steady for ten minutes
at temperature
after
which it was driven
furnace at a rate of 0.033mms-1.
After
downwards through the

the sample had moved
by 70-100ngn, the wire was cut and the sample quenched.
93
Specimen Examination
5.7.5
In order to obtain
material,
solidified
of 10mmalong their
fracture
surfaces
from the directionally
samples were saw-notched lightly

length,
and were broken with
blow at each notch in turn.
The resulting
at intervals
a single
fractures
hammer
were
examined in the SEMfor any evidence of AIN precipitation.

It
was necessary
of observing
5.8
to adopt
approach because of the difficulties
this
AMN in microsections.
Industrial
Examinations
During the course of this

problems with
work, several
T. F. and short
foundries
term investigations
out under the auspices of S. C. R.A. T. A.

involved
technical
visits
personnel,
metallographic
reports
to the foundries
are included
have been carried
These investigations
concerned for discussions
the sampling of embrittled
examinations
have encountered
in the laboratory.
in Appendices 2 and
castings,
with
and
Two typical
3.
15
3
. r'...
,r
-946
Chapter
Results
6.1
The ? chanism of A1N-induced Intergranular
room temperature intergranular
A macroscopic view of a typical

fracture
is shown in Fig.
surface
bend testing
slow three-point
Fracture
6.1.
This was obtained by the
of a quenched and tempered sample
taken from cast 4176 which contained 0.18%A1 and 0.015%N.
grain boundaries of the
had taken place around the large as-cast
brittle.
scale
appeared
a
macroscopic
sample and on
under a binocular
and occasional
some relief
exhibited
from features
seen arising
These are, however, similar

when suitably
For certain
'families'
reflecting
of parallel
orientation
some crystallographic
an observation
which will
to those seen optically.
Fig.
showing the presence of several

crystallographically
magnifications
to flat
(Fig.
plate-like
can be seen.
to the light
features
source.
surface,
whole
were observed which were

facet.
This suggests
between the features,
relationship
be discussed in Section 6.2.1.
of the fracture
SEMexamination
to
areas and also reflect
of the fracture
over each intergranular
distributed
evenly
could be
In addition
features
with respect
oriented
facets
6.2 is an optical
Fig.
facet.
to the bright
orientations
specific
reflections
on the surface.
numerous dark linear
areas
the reflective
strongly
bright
showing one such intergranular
fractograph
When viewed
however, the intergranular
microscope,
Fracture
oriented
surface
revealed similar
features
6.3 is a low magnification

large grains,
each with
surface markings.
micrograph
the
At higher
6.4) these markings can be seen to correspond

each
features which lie at specific angles to
-95-
Energy dispersive
boundary
in
the
surface.
grain
other
(Fig.
were enriched in aluminium,
6.5) showed that these plates
it
but because of atomic number limitations

analyse for nitrogen.
the fracture
(Fig.
hexagonal
the
of
precipitates
as A1N by selected
The agreement with
A1N structure.
based on the A1N lattice
in conunercial
been identified
Although the room temperature
area electron
6.1).
calculated
was excellent,
Similar
features
have also
failures
(see Appendix
fracture
surface was macroscopically
2, Fig.
6.4 does show the presence of considerable
Fig.
This is manifest
ductility.
parameters
0.5% (Table
to within
generally
brittle,
taken from
{0001}
basal planes
found
to
to
correspond
and were
diffraction,
spacings
replicas
large plate-like
These were identified
6.6).
to
was not possible
However, extraction
surface contained
analysis
as the background of fine
larger
dimples
the
which
on
shaped
microdendritic
features
plate-like
4).
are
superimposed.
It was impossible
the formation
the plates,
to see any detectable
of these dimples in the SF,1, although,
of extraction
the presence of extensive
electron
diffraction,
well with
precipitates
calculated
were responsible
as with
8).
A1N precipitates
These were identified
and the observed lattice

values
for
in the TEM revealed
replicas
arrays of dendritic
6.7 and Appendix 2, Fig.
responsible
with an increased count rate of Al.
they were associated
However, examination
(Fig.
precipitate
(Table 6.2).
for initiating
doubt.
is
beyond
Fig.
SEM
in
the
observed
dendritic
feature
a
electron micrograph of
by
spacings agreed
The fact
that these
the micro-voids
6.8 shows a scanning
on the fracture
surface
96
-
(as-cast)
4176
cast
of
together with a TEM dark field
AIN dendrite
from the same sample.
extracted
image of an
The dendrite
is
is
Zum,
the
order
of
which
considerably
of
spacing
dendrite
the solidification
arm spacings (typically
The mechanism of A1N-induced

form of the nitride
dendritic
grain
boundaries
acts
boundaries
result
the exact
position
which
is present
front
decohesion,
These are scanning
electron
fracture
one side
This
in the as-cast
be noted from-Fig.
6.5 that associated
on some fracture
surfaces were 'spines'
either
as inclusions
on the fracture
the sulphides
with their
surface
(Fig.
to be heavily
6.11).
faulted
The fact
that
(Fig.
solubility
stage of primary
cooling
of globular
or
by the inclusions
showed
which is consistent
This
state.
product
dispersions
of MnS
of secondary
(see Section
3.4.2.2).
are in such close proximity
the MN suggests that the two precipitates

similar
6.12),
grain boundaries
the MiS inclusions
is
nitride
T. E. M. examinations
in the solid
of the decreasing
at the austenite
of an
the plate-like
with
or as holes left
during cooling which often produces fine

inclusions
halves
These were found to be NiS and
having been precipitated
occurs as a result
6.9 and 6.10.
feature.
It will
were manifest
from
by a mechanism
aluminium
of each plate-like
inclusions.
deviating
of mating
and show that
rod-like
to the grain
as shown in Figs.
on only
occasionally
at room
occurs
present
features
The
two-fold.
at an angle
micrographs
surface
20-200M).
occasionally
of the boundaries.
than
smaller
inclusion
lie
which
in the crack
of precipitate/matrix
intergranular
therefore
as a void-initiating
The AlN plates
temperatures.
T. F. is
arm
to
may have formed at a
in the austenite
region.
However,
97
numerous A1N plates
not
be considered
6.2
and for
the MnS 'spine'
contain
on the fracture
were present
to contribute
the sulphides
reason
to the fracture
significantly
cannot
process.
A1N Precipitation
Both forms of A1N are extremely

and could
not be resolved
section.
By examining
fracture
several
6.13).
inadequacies
any
in a 'plateau'
region of the
the precipitate
was identified
assume a typical
This represents
in the technique would result
20nm thick
A1N thickness
was measured
an upper limit,
similar
Plate-like
is therefore
of -'SOnm(0.051zn).
of the
carbon film
reasonable to
All
the precipitates
since they
contrast.
A1N
The crystallographic
nature of the plate-like
examined using the eucentric
to {000'}AlN
angular relationships
form of MN was
goniometer stage of the SEM. Since
it was known from the TEM studies

was parallel
it
since
in overestimates
to be of a comparable thickness,
observed were estimated
could
when the apparent
In this way, the thickness
which was approximately
to estimate
was possible
Because of the presence of the supporting
thickness.
exhibited
it
when viewed on the screen was a
to be 65nm (650).
directly
of intergranular
replicas
This was done by searching
This position
of the precipitate
minimum (Fig.
extraction
the specimen stage until
be seen 'edge-on'.
in a metallographic
when viewed
prominent precipitate
and tilting
thickness
optically
of the precipitates.
for a suitably
replica
thin under normal circumstances
in the TEM, however,
surfaces
the thickness
6.2.1
this
which did
surface
that the plane of the A1N plates
the approach taken was to measure the
between the 'families'
of plates
observed
98
-
on a single
grain boundary surface,
and to relate
interplanar
angles of the austenite
matrix.
the habit
to establish
possible
and therefore
developed with the austenite
room temperature when the structure

Preliminary
any orientation
cannot be observed at
has transformed.
out using the broken half
experiments were carried
from
4210.
impact
Charpy
taken
cast
specimen
a
microscope (Fig.
souce of light
a point
sample was tilted
repeating
this
until
a family
under
was provided by
darkened room.
of plates
were plotted
that a commonly occurring
families
of plates
on a stereogram,
and it
angle between families
The
was in a
and the goniometer readings were noted.
procedure for several
angular positions
approximately
Illumination
in an otherwise
away
-2m
and rotated
position
reflecting
6.15).
of
This was mounted
on a goniometer head and examined optically
in 'Plasticine'
a binocular
It was
method because the precipitation
takes place at high temperatures,

relationship
In this way it was
plane of the precipitate.
indirect
necessary to adopt this
these to the
By
the relative
was noted
of plates
was
(The angles between {111} planes in austenite
70.
are 70.5 3 and 109.4 7) .

More accurate measurements were made using the goniometer stage of
the SEM. In this
holder
(Fig.
The fracture
was parallel
tilted
until
disappearing
case the sample was mounted in an auxiliary
6.16)'and
viewed in the normal secondary electron
surface was then rotated

to the horizontal
the flat
(Fig.
tilt
surfaces
until
one family
mode.
of plates
axis of the viewing screen and

of the plates
6.17 and 6.18).
were on the point
This uniquely
defined
of
the direction
of the plate normal and the angular readings of the goniometer
99
drive
it was not possible
on the specimen stage,
of tilt
'extinction'
the plate
In this
of the plates.
normal was calculated
individual
on one grain boundary surface are plotted
At first
in Table 6.3.
several
6.19,
in Fig.
projection
sight,
it
families
on a stereographic
70 or 110, but that other

However, it
is important
remember that the grain boundary surface originally
fracture
and that both have contributed
to
comprised
one of which is on the mating half
grains,
surface,
of plates
is apparent that there are
angles are also present.
two austenite
of
and the angles between them are presented
angles of approximately
arbitrary
to achieve
the direction
situation,
range
by the method shown in Appendix 4.
of the normals to five
The position
because of the limited
Occasionally,
unit were recorded.
of the
to the features
observed.
This is shown quite
clearly
the linear
discontinuity
represents
the line
The fact
In each case
in the morphology of the fracture
of intersection
is a single
prior
surface
of three columnar grains.
In Fig.
surface.
line
the
across
of the grains,
has arisen
indicating
grain which is present on the fracture
terminating
that these platelets
on either
at the discontinuity.
have grown into
of the
observed is continuous
from an AUN plate
Fig. 6.21, however, shows platelets

intersection
grain which has been in contact
6.20, the platelet
of intersection
feature
the
case,
the austenite
austenite
These are now on the mating half
with two other grains.
this
6.20 and 6.21.
that the surface being viewed is convex in nature means
that this
fracture
in Figs.
that in
growing into
surface.
side of the line

It
of
can be concluded
the two adjacent austenite
grains
100
-
half
the
mating
are
on
which
of the fracture
Therefore
of angular
are two sets
there
are at some arbitrary
which
five
families
that
the angles
{111}
1,3
for
angles
(70.53
y
in the SEMare estimated
it
it was possible
involved
between them.
grains
This was done by tilting
both were on the point
(Fig.
6.22).
the reasons
noted
planes
AIN plates
Similar
surfaces
to their
measurements
confirmed
the
angular relationship.
the atomic
orientations
by the use of thin

However,
the austenite
foil
the examination
from the grain boundary region of an as-cast

growing into
simultaneously
Measurement of the angle
to be 710 + 1.
to confirm
earlier.
surface,
the sample
and rotating
and other fracture
occurrence of this
{lll}Y
measurement was
normals were then perpendicular
on numerous other grains
10C)01JAIN //
the
to the
parallel
on the fracture
of disappearing
between the normals shows it
was not possible
that
as in Appendix 4.
traces and in the plane of the photograph.
It
68 and 76
a more accurate measurement of the angle
until
frequent
seen
in the measurement of the angles
which intersected
The plate
is
and 5 are 1090,74
to be +30 when a direct
to obtain
it
can be concluded
made, and +5 when the angle was calculated

By choosing two plates
6.3a)
the
the angles between {111} planes
the austenite
The errors
planes.
(Table
2,3
plates
and 109.47)
grow into
plates
By dividing
and 4 are 108,
Comparing these angles with
in austenite
{0001}
two groups
between plates
and the corresponding
and 700.
into
of plates
the two austeni, te grains
to each other.
angle
in Table 6.1
relationships
of AIN into
to the growth
corresponding
surface.
grains
within
the
TEM specimens
of foils
for
taken
sample did show the

the
of
side
on each
101
-
(Fig.
boundary,
6.24).
ferrite
pro-eutectoid
had of course transformed
The austenite
during cooling
and no orientation
to
relationship
could be inferred.
AiN
Dendritic
6.2.2
Solidification
Results of the Directional
6.2.2.1
With the power inputs
employed during the solidification
the maximumtemperature
attained
two phase (solid/liquid)
position
30mmbehind the liquidus.
was determined from a longitudinal

The dendrites
microscope.
solidification
process had a considerably
quite
Fig.
clearly
solidus,
so the interface
solid
finally
between the two was
morphology varied with position
At low magnifications,
the fractures
in
were similar
In the areas which had been quenched from above the
porosity
prior
morphology was encountered
was also evident.
to quenching,
areas which had partially
intergranular
an
gave
austenite
during quenching
for both the high Al and N (4383) and low Al and N
an interdendritic
Some central
fully
6.26),
arm spacing than
recognisable.
along the casting
both cases.
larger
section
from the directional
arising
which had formed from the liquid
6.27 shows how the fracture
(4382) casts.
of
Fig. 6.25 shows how the
in the optical
(Fig.
the
sample
of
revealed the
observations
region to extend for a distance
of the liquidus
the dendrites
process,
in a dummyspecimen was found to
be 1610C, and subsequent metallographic
approximately
Work
fracture
grain boundaries.
(Fig.
6.27).
In areas which had been
the fracture
transformed
around ferrite
was fibrous,
and
to ferrite
(Fig.
6.28)
networks at the prior
102
The main areas of interest
were the interdendritic
the partially
and these were examined in more detail
for
solid
evidence
region
of A1N precipitation.
(low Al and N) exhibited

interdendritic
The samples from cast

II
numerous type
(Fig.
regions
6.29)
but with
(high Al and N), however, contained fine

superimposed on the interdendritic
and these were found to be rich
fracture
intergranular
6.2.2.2
surfaces
fracture
of extraction
in some cases the dendritic
Fig.
for
replicas
dendrite
the
of
arms.
observed
example,
Fig.
on
6.8).
in the grain boundaries

state precipitation
of
and dendrites
appearing to be merely extensions
of Processing Variables
Table 6.4 gives details
the mode of failure
Contents
of the room temperature
of the 0.30C-1.50Mn steels
condition
an order of magnitude
taken from the intergranular
A1N present
the plates
with
6.3.1
arm spacing of
6.31 shows areas where the plates
are continuous,
Effects
6.30)
arm spacing and is in
may act as a nucleus for subsequent solid
6.3
4383
of cast 4176 revealed evidence to suggest that
surface
AIN plates.
to suggest
Observations
Metallographic
The examination
in the
(Fig.
surfaces
of A1N dendrites
(see,
4382
inclusions
The dendrite
dendrite
that
agreement with
reasonable
fracture
was 1-2um, which is at least
than the solidification
smaller
no evidence
dendritic
in Al.
from
NhS precipitates
The D. S. samples made from cast
any A1N precipitation.
the precipitates
fractures
used in this
of castings
fracture
investigation,
morphology
showing that
in the quenched and tempered
depends on the aluminium and nitrogen
contents of the steel.
103
-
For a given steelmaking
increasing
cooled
below which
-1.5
(Practice
of 0.1C sec-1,
at a rate
instance corresponding
I. F. will
not
3 (comparing
x 10
occur
'A'),
corresponds
increased cooling
Li
value
Comparing these values with

by Lorig
as high
of
the susceptible
suggests that
4.1) it
made by
only 50% I. F.
cooling
rate curves obtained
can be seen that they lie

This
rate.
and Elsea err on the side of
be used with some confidence.
safety,
and can therefore
further
be remembered that
aluminium levels
their
added, and a recovery rate of approximately

This has the effect
to I. F. decreases with
region for each cooling

of Lorig
the results
[%N]
as 3.7 x 10-3.
the critical
and Elsea (1947) (Fig.
well within
of their
to a value
'B' which were cooled at 0.23C sec -1 contained

[%A1]
with
[%A1]
The small keel block castings
rate.
level
the critical
4211 and 4351).
casts
Table 6.4 also shows how the susceptibility
Practice
to
rate) the amount of T. F. observed increases with

[%N].
For the 75mmsquare castings which were
x
cooling
[%u]
a constant
(in this
practice
of halving
It should
to the Al
refer
50%will
be expected.
the values on the horizontal
axis
graph.
The effects
of Al micro-segregation
were measured by EPMAtechniques
had
4210
which
a nominal Al content of 0.17%.
on cast
shows the micro-hardness
the probe.
interdendritic
indents which identified
The maximun concentration

region
Fig.
the scan path for
detected was 0.19%A1 in the
compared to 0.16%A1 in the dendrite
This corresponds to a segregation
ratio
6.32
core.
of Cmax/Cmin = 1.19.
104
Carbon Content
6.3.2
the carbon
Increasing
0.56% and 0.65%C (casts
75uunsquare
of three
content
4353,4354
and 4355 respectively)
of 0.42%C, the fracture
At a level
of a 0.30%C steel.
to that
exhibited
of the grain
the size
Fig.
This
6.33).
boundary
corresponds
from the peritectic
behaviour
morphology.
intergranular
and similar
The 0.56%C and 0.65%C steels
intergranular
a fully
was fully
resulted
fracture
in a marked change in the quench and tempered
fracture
facets
but
surface,
still
in this
case
(see
was much smaller,
to a change in the solidification

transformation
directly
: 0.50%C to solidification
to 0.42%,
castings
at carbon
to austenite
contents
at higher
carbon
levels.
It can, however, be concluded that

in the formation
results
austenite
is not
contained
IF.
Pouring Temperature
The pouring
effect
steels)
since the 0.65%C, 1.50%mri
process,
and still
pearlitic
(which
network at the prior
for hypoeutectoid
the precipitation
steel was fully

6.3.3
of a ferrite
grain boundaries
influencing
the y-oa,transition'
temperature
fracture
the
on
embrittled
of the casting was found to have little

mechanism.
0.30C-1.5OMn steel
Three keel block castings
were produced with pouring
1700C
1620C
15500C,
and
corresponding
of
120C and 200C respectively.
was fully
intergranular
etched sections
differences
After
in as-cast
the fracture
in each case, and the examination
grain
structure.
temperatures
to superheats of 50C,
heat treatment,
through the castings
of
of macro-
revealed no discernable
105
Heat Treatment
6.3.4
(a)
Cast 4176 was initially
hardness
treatments
are presented
and the cast
In the as-cast
after
6.34.
The close
was only after
annealing
of different
The results
were
which
the fracture
such as quenching and
the fractures
became intergranular.
It
in the furnace from 900C that the amount

40%, the remainder of the
hardness levels
on impact properties
will
be presented
to the high temperature
A1N as reported
by Lorig
times at 600C.
and 4351 (0.12A1,0.014N)

solution
treatments
were
shown in
of I. F. by redissolving
and Elsea (1947).
However, there was no marked difference

appearance before
and after
between the macroscopic
heat treatment
In both cases the amount of intergranular

heat treatment
was
in Section 6.4.2.3.
6.35 to attempt to reduce the levels
but after
heat
occurred by a cleavage mechanism, but
Casts 4210 (0.17A1,0.017N)
fracture
various
be seen.
Charpy
by
tempering
samples for various
also examined
Fig.
Results
being ductile.
The effect
subjected
I. F.
surfaces
between
association
of I. F. was reduced to approximately
(b)
of matrix
of the casting,
can clearly
failure
tempering or normalising,
fracture
The fracture
hardening heat treatments
various
out after
section
cross
structure
state,
carried
in Table 6.5.
a full
'reconstruct'
is shown in Fig.
facets
bend tests
point
for
and microstructure
of the slow three
used to
used to examine the effect
the fracture
have
been
facets
attributed
which
shiny
fracture
surface
of either
cast.
remained constant,
did not exhibit
to the A1N plates
the
and the
106
Examination of the fracture
more dull.
appearance was altogether
in the SEMrevealed the reason for this
surfaces
Although the high temperature heat treatments

the A1N, some considerable
in dissolving
precipitates
with
had taken place.
coarsening of the
The dendritic
morphology (Fig.
and assumed a rod-like
failure
had been unsuccessful
features
associated
dimples on normal T. F. surfaces had coarsened
the ductile
had begun to spheroidise
features
difference.
(Fig.
6.36),
whilst
the plate-like
6.37) and also induced
by void nucleation.
Hence although
the macroscopic features
had not changed, on a microscopic
of the fracture
surface
scale the mechanism of failure
had been modified.

The coarsening of the A1N meant that
be seen in the optical
the precipitates
microscope at high magnifications
in
E.
P.
M.
A.
be
the
analysed
and could
aluminium and nitrogen
ratio
of 2: 1.
(1.93: 1).
silicon
could now
Using this
(Fig.
technique,
6.38)
both
detected
had
and
an approximate weight
were
The corresponding
ratio
for pure A1N is 27: 14
No other major element such as sulphur,
manganese,
found
in
the nitride.
was
or phosphorus
Using the SEM to observe polished
microsections,
to view the precipitates
in some detail,
The use of backscattered
electron
techniques highlighted
dispersive
analysis
as shown in Fig.
imaging and contrast
the coarsened precipitate,
was able to detect
in the region of the precipitate.
it was also possible

6.39.
enhancement
and energy
an increased Al count rate
107
6.4
The Results of Mechanical Testing

Testing
Tensile
6.4.1
The room temperature
tensile
(cast 46/89) and an unembrittled

of heat treatment
two states
of I. F. on the tensile
are presented in Table 6.6.
properties
in the
ductility
falling
the tensile
with
of area (3% elongation)

for this
The specification
This is thought to arise

of the castings,
(BS 3100 AS, 1976)
higher
tensile
both
condition
sets
and UTS specifications
Table 6.7 and Fig.
from the variations
Ma content
heat treatments.
in manganese contents
of results
of cast
heats (see
46/89 has contributed
In the quenched and tempered
strength.
were,
however,
the 0.2% P. S.
within
of BS 3100 AS (1976).
6.40 show the variation
of cast 46/89 with
ductility
identical
which were made from different
The higher
5.1).
temperature.
in tensile
strength
The temperature
and
dependence
to that which would be expected for normal fibrous
is similar
in that both the 0.2% P. S. and the UTS decrease
failures,
significantly
with
the earlier
fracture
steel.
cast 46/89 had a higher 0.2% P. S.
46/4
46/1
UTS
than
and
after
casts
and
with
in the embrittled
grade of steel
be noted that
further
It will
to its
in the base material
a minimun of 13% elongation.
requires
Table
The effect
can be seen most clearly
of area (16% elongation)
from 57% reduction
steel
Ccasts 46/1 and 46/4)

-in
steel
quenched and tempered condition,
to 12% reduction
of an embrittled
properties
increasing
observations
temperature.
(Section
This is in agreement
6.1) that
intergranular
proceeds by a mechanism of void nucleation
AMNinclusions
which are localised
at the position
and growth at
of the
rior
108
-
boundaries.
grain
austenite
to the microstructure
with respect
and the 'intergranular'

yield
Hence the fracture
strength
path is trans granular
present at the time of testing,

depend to some extent on the
will
of the matrix.
strength
in excess of 200C
The increased values of the UTS at temperatures

can be attributed
fracture
Typical
failure.
modes of
are shown in Fig.
surfaces
6.41.
of T. F. on Inpact Properties
The Effect
6.4.2.1
of 1. F. on impact properties
The effect
be seen in
can clearly
6.42 and 6.43, which give the Charpy impact transition
curves for imembrittled
and embrittled
from ductile
showed the usual transition
at high temperatures
failures
respectively
in
WQ;
WQ). Cast 4131, which had a low Al and N content
600C for lhr,

6.42j
castings
(950C for l1hrs,
the quenched and tempered condition
(Fig.
to fibrous
transition
Impact Testing
6.4.2
Figs.
to a partial
to cleavage failures
The impact transition
temperatures.
the upper shelf
fibrous
at lower
temperature was -60C, and
energy was 83J.
Cast 4210, however, which contained 0.17%A1 and 0.017%N exhibited

significantly
different
(-196C) the failure

a transition
firstly
fibrous
(Fig.
6.43).
At low temperatures
mode was by cleavage, but instead
to fibrous
in a fully
failures,
intergranular
mechanism.
than the unembrittled

well with
behaviour,
increasing
fracture,
This gave a significantly

material
the observations
of promoting
the temperature
resulted
then a mixed I. F. /
lower energy fracture
at the same temperature and agreed
of Wright
(1962) which were presented
109
-
in Fig.
However, by increasing
3.1.
further,
still
a second transition
excess of this
fibrous
the testing
and an upper shelf
In
was observed at -200C.
the fracture
temperature,
temperature
mode became fully

to that of cast 4231
energy similar
was attained.
The effect
results
Fig.
in Fig.
markedly
quite
6.44 which
However,
it
a least
be noted
will
than -85% did
the %I. F. was greater
of Testing
Effect
In order to investigate
that
region
in fractures
only
the impact
used to produce further
where
below
having to use high
without
embrittled
casting
Charpy specimens.
this
an impact energy of 82J, (Fig.
to the upper shelf
(cast 4351) was
At room temperature
and in the quenched and tempered condition
failed
6.45).
energy of the unerbrittled
down
to a temperature
encountered
became one of cleavage.
in a ductile
This is similar
material.
the temperature below 0C, however, an intergranular
By reducing
regime was
of -164C when the failure
The fracture
mechanism
morphology at each testing
is also shown in Fig. 6.45.
Examination of the fracture

and continuous
fibrous
fall
energy
of
between the various
the transitions
a less severely
temperatures,
temperature
of the
plot
Temperature
fully
more
mechanisms
manner with
squares
minimum of 25J (BS 3100 AS, 1976).
the specified
fracture
is
is shown
energy
from the mixed intergranular/fibrous
obtained
6.43.
6.4.2.2
of T. F. on the impact
of the presence
failures,
transition
surfaces
with
in the SEMrevealed a complete
decreasing
through mixed fibrous/I.
temperature
from fully
F. to almost fully
(-90C) and then through mixed I. F. /cleavage
to fully
I. F.
cleavage.
110
of the broken
SEM examinations
test
revealed
pieces
the following
characteristics.
i)
fracture
In the fibrous
region,
were observed (Fig.
features
occasional
6.46a).
These were on a much larger
scale than the voids nucleated by AIN (Fig.

to be associated
The fracture
the dendritic
with
coarse dendritic
6.4) and appeared
structure
of the casting.
could not be described as interdendritic

(Fig.
as shown at higher magnification
6.46b).
Thus the micromechanism of failure
casting.
failures,
of normal fibrous
inclusions
is identical
to that
is only the distribution
of
appearance in certain
on the impact energy were noted in either
adverse effects
intergranular
fracture
scanning electron
instance.
temperature was decreased, not only did the
As the testing
macromechanism of failure
change, but the micromechanisms of the
process also changed.
micrographs of intergranular
broken at -300C and -164C, respectively.

there is evidence of ductile
(Fig.
regions of the
This phenomenonwas also observed in cast 4231 but no
areas.
ii)
and it
in the dendritic
which results
at MnS inclusions,
appearance is considered to be
of MnS in the interdendritic
density
the greater
had
Failure
occurred by the usual mechanism of void nucleation

but the reason for the dendritic
per se,
facets
from samples
temperature
dimples around the A1N dendrites
At the lower temperature however, the overall

facet
6.47a and b show
At the higher
6.47a) which is the mechanism normally
of the intergranular
Figs.
associated
fracture
is one of cleavage (Fig.
with
I. F.
appearance
6.47b).
The
A1N appears to have taken the role of cleavage crack initiator,

fracture
proceeding
boundaries.
grain
for short
distances
Although less clearly
along the prior

defined,
austenite
some of the
with
111
-
features
plate-like
of room temperature failures
typical
can still
be resolved.
At temperatures below -164C, the fracture
iii)
predominantly
transgranular
fracture
surface.
6.4.2.3
The Effect'of
Matrix
6.48 shows a typical
and Fig.
cleavage,
mode was
Hardness
hardness on the impact strength
The effect
of matrix
examined.
Samples from casts 46/6 and 46/7 were solution
at 950C and water quenched, followed

ihr,
curves obtained are shown in Fig.
transition
photographs of the fracture
surfaces
The impact
6.49, and optical
are presented in Fig.
It is apparent that the samples with the higher matrix

(shorter
tempering times) were not only'more
by I. F. at room temperature,
treated
by tempering at 600C for
2hrs, 4hrs and 8hrs, respectively.
lhr,
was also
hardness
susceptible
but also exhibited
6.50.
to fail
the phenomenon
temperatures.
In the samples which
had been tempered for
8hrs to give a matrix
hardness of 186 HV30
there was very little
evidence of any I. F.
This is concordant
of Wright and Quarrell
(1962) who used
over a wider range of testing
with
the observations
isochronal
tempering treatments
for
susceptibility
6.4.3
Fracture
T. F. on matrix
The results
hardness.
Toughness Testire
The method of calculating

significance
to show the dependence of the
of c, i,
CODvalues from the. test

u and
of the CODtests
6max are discussed in Appendix 1. b.
carried
in
6.8
Tables
6.11.
to
are given
data and the
out at different
temperatures
e, di,
6u and 6max
Values of
112
-
The material
are given where appropriate.
of tests were as follows:
of the four series
HHQT: High aluminium, High nitrogen,

LLQT : Low aluminium,
Low nitrogen,
Quenched and Tempered.

Quenched and Tempered.
HEIN : High aluminium, High nitrogen,

LLN
: Low aluminium,
Low nitrogen,
Normalised.
Normalised.
For the quenched and tempered material,

tested
to allow
codes assigned to each
the full
behaviour
transition
A smaller number of normalised
sufficient
samples were
to be examined.
for comparison
samples were tested
purposes.
Comparison of Tables 6.8 and 6.9 reveals
an interesting
in behaviour between the HHQT(susceptible

(non-susceptible)
fracture
behaviour,
not vary signficantly
the initiation
steel.
value of the COD (Si)
does
However, comparing the values of
of maximum load (6
values for the HHQTsteel

The criteria
in overall
between the two sets of samples, and is in
the range 6i = 0.06 - 0.09m.

the CODat the point
to I. F. ) and LLQT
Despite the difference
samples.
difference
max)
it
can be seen that the
are in general much lower than for the LLQT
for the selection
of a 'critical'
value of the
have been considered in Appendix lb.

COD(di vs 6
Figs. 6.51
max)
based
6.52
transition
give
curves
on 6i and mx respectively.
and
At low temperatures
event,
there is no ambiguity
in determining
the critical
and the value of CODused is 6c.
The difference
between the two kinds of fracture
be seen more clearly

displacement
6.53 to 6.55.
with
reference
curves and typical
behaviour
can
to the schematic load vs
fracture
surfaces
shown in Figs.
113
Fig.
6.53 shows the behaviour
quenched and tempered

Fracture
to suggest
slow crack
After
steel.
curve
initiation
bursts
no evidence
the LLQT (uaembrittled)
deformation,
a slow
to grow in a uniform way.

control,
Since
a maximum
as the
progresses.
for
the HHQT material,
identical
almost
to that
growth.
of slow crack
limited
with
out under displacement
6.55 shows that

is
with
is reached and the load decreases steadily
force plateau
Fig.
and continues
is carried
front
crack
associated
amount of plastic
a small
initiated
is
crack
the test
brittle,
of -100C
to failure.
growth prior
the behaviour
6.54 is
the samples (both
by all
at temperatures
and normalised)
is macroscopically
below.
and
Fig.
exhibited
amount of crack
along
grain
6.54 up to the
Subsequently,
however,
fracture
observed
This
after
in sharp
proceeds
boundaries.
in load
decreases
the discontinuous
shown in Fig.
propagation,
the embrittled
the load vs displacement
gives
rise
to
the attainment
after
load.
um
m=im
of
At first
initiation
of I. F.
sight,
However, examination
austenite
fatigue
oriented
is not sensitive
of the fracture
6.56) shows that in all
in a fibrous
The reason for this

position
seems strange to find
value of the COD(Si)
samples (Fig.
initiated
it
therefore,
boundaries
grain
embrittled
surfaces
of embrittled
has been
cases, fracture
manner at the root of the fatigue
crack tip with
respect
in the castings.
is unlikely
to end exactly
the
to the presence
was thought to be due to the highly
fatigue
the
of
crack tip
that
crack.
localised
to the large prior
Because of this,
the
favourably
a
at
fibrous
boundary,
some
and
grain
crack growth
114
has to take place
Fig.
manner.
region
6.57 is
of ductile
fatigue
crack
manner,
the crack
the original
focussing
before
tip.
crack
conditions
failure
a scanning
fibrous
growth
over
This
micrograph
immediately
to propagate
had to cross
plane.
electron
crack
In order
in an intergranular
can proceed
showing a
ahead of the
in an intergranular
to a plane
corresponds
on the SEM shown in Fig.
1.5mm away from
to a change in
6.57.
the
115
Chapter
Discussion
'. 1
Introduction
work have provided
The results
of this
information
for cast steels
fracture
played by A1N in the fracture
This has been supported by the observation
process.
in heat treatment,
caused by variations
amount of
on the nature of the intergranular
and the role
surface
a considerable
of effects
and testing
composition
conditions.
This chapter considers
fracture
intergranular
proceeds,
The effects
form.
precipitates
the mechanism by which AIN-induced

and the way in which the AIM
of some processing
discussed in Section
7.4, and finally
mechanical properties
is considered
the influence
in Section
Although most of the work has been carried

the industrial
environment,
variables
significance
are
of I. F. on
7.5.
out in a laboratory
of some of the results
is highlighted.
7.2
The Mechanism of I. F.
have confirmed
The results
grain boundaries
primary
fracture.
crack propagation
microstructure
is actually
which exists
merely follows
to delineate
can be a major cause of intergranular
is important
it
of AIM on the
the precipitation
However, in order to understand
I. F. occurs,
front
that
the mechanism by which
to remember that
trans granular
in most cases the
with
respect
at the time of testing.
the network of A1N precipitates
the original
boundaries
to the
The crack
which continue
formed.
they
on which
Hence
116
-
it
to find
is not surprising
depend to a certain
the micromechanisms of I. F.
that
of the
on the mechanical properties
extent
matrix.
The mechanism proposed
and in broad
occurred
through
boundary,
location
of the boundary
into
provided
jagged
constant'
The results
to the grain
in a longitudinal
section
at a 'fairly
boundary.
have
the
work
enabled this
present
of
microscopy (unavailable
proposed
The use of scanning
mechanism to be extended and modified.

electron
such
to the dendritic
in the grain
to lie
side.
for
These he attributed
surface.
form of A1N which he considered

angle
at either
justification
steps
from
the A1N 'needles'
grains
some experimental
when he observed
the fracture
the austenite
deviated
but
to follow
3.21
fracture
that
was suggested
of the grain
(1962)
a theory
It
correct.
which projected
Wright
(1952) was shown in Fig.
in the region
the precise
(sic)
terms is
by Lorig
to these earlier
workers)
has
by
indeed
Wright
the
that
are
steps
observed
at several
shown
well-defined
boundary
(Section
the
to
angles
grain
However, as Figs.
6.4 and 6.6 reveal,
AUN, but from the plate-like
from the dendritic

precipitate
the adjacent
the features
which has nucleated

austenite
6.2.1).
arise not
form of the
in the boundary and grown into
grains with a specific
orientation
relationship.
The general mechanism of I. F. is,
crack front
broadly
follows
therefore,
the position
one in which the
of the prior
grain boundaries which are defined by the dendritic

but occasionally
deviates
from the boundary when it
austenite
form of AlN,
encounters
117
plate-like
The exact mechanism has, however,
of A1N.
precipitates
been shown to depend on the temperature of testing

overall
fracture
steel
transition
usually
phase particles,
In embrittled
occurs
as a result
the dendritic
exact
of decohesion
(Fig.
grain
at the interface
(Figs.
and the matrix
void
of preferential
of the prior
second
or oxides.
in the same temperature
A1N precipitates
position
in Section
and growth at appropriate
sulphides
however,
steel,
(DBTT) the unembrittled
temperature
by void nucleation
fails
At temperatures above
mechanism of the matrix.
the ductile/brittle
and the
nucleation
6.4).
and growth
Deviations
boundaries
occurs
of the plate-like
6.9 and 6.10).
regime, I. F.
This
from the
as a result
A1N precipitate
situation
was considered
3.4.2.
Below the DBTT the fracture
mechanism of the uaembrittled
is one of cleavage and this
is reflected
intergranular
fracture
surface
of cleavage which are confined

boundary (Fig.
material
features
characteristic
Wright
grain
are much less
This is probably because deviations
from the
unfavourable.
In both the high temperature and low temperature
of the nitride,
by areas
to the region of the as-cast
plane of the cleavage crack are energetically
the fracture
at similar
now appear to be linked
6.47b) and the plate-like
defined.
matrix
in the nature of the
of embrittled
The A1N dendrites
temperatures.
clearly
at
regions,
therefore,
process appears to be dominated by the dendritic

with
the plate-like
ozm being responsible
spangled appearance of the fracture
form
for the
surface.
(1962) has already emphasised the importance of relative
118
grain boundary and matrix
it
is possible
observed
the change in fracture
to explain
to I. F. to cleavage
with
decreasing
If we consider
Orowan (1945) model used to explain

can be seen that
it
transitions,
and the cleavage
fracture
'intergranular'
of the embrittled
the strength
the classic
to brittle
the yield
strength
to include
aIF which
a
to
refers
grain boundaries.
prior
temperature has been shown to be similar
of aIF with
strength
the mode of failure
This model can now be extended
may be predicted.
conceptual
by comparing
at any temperature
strength
mode from fibrous
ductile
normal
temperature,
This has been
temperature.
6.43 and 6.45.
in Figs.
the susceptibility
Since both of these vary with
4.3.1).
to I. F. (Section
in determining
strengths
The variation
to that of
both
DBTT,
the
since
are governed by the ease of void
ay above
nucleation
shows how this

strength
'intergranular'
Qy is low, fibrous
second transition
falls
the temperature
mode of failure,
failures
to fibrous
This is thought to arise

fracture
with
At low
failures
mechanism, since acl
The reason for this
is that the yield
fracture
to an
at high temperatures when
predominate.
strength
due to the constraints
strength
(See Fig.
involved
7.1).
in
increase
boundary
tend
to
the
aIF
which
grain
along
respect to the uniaxial
there will
the fractographs
stress.
yield
In the region of each transition

that
7.1
in a transition
results
whilst
below the intergranular
Fig.
at a given temperature.
cleavage is the most favourable
Increasing
intergranular
6.40).
compares to the yield
strength
and cleavage strengths
temperatures,
is low.
(Fig.
at second phase particles
temperature
be mixed modes of failure,

presented in Fig.
6.45.
it
is to be expected
which is verified
by
Thus with decreasing
119
-
be a continuous
temperature there will
through mixed fibrous/IF
from fibrous,
range of fracture
mechanisms
to IF and through mixed IF/
cleavage to cleavage.
Fig.
7.1 can be used to interpret
work, and will

position
will
several
to again in latersections.
be referred
of the 'intergranular'
to Fig.
reduced and reference
strength
the
In
be
will
7.1 shows that there will
interval
increase in the temperature
Clearly
of the A1N embrittlement.
for example, this
material,
embrittled
of this
to the other curves
curve relative
be determined by the severity
heavily
of the results
be an
over which IF occurs.
Reducing the amount of A1N present at the boundary may increase

that
aIF to such an extent
IF is not observed at any temperature.

from cleavage to fibrous
case a simple transition
In this
fracture
takes place.
The hardness and condition
also affect
the relative
is because the yield

may all
be changed.
relative
right
7.3
The results
of different
show how the temperature

increase with
of the strength
intergranular
strength,
out on material
carried
positions
vs temperature
increasing
interval
matrix
strength
This
and cleavage
of the Charpy tests
matrix
hardness (Fig.
6.49)
over which IF occurs tends to

hardness.
movement of the QY vs temperature
in Fig.
of a casting will
7.1, although here matters are more complex.
curves in Fig.
strength
of heat treatment
This corresponds to a
curve upwards and to the
7.1, which broadens the IF region.
AMNPrecipitation
The role of each form of AIN in the fracture

7.2.
has
been
process
120
-
Although the presence of two morphologies of A1N has been recognised

for a number of years,
the temperature
has not been clear.
precipitation
and directional
have shown that the dendritic

liquid
is effectively
when it
Precipitation
stage of primary
data available
form takes place in the solid
cooling,
a steel
Al and N contents
and it will
form of ANN may in some cases act

6.31 and Appendix 2, Fig.
to the solubility
O. loAl and 0.01oN, the data of
(1967) given in Table 4.1 predict
this
the austenite
The temperature
limit
that the solubility
may well
knowing the microsegregation
lever
is appropriate
Details
rule
lie
phase field.
can begin during solidification

characteristics
of
of each of these in the residual
is determined using the Scheik equation
in iron.
For higher
region and in the solid/liquid
The concentration
and the equilibriun
temperature would of course be increased
at which precipitation
may be calculated
The latter
These
9).
4.4).
containing
be recognised
the Al and N.
state
and there is evidence to
temperature of 1401C for JUN in austenite.
solution
diffusion
grain boundaries.
ANN
Glacrnan and Pickering
liquid
stage of solidification
to the as-cast
for AMN, (Section
Dendritic
If we consider
observations
can precipitate
now be discussed with reference
will
observations
(Fig.
site
as a nucleation
outside
at a late
confined
suggest that the dendritic
7.3.1
form of the nitride
of the plate-like
at a later
The metallographic
experiments of the present work
solidification
from solute-enriched
and mechanism of its
respectively
for nitrogen
(Scheik,
(see Section 2.4.2).
in view of its
of the calculation
1945)
rapid
are given in
121
-
Appendix 5, and the results

bulk
For initial
limit.
exceed the A1N solubility

would be necessary
precipitation
precipitation
it
x=0.001,
to begin
for
liquid
treatment
a rigorous
the kinetics
also
will
of the residual
7.2 does show that
Fig.
Col
with
composition
Although
to consider
process,
7.2.
of Al and N, precipitation
concentrations
when the Al and N contents
become possible
it
in Fig.
are plotted
of the
for
a starting
be possible
should
for
is more than about
when solidification
70% complete.
This model does not,

interactions
with
of course, take into
carbon which also segregates into
the residual
Since the interaction
coefficients
during solidification.
liquid
account any solute
both
N
Al
are
and
positive,
with
of carbon
local
increase
and promote precipitation
solubility
by Valencia
(1981) in the context
higher
at a still
of nitrogen
temperature.
and experimentally
blowhole formation.
AIN was observed on the surface of blowholes,

can occur during the later
that AIN precipitation
any
tend to decrease the A1N
have been examined theoretically
These effects
Dendritic
in carbon content will
(Table 4.2),
confirming
stages of
solidification.
The limitations
segregation
residual
predict
but it
are recognised,
90% solid,
approximately
Beyond this
in using the Scheil
point,
liquid
is considered that up to
however, the predicted
increases
to model Al micro-
the model is sufficiently
asymptotically
some AN precipitation
solidification.
equation
accurate.
Al content
in the
and the model would always
in the very final
stages of
122
-
of A1N can occur in
It has been shown that precipitation

the liquid
modest Al and N contents.
with relatively
When the effects
of Al and N are also considered
of macrosegregation
is not difficult
it
(see Section 2.4.2)
to see why a large casting
may exhibit
I. F. even when the bulk Al and N contents
excessive.
Foundries producing
castings
been known to have problems with
still
force for such a morphology will

of Al and N in the residual
with a temperature
gradient
A]N morphology.
of dendritic
precipitation
1981).
A1N precipitates
the driving
that
be the concentration
as a function
liquid
This will
parallel
dendrites,
of the solidification
is likely
it
interface.
behind the solid/liquid
(Wilson,
of the dendritic
although
remains uncertain,
dendritic
I. F. with bulk Al contents of
mechanism of formation
The precise
of up to 200 tonnes have
of 0.013%.
levels
only 0.03% and nitrogen
are not
of the distance
also be coupled
to the direction
which will
further
An analogous situation
silicate
which were the subject
gradient
inclusions
of growth
favour a
is the
in iron-nickel-
of directional
solidification
silicon
alloys
studies
by Aritomo and Gunji (1979) and Sakaganu et al (1969).
These workers concluded that precipitation

liquid
the microsegregation
the driving
enriched
solidification
eventually
dendrites
it
force in this
case being
of oxygen.
once the AIN has begun to precipitate

liquid,
took place in the residual
in the interdendritic
solute-
may then be pushed ahead of the growing
dendrite.
As solidification
proceeds it will
become entrapped between two independent solidification

boundary.
form
the
grain
which
Uhlmann et al (1964)
123
have studied
different
in several
(1972)
the "pushing"
organic
observed,
below which
This may provide
a further
sufficiently
liquid
If
was
the cooling
but if
be less likelihood
solid.
of the effect
of cooling
rate is
of A1N in the
the precipitation
not only will
become less favourable,
occur, there will
in the growing
explanation
for
I.
F.
tendency
the
rate on
high,
dendrites
were pushed by the interface
the particles
they became entrapped
and above which
in steel.
examined by Uhlmann, a
of the solidification
velocity
growth
inclusions
case of silica
type of particle
For each particular
interfaces
and Myers and Flemings
materials
examined the particular
critical
by liquid-solid
of particles
such precipitation
does
of the precipitates
being
interface
pushed ahead of the growing solid/liquid
and eventually
becoming trapped at the grain boundary.

7.3.2
Plate-like
A]N
nature of the plate-like
The crystallographic
form of A1N seen
in Fig. 6.4 has been confirmed by the SEMstudies

The plates
described in Section 6.2.1.

boundaries
grain
into
the adjacent
during primary
austenite
planes in each structure
in the austenite
of the casting
and grow
an orientation
relation
These are the most closely
and examination
packed
of the atomic arrangements
the planes shows that the best matching is obtained with
<10I0>AIN//
<110>. (Fig.
these directions,
7.3).
and whilst
interface
a coherent
within
grains with
{111}Y.
(0001)//
form
the
of
within
cooling
nucleate
which were
This gives a misfit

the generally
is -5% misfit,
these planes is significantly
perpendicular
[0001]
//
of 6.5% along
accepted threshold
for
(Chadwick, 1972), the misfit

smaller
<111>1 directions.
than the misfit

This explains
in the
why
124
are so thin,
the precipitates
interface
the incoherent
into the austenite
(thickness)
in the [0001]
AN
estimated thickness
direction
of M500, this
about one hundred unit
cells
It is not suggested that this
thick
With an
(Section
are
6.2).
is the only possible
orientation
for MN since the precipitate
found in other morphologies.
For example, Yamanaka and
in a 0.20C-1.40Ni
steel
formed under conditions

orientation
relationship
[1120}AlN //
{I10}
[0001]MN//
was
Y.
containing
in thin
with
precipitates
and had an
transformation
the parent austenite
The preferential
of MN
0.04oAl and 0.015%N. These were
of isothermal
of the form
growth direction
of the rods
was determined by
studies
of the A1N/martensite
foils.
Using the Kurdjwnov-Sachs relationship
{101}a, and <I10>Y //
({111}Y //
acicular
<110>Y. This relationship
diffraction
relationship
to give the A1N/Y orientation

rather
is not favoured.
means that the plates
Ohmori (1978) observed intragranular
electron
grains and coarsening
be
established
can
which
relationship
is often
since growth occurs by movement of
<111>a, ) this
relationship,
orientation
was transformed
which is therefore
indirect.
The most familiar

structure
orientation
and austenite
relationship
between an h. c. p.
is that derived by Raynor et al (1966)
for 1b2Cwhich gives {0001}
//
{111}Y and <1120>
//
<110>1.
2C
2C
The atomic arrangements on the (0001) Nb // (111). planes are shown
2C
in Fig. 7.4(a) and it can be seen that there is good matching of
Mo and Fe atoms when the close packed directions
However, if
kind,
Fig.
the AlN were to assure an orientation

7.4(b)
are also parallel.

relation
shows that there would be a considerable
(-18%) at the AlN/y interface
and large distortions
of this
strain
of the austenite
125
would be necessary to accommodate the A1N. With the
lattice
proposed in the present work, the
relationship
orientation
ANN
the
unit
of
volune
excess
to be positioned
Fe atoms in the austenite

in the corresponding
The Effect
7.4
is incorporated
cell
(0001)AN plane,
by allowing
at inter-atomic
as in Fig.
sites
7.3.
on the Susceptibility
of Processing
Variables
Contents
to I. F.
7.4.1
It
is now well
of a casting
contents
a given
used in this
levels
[%Al]
such that
it
7.2,
Fig.
It
of Al and N required
[%N]
-1.5
If
can be seen that
at this
level
However,
cooling
rate
Al and N contents
is important
the kinetics
will
this
to remember that
occur at this
necessarily
size,
be susceptible
microstructure
important
role.
is
-1
sec
compared with
of Al and N, A1N
is more than 50%
process
why I. F. is
avoided
level.
the model described
in Section
at which the solubility
limit
temperature.
that precipitation
to I. F.
Other factors
7.3.1
is
will
the fact
Nbreover,
has occurred does not necessarily
A1N precipitation
casting will
this
explain
inferred
be
not
should
It
of 0.1C
of the precipitation
probably
below
castings
to cause I. F. were
when solidification
only determines the temperature

exceeded.
at a rate
and nitrogen
to I. F. at
the susceptibility
For the case of the 75nn square
is predicted
completed.
the aluminium
x 10-3.
precipitation
at this
increase
will
which were cooled
study
'critical'
the
for
rate.
cooling
increasing
that
established
that
mean that a
such as the grain
and hardness have also been shown to play an
In commercial foundry practice,
it
should be
126
the incidence
to minimise
possible
there
content
2.1.1
in Sections
but
and 2.2.2,
for
This
precipitation
(i. e. not
condition
before
limit
A]N
A1203)
the
to
solubility
exceed
as
cbmbined
can occur.
been
a given nitrogen
Al in solution
has to be sufficient
control
have already
Sources of nitrogen
of Al and N contents.
discussed
I. F. by careful
of
can be satisfied
AIN
in two
ways:
(i)
by the addition
In small castings,
beyond that which is required
of excessive amounts of Al
deoxidation
for full
avoidance of Type II NhS. Here, the steelmaking

important
the
are
melt
of
carbon content
to deoxidation
oxygen content prior
and the
and final
practice
since these determine the
and hence the amount of Al
(See also Section 2.2.1).
required.
of commercial failures
During the examination

Al contents
from several
foundries,
in excess of 0.15% have been encountered which are
be
totally
to
considered
The failures
superfluous.
in
reported
Appendices 2 and 3 had Al contents of 0.053% and 0.12% respectively,

but in the first
case this
was coupled with
ladle
the dangers of taking
content of
Appendix 3 also highlights
to the T. F.
0.018% which gave rise
a nitrogen
samples to analyse for Al or 'N as AIN',
for
both
to
the observed
these
account
analyses
were
unable
since
incidence
(ii)
of I. F.
In larger
castings
been added, the effects
even when only a modest amount of Al has

of micro-
and (more importantly)
segregation
may be such that areas of the casting
susceptible
to I. F.
This is particularly
are rendered
the case at the centre
rate is also extremely
of
large castings
It
is suggested that under these circumstances,
where the cooling
macro-
an addition
slow.
of
127
-
and/or zirconium would be justified
titanium
with a bare minimum of Al.

for deoxidation,
In this way most of the Al is used
the Ti/Zr
whilst
additions
the danger of encountering
without
deoxidation
after
T. F.
prevent pinholing
The reluctant
attitudes
have already been discussed
towards the adoption of such a practice

in Section 4.3.2.1
Carbon Content
7.4.2
By increasing
the carbon
been shown (Fig.
6.33)
eutectoid
composition
the prior
austenite
Hence it
is possible
network
fracture
behaviour
increasing
I. F. still
that
is no ferrite
when there
grain
boundaries
to discount
during
network
primary
the theory
(Wolf,
1980).
Fig.
that
fracture
change from peritectic

a pure Fe-C alloy)
to solidification
composition.
Few experimental
the peritectic
transformation
cooling.
the presence
for
in a finer
grain structure
fragmentation
than in higher
directly
data exist
to aus tenite
regarding
larger
above this
the effect
of
on the grain size of steels.
occurs during peritectic
carbon alloys,
with a
below -0.5%C (0.51%C for
However, West (1950) and Bibby (1972) have shown that

dendritic
of
intergranular
This coincides
surface.
solidification
formed at
6.33 does show, however,
the carbon content results
on the intergranular
has
it
even at the
occurs
may in some way be necessary
a ferrite
that
of the base composition,
content
and this
grain size for low C contents.
less
solidification
would tend to promote a

Nbreover, Bibby and Beech
(1973) have shown that the size of the columnar region also
decreases as the carbon content of the melt is increased.
128
-
It has been shown in Section 4.3.2 that increasing

tend to increase the susceptibility
content will
increasing
the matrix
the carbon
to T. F. by
(Wright and Quarrell,
strength
1962).
However, another way in which carbon can influence

of AiN in steel,
reducing the solubility
7.5, using the solubility
is shown in Fig.
(1969) and interaction
7.4.3
data of Gladman and

taken from Table 4.3.
coefficients
has been studied
of these two variables
However, the results
the present work.
temperature has little
effect
cases where the primary
increase the density
of AlN precipitates
and Quarrell,
have confirmed
that
the larger
significantly
Any increase
of grain
even with
6.3.3).
been shown to have quite
to I. F. (Lorig
1960).
The results
a slow cooling
(100mm square)
lower Al and N contents
and Elsea,
a marked
1947;
of the present
tends
rate
castings
keel
block
25mm
castings,
square and
explanation
per unit
were not noted,
has in the past
Woodfine
to I. F. in
of excessive superheat would tend to
(Section
200C
of
superheat
rate
suggest that pouring
boundary area, but these effects
The cooling
in
extensively
grain size remains constant.
in grain size as a result
since
is formed.
Pouring Temperature and Cooling Rate
Neither
effect
the
product of A1N at 1300C
of carbon on the solubility
Pickering
thereby increasing
temperature and the amount of A1N that
precipitation
The effect
T. F. is by
to promote
exhibited
has already been discussed in Section
I. F.,
I. F. at
than the smaller
(Table 6.4).
work
75mm
One possible
7.3.1.
129
-
the cooling
In normal foundry practice,

by the physical
fixed
usually
such as the need to avoid

been noted
already
imperative
determine
of the cooling
of small
are these
of the casting,
to contain macro-segregates.
thermal
slowly
it
castings
There is,
bars which
concerns
used to
are often
must be
It
of a casting.
likely
to be cooled
but
they are also
Both these factors
is
however,
and that
effect,
has
It
stresses.
cooled
rate
and considerations
significantly
unlikely
tend to reduce
of the test bar to I. F., and any results
the susceptibility
must be treated
test
properties
not only
than the bulk
faster
cast-on
the mechanical
remembered that
of the casting
high Al and N contents.
to avoid
the relevance
excessive
in large,
that
implication
another
size
is
rate of a casting
to the parent casting.
caution when applied
with
The present work has, however, shown ways in which any susceptibility
to I. F. may be emphasised by other means in order to take such
factors
for
into
For example, it
account.
I. F. in a quenched and lightly
(see Sections
6.3.4,7.2
test bar gives a fully

further
this
7.4.4
tempered test
is intended to be used in the as-cast
the casting
state
may be prudent to test
test
fibrous
should be carried
and 7.4.4).
fracture
bar even though

or normalised
Moreover, if
the
at room temperature,
out at a lower temperature,
can also emphasise any tendency for
a
since
I. F., as shown in Fig.
6.45.
Heat Treatment
The effect
of relative
matrix
been
in
Section
noted
already
to grain boundary strengths

7.2.
It
is important
I. F. may not only be enhanced by the effects

disguised.
be
may also
has
to realise
that
of heat treatment
it
-
For example, in the as-cast
or as-quenched
130
condition,
cleavage
in pearlite
I. F. will
tempered
occur by a fibrous
the fact
to reduce the yield

In both
at temperatures
fracture
[Al]
13000C.
In steels
in this
[N]
x
solubility
lower
containing
and Woodfine
product
of only
of a 0.17%oAl-0.017%N
and that
(Fig.
5x
claimed
implications
virtually
and burning
may be
the reason,
of using
preclude
Also at these temperatures
dangers
of overheating
added
it
mode was simply

Whatever
strength.
and
a reduction
in excess of 1200C and the high cooling
in
industry.
method
4.4) which
10-4 at
at 1250C, but
fracture
that the practical
necessary to avoid reprecipitation

this
the
by water quenching
(1962)
treating
case the intergranular
is considered
temperatures
to redissolve
amounts of Al and N, Lorig
and Quarrell
in
by
the matrix
changes
masked
it
treatment
for AUN in austenite
in the amount of I. F. by heat

that
the
This is only to be expected from
data available
an
(1947)
may
to be inadequate,
of up to 13000C followed
intergranular.
remains
predicts
Elsea
however,
in a coarsening of the precipitates,
the solubility
annealed
fracture
of this work have shown that treatment
merely results
is
and
is not considered to be of commercial significance.
A]N precipitates
steel
6.34),
the steel
cases,
one of
no T. F. is observed.
The use of a high temperature solution
The results
(Fig.
strength
are likely
properties
that
if
Similarly,
mechanism.
mechanical
resulting
mechanism is often
respectively
or martensite
be observed.
rarely
or extensively
despite
fracture
the most favourable
(Section
rates
the use of
there are the
3.4.2.2).
131
7.5
The Effect
The results
of
Properties
T. F. on Mechanical
programme have highlighted
of the mechanical testing
in
intergranular
the
which
presence
of
an
ways
several
of A1N can affect
conditions
important
particularly
embrittlement
7.5.1
The temperature and
mechanical properties.
employed have been shown to be
test
of the specific
in determining
the extent
to which
may be detected.
Tensile
Properties
In the simple case of a room temperature uniaxial

the presence of I. F. results
measured by both the
in a deterioration
elongation
depend on the relative
boundaries to the tensile
of the embrittled
would be expected.
these properties
Chandley (1962) obtained reductions

intergranular
32.2% for fully
ductile
for
40%
R/A
of
values
pronounced the larger
indicates
The variation
of the casting
in tensile
Therefore,
that
of the matrix
'intergranular'
respect
becomes more
(Fig.
fracture
to the microstructure
even if
in relation
a tensile
with
fracture
6.40).
is
worse than this.
temperature
strength
Bearing
actually
result
to meet the specification,
may be significantly
properties
and
This compared to typical

The effect
material.
piece.
in
in area ranging from 5.5% to
fractures.
dependence of the intergranular

strength
For example, Harris
I. F. with an adequate ductility
the properties
grain
the grain size of the material
to the size of the test
largely
will
and hence a wide variation
axis,
as
in area (Table 6.6).
these properties
orientation
test,
tensile
of ductility
and reduction
to which I. F. affects
The extent
network
indicate
on the yield
in mind once again
transgranular
with
present at the time of testing
this
is
132
not unexpected, since the strength
on the ease of void nucleation
this
case the AIN).
in the ductile
(in
at second phase particles
temperature is increased,
As the testing
the ease of void nucleation
regime depends
at MnS inclusions
also becomes more
favourable,
(Thompson and Weihrauch, 1976), and because of
geometrical
considerations
along the JUN embrittled
fracture
is reached when it
for fracture
manner around the YhS.
been discussed in Section

7.5.2
grain boundaries,
becomes preferable
'trans granular'
a truly
involved
and the constraints
to proceed in
This has already
7.2.
on the fracture
of temperature
behaviour
been
discussed
has
in
Section
already
specimens
is that instead
observation
to mixed I. F. /fibrous
failures
as reported
transition
the relative
In less severely
may not be well
transition
increases
gradually
with
(1960)
The
is from cleavage to I. F., and the
of the matrix
embrittled
from cleavage
by Wright and Quarrell
failures,
This behaviour has been interpreted

strengths
The main
in two transitions.
higher temperature one from I. F. to fibrous

in Fig. 6.43.
of impact
7.2.
of a simple transition
3.1) the presence of I. F. results
lower temperature
In this
a temperature
Impact Properties
The effects
(Fig.
in
steels,
as shown
in terms of
and grain boundary (Section

however, the double
defined and the impact energy absorbed
increasing
temperature as in Fig. 6.45.
difference
is
large
there
not
a
case
between the inter-
and hence the I. F. is only manifest
and intragranular
strengths
over a relatively
small temperature range.
7.2).
133
of I. F. on the impact
The effect
that
6.43 is
of Fig.
region
increasing
impact
shown in Fig.
6.44,
83 -
can be seen
and it
in a decrease
the amount of I. F. results

the empirical
energy which satisfies
E (in J)
in the mixed I. F. /fibrous
energy
relation
0.685 x(%I. F. ).
Hence, even in samples which were 100% I. F. the impact
was still
The reason for this
-15J.
proportions
features
These do not appear to be a function

mixed mode regime, and are likely
parallel
on the fracture
boundaries will
the
to depend on the orientation
to the grain boundaries.

the specimens so that
of the notch root relative
have given rise
surface.
of temperature within
to the length of the columnar grains,
the exact position
there
region,
which correspond to the differing
of I. F. and fibrous
was minimised by notching
some micro-ductility.
the mixed I. F. /fibrous
of results
of the test piece relative
energy
is the mechanism of I. F.
7.2, which incorporates
Fig. 6.43 shows that within

is a large scatter
in
to significant
This effect
fracture
occurred
but inevitably
to the grain
variations
in %I. F.
and impact energy.

The effects
of matrix
shown in Figs.
hardness on impact properties
6.49 and 6.50.
600C decreased the temperature

and improved the upper shelf
show that
Increasing
the tempering time at
interval
over which I. F. occurred
energy.
The fractographs
for hardnesses above HV30 = 200 (tempering
less than two hours) the steel

range of testing
temperatures
the low upper shelf
have been
exhibits
in Fig.
6.50
times of
some I. F. over the whole
investigated.
This corresponds to
energies observed for casts 6B, 6D and 7A.
- 134 -
Cast 7B, which was tempered to a hardness of HV30 = 182, exhibited

and this
I. F. over a narrower range of temperatures

disappeared at temperatures
it
behaviour
of the matrix
(Fig.
boundaries,
grain
of the matrix
and finally
contracted,
(Fig.
and I. F. is observed
7.6(b))
so that
tempering
after
time
for
7.1,
the yield
of the
over a range
reduces
the
is
the I. F. regime
8 hours,
it
disappears
7.6(c)).
Fracture
7.5.3
7.5.3.1
Toughness
COD for
The main feature
Crack Initiation
position
not until
of the properties
some slow fibrous
This may involved
the crack front
(Fig.
The
localised
of the embrittled
6.57).
and
of
crack coincides
the CODvalue measured

of the matrix.
It
is
crack growth has occurred that the
crack encounters an embrittled

propagate.
to
except for the distribution
of A14 precipitates,
be representative
6.51).
from the highly
unless the root of the fatigue
a line
(i)
of
crack tip with respect to the embrittled
samples are identical
AIN precipitates,
exactly
(Fig.
Since the microstructures
grain boundaries.
with
was the insensitivity
temperatures.
is thought to arise
of the fatigue
unembrittled
results
measured CODfor crack initiation
the presence of I. F. at all

for
this
reason
(Si)
of the CODtest
the conventionally
will
tempered material
the tempering
(Fig.
energy of -60J.
compared to the strength
7.6(a))
Increasing
of temperatures.
strength
is high
cast 7D (HV30 = 170)
model in Fig.
the strength
with
in the lightly
can be seen that
strength
Finally
any T. F. and had an upper shelf
did not exhibit

Comparing this
above 50C.
had almost
grain boundary along which it

a significant
can
step in the plane of
135
This highlights
a problem which often
and the need to consider
testing
should be emphasised,
extension
invalidate
for
has been reported

who found that
5i was not sensitive
found difficulties
tip
the HAZ.
within
high
specificity
have also
explain
crack
Gittos
The crack
tip
been cited
observed
anomalies
zone (HAZ)
in locating
the fatigue
positioned
and the remainder
toughness
to
(1979)
was correctly
by Ritchie
during
and Brook (1975)
of T. E.
and Dolby
of the COD. The effects
values
example
growth prior
the heat affected
20% of the specimens examined,
erroneously
Another
to the presence
Similarly,
in measuring
of crack
by Berry
steel
of welds because of the problems
toughness
in only
by a test.
of slow ductile
failure.
intergranular
toughness
in many cases these may
since
a temper embrittled
because of the initiation
crack
the micro-mechanisms
data generated
the numerical
in fracture
arises
gave
of crack tip
et al
(1976)
to
4340
of AISI
testing
steel.
COD at Maximum Load (Smax)
7.5.3.2
Fig.
6. S2 has shown that
of COD at maximum load
(S)
quite
governed by necking
is largely
6
max
the sample after
the initiation
and is
sensitive
therefore
same way as is the tensile

effects
have little
dependent
is
measured
crack
tip,
intergranular
This
in the uncracked
to the presence
ductility.
is because
ligament
growth
(Knott,
of
1973c)
of I. F. in much the
Fatigue
location
crack
on 5max, because the parameter

on properties
and which are averaged

In a sample tested
cracking
the value
significantly.
of slow crack
influence
being
the sample.
of I. F. lowers
the presence
from the
some distance
over the cross-sectional
under displacement
may take place
by rapid
area of
control,
bursts
ahead of the
136
-
front
crack
main
load-bearing
5
om.
after
initiation.
it will
been initiated
it would be expected that once I. F. has
propagate rapidly
Commentary on Sc, di,
Someof the considerations
to
and give rise
6,, and Smax
involved
in choosing a 'critical'
design
have
for
been outlined
COD
the
purposes
of
is unanimously accepted as being a critical

process (Harrison,
is Sc, which
event in the fracture
1980).
It is only in the last

on the need to detect
10 years that emphasis has been placed

initiation
and to record Si values.
more pessimistic
are considerably
with
than are 6max values and there is still

is more relevant
to service
regard to crack-tip
discussion
application
of maximum load CODvalues.
consideratirnswhich
geometrical
bend-test
will
underestimate
from other configurations.

been based quite
and Harrison
successfully
These
ductility
as to which
(Knott,
Towers and Garwood (1979) have put forward an argumnt

the application
value
in Appendix lb.
The only value of CODfor which there is no ambiguity
figure
which
failure.
catastrophic
7.5.3.3
of load control
under the conditions
apply in service,
usually
tend to reduce the
area of the sample and hence reduce
cross-sectional
In contrast,
This will
1973c).
justifying
This was based on
suggest that the results
from a
the toughness which may be expected

Certainly
designs have in the past
on du and Smax data (Knott,
(1980) advocates their
continued use.
1973c),
137
-
Hence, with regard to the specific

that if
this will
problem of I. F., it
appears
a design is based on the CODfor crack initiation,

be sufficiently
conservative
lowering of toughness as a result
to incorporate
of I. F.
mode of failure
any
In normal circumstances,
however, the use of 6max or other design criteria

intergranular
di,
cannot be tolerated.
mean that an
138
Chapter
Conclusions
8.1
The precipitation
on the as-cast
boundaries is a major cause of intergranular

It
castings.
8.2
is not,
from excessive additions
results
high
bulk
with
a
nitrogen
coupled
aluminium
also exacerbated by a slow cooling
macrosegregation
during the later
form of A1N.
The latter
in some cases this
grows into
Examination of the atomic arrangements within

close matching with
8.4
For a cooling
section.
Hence the inability
in the optical
{111}Y.
these planes reveals
50nm. This means that
of the A1N
the A1N can
in a metallographic
to detect
a grain boundary network
microscope cannot be taken to imply freedom from I. F.
The mechanism of fracture
testing
(0001)A//
the thickness
be resolved when viewed optically
rarely
the austenite
<110>y.
rate of 0.1C sec-1,
is approximately
precipitates
8.5
<1010>A//
of
precipitation
side of the grain boundary with
grains on either
solute-enriched
for
subsequent solid-state
nucleus
act
as
a
may
a plate-like
At high
stages of solidification
There is evidence to suggest that
liquid.
the
to IF even though the
in two morphologies.
form can occur in the residual
dendritic
In large castings,
rate.
are not high.
A1N often precipitates
temperatures
of
It is
content.
of Al and N may give rise
bulk Al and N concentrations

8.3
in steel
however, the only cause.
IF usually
AIN-induced
fracture
grain
and embrittled
steels
changes with the temperature

exhibit
a full
transition
from
of
139
-
to fibrous
cleavage to intergranular
failures
fracture
temperature.
Because the 'intergranular'
transgranular
with respect to the microstructure
extent dependent on matrix
fracture
inclusion
seen on
of decohesion at
interface.
The 0.300-1.5OMi steels
examined were most susceptible
I. F. in the quenched and tempered condition,

strength
for the highly
facets often
These occur as a result
surface.
the A1N/matrix
8.6
oriented
the fracture
Here,
acts as a void-initiating
AMNis responsible
and the plate-like
reflecting
however,
possesses some microductility.
form of the nitride
the dendritic
the
grain boundaries are linked
Above the DBTT of the matrix,
by areas of cleavage.
the intergranular
are to some
At low temperatures
properties.
of AIN on the as-cast
precipitates
path is usually
present at the
the micro-mechanisms of failure
time of testing,
increasing
with
is high compared to the strength
to
when the matrix
of the A1N embrittled
boundaries.
8.7
The Charpy impact
intergranular
energy
fracture.
region
8.8
of the curve:
Initiation
little
showed
steels
despite
condition,
between the impact

fracture
intergranular
of
amount
E (in
to the presence
sensitive
For the 0.30C-l.
the quenched and tempered

was established
is
5O h steel
an empirical
energy
observed
studied
the overall
in
because
all
was
in
relationship
and the
in the mixed IF/fibrous
Joules)
= 83 - 0.685x(%I.
F. ).
values of the crack opening displacement

difference
of
between embrittled
change in fracture
cases above the transition
(Si)
and unembrittled
morphology.
This
temperature,
fast
140
-
intergranular
fracture
was preceded by slow fibrous
at the root of the fatigue

at maximumload
steels
8.9
crack.
However, values of the COD
were significantly
max)
than for the unembrittled.
Heat treatment
fast cooling
lower for the embrittled
to remove I. F. from embrittled
impractical
be
to
considered
rates required
crack growth
castings
is
because of the high temperatures

to dissolve
and
the AUN and avoid
reprecipitation.
8.10
The precipitation
and Zr for final
of A1N can be avoided by the use of Ti
deoxidation
after
the addition
of a small
amount (<0.02%) of aluminium.

8.11
Results obtained
should be treated
levels
from test bars taken from large castings
with caution.
of segregation
Differences
may mask any tendencies
in cooling
for
I. F.
rate and
Acknowledgements
I am most grateful
G. J.
Professor
Davies
and encouragement
Science
Trade Association
during
and co-operation
of this
the course
and Steel
of numerous people,
exception.
and friends
at the University,
contributions.
like
on the interest
and this
one has been no
to thank all
my colleagues
at SCRATA,and at home for their

In particular,
I would like
Kate Croft,
John DeVine, Naila Dinis,
Ted Needham, Ernest Ridal,
Alan Sheldon, and last
but by no means least,
this
a special
thesis
to
three years by
Bob Hough, Steve Joel,
Finally,
and to the
of funds.
help
the
given to me over the last
acknowledge
Beech, Martin Bridge,
guidance
Research and
depend to a large extent
I would therefore
'Bill'
their
work,
Castings
for the provision
Most research projects
for
and Dr. W. J. Jackson
Research Council
own personal
Dr. A. R. Entwisle,
to my supervisors,
Kevin Selby,
my parents.
word of thanks to Mrs. Anne Bower for typing
much faster
than I could write
it.
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Laboratories.
APPENDICES
-Al-
APPENDIX1
Fracture
la.
Sample size
BS 5447 (1977)
the .crack
(KIC)
2.5
cry
Toughness Testing
requirements
that
specifies
(a)
length
for
valid
for
a valid
Initially,
the test
of the material
of the KIC of the material
(preferably
an over-estimate)
To take into
to the size requirements
account uncertainties
the KIC value and the possibility

other validity
under the
of 0.2% P. S. to Young's Modulus which
be
related
can
of the test
BS 5447 further
criteria,
via a table.
such as underestimation
not meeting
recommends that
Using the data of Selby (1977) for a 0.23C-1.25bh steel,

KIC value for the 0.30C-1.50Nh steel
3"2
be
to
-120Mir
estimated
.
Therefore,
is
in equation
ay
370NNm 2,
(la. 2), Bz4
the
used in this work was
The minimwn value of the proof stress

material
the
(l a. 2)
B>4
this
of
of sample size should be
for selection
(Ziyy) 2
for
than
dimensions
should be based on either
piece
An estimate
The ratio
criterion
less
(la. l)
of test.
or
be not
conditions
ii)
both
KIC measurement,
(B) shall
and the thickness
0.2%
is
the
proof stress
ay
where
i)
KTC measurements
given in the specification

(BS 3100 AS, 1976)
2
370
= 0.42m
-A2-
i. e.
the minimun thickness
With a typical
thickness
that in order to obtain
B=
420mm.
to width ratio
a valid
of 0.5,
KTC result
this would mean
the samples would have
to be of the approximate dimensions 4m x lm x 0.5m.

lb.
i)
Procedure for the Calculation
of CODValues
Nomenclature
Symbol
Term
Test piece width
Test piece
Notch width
Effective
Distance
thickness
crack length
of clip
gauge location
from test
piece
surface
force
Pf
Fatigue pre-cracking
Stress intensity
coefficient
Stress intensity
factor
Applied
Clip gauge displacement
Value of crack opening displacement
ay
0.2% proof stress
Young's
Poisson's
Additionally,
force
Nbdulus
ratio
the following
fracture
in
the
events
(see Fig. Al. l)
(compliance function)
suffices
process,
are used to denote significant
and can be applied
to P, V and S
-A3Event
Suffix
fracture
Onset of unstable
brittle
or an arrested
This term only applies where
crack.
there is no evidence to suggest prior
slow
crack growth.
i
Initiation
max
Point of first
Onset of unstable
of slow crack growth.

of maximun load.
attainment
fracture
or an arrested
crack which has been preceded by
brittle
slow crack growth.
ii)
of a tCriticalt
Event
where unstable
fracture
Definition
For situations
prior
growth,
slow crack
is
process
of affairs
clearly
the critical
at low temperatures,
takes
event
by dc.
represented
in the Fracture
This
place
Process
without
in the fracture
is
the normal
as shown schematically
state
in
Fig. Al. l (a) .

However, at temperatures where slow crack growth precedes either
rapid
fracture
the critical
either
i,
of a maximumforce plateau
or the attainment
event
Su or
in the fracture
m,
(Figs.
The choice of an appropriate

the design criteria
process
Al. l(b)
collapse,
value.
and (c)).
value depends to a large extent on
or component can be tolerated.
then Si would be chosen as a critical

If
by
which are being used, and whether or not slow
in
a structure
growth
crack
displacement.
may be represented
the design criterion
then it would be appropriate
If not,
value of the crack opening

is based on plastic
to consider
6max as a critical
-A4Calculation
iii)
of COD Values
The case of an inembrittled

be considered,
will
load vs.
clip
tested
steel
and the autographically
gauge displacement
of the fracture
photograph
length
the crack
of
gauge 1 (Vl)
A1.2 and A1.3.

was used for
surface
traces
plotted
1y1) and clip
gauge 2 (V2) are shown in Figs.
clip
at room temperature
vs.
An enlarged
measurements of
Ca).
The specimen dimensions (B, W and N) were measured using a

micrometer prior
to testing.
Fig. A1.2 shows that fracture

a slow crack and that
first
of the crack was determined by noting
double
in
the
of
slope
clip
change
V1 axis in Fig. A1.3.
This clip
load for the initiation

initial
the
to
tangent
a
possible
to measure the plastic

at initiation
displacement
The equations
towards the
gauge plot
graph to determine the
of slow crack growth (Pi).

elastic
the
gauge displacement was then
onto the load/displacement
translated
of
of the sample has occurred.
general yielding
of initiation
The point
has occurred by the initiation
region of this
By constructing
curve,
component of the clip
(Vp)i,
used for calculating
it was
gauge
as shown in Fig. A1.2.

CODvalues were originally
due
to Dawes (1976) and are as recommendedby BS 5762 (1979).

K2 (1 - v2)
S=
2QE
y
where
K=
Y
and
of a/W.
0.4
(W - a) Vp
0.4W + 0.6a
YP/BWI
is determined from tables
(lb. 1)
+Z
(lb. 2)
of the compliance as af mction
-AS
Hence for
sample 46/1D,
a=
20.08nn
B=
20.12mm
W=
40.00mm
is
the calculation
(measured on fracture
measured prior
as follows:
surface)
to testing
N=2.52mm
a/W = 0.502 which gives Y= 10.68 from Table 1 of
',
BS 5762 (1979).
ay
= 348NNm'2 (from independent tensile
P.
= 23800 N
(Vp)
--
BWI
in equation
1997.52
6=
i2x
Si
(lb. 2)
10.68 x 23800
20.12 x (40.00)2'
Y_
'.
A1.2.
0.185mm
from equation
K
measured from Fig.
tests).
(lb. 1) and taking

(1 - 0.32)
348 x 207571
3/2
1997.5 Nmm
0.4
E=
207570, v=0.3
(40.00
20.08)
-
()x
0.4 x 40) + (0.6
and Z=3.6m
x 0.185
20.08) + 3.6
= 0.072mm
Similar
calculations
significant
points
can be used to determine the CODat other

on the curve.
Cl
fit'
CO
LU
Z
U. i
4-i .
vi
&0
Gg
%
J
cu
,
41
U
-H
"
o-0
au
d OVOI
C)
4-1
i
LM
C) b
cu
2+ c3 0
,.
30
20
PMU
tp.
P
(kN)
10
u5iu1.5
Fig.
A1.2
2.0
Vl (mm)
Load/clip
gauge displacement
46/iD at room temperature.
0.5
Vs(mm)
for
curve
COD sample
crack
initiation
0.25
025
Fig. Al. 3
0.50
V2(mm)
0.75
Clip gauge (Vl) vs clip gauge (V2) curve for COD

Initiation
sample 46/1D at room temperature.
of
slow crack growth is defined at the first
significant
change of slope towards the V1 axis.
2.5
-A6APPENDIX 2
Director:
J. A. Reynolds, B. Sc., Ph. D., F. I. B. F., F. I. M.
Castings
Steel
Research
and
Trade
Association
la
Your reference:
Registered Office: 5 EAST BANK ROAD, SHEFFIELD
Our reference:
Telephone: 0742 28647
Telex: 542811 C R. T.A. Sheffield
29th February,
1980
Report No. NQ/E 19753

Report
to
Foundry 'A'
Investigation
into
the Fracture
of a Mill
Housing
by
N. H. Croft
Introduction
The aim of this investigation
was to determine the cause of
failure of a large mill housing which had fractured in a coarse interfracture of cast steels has frequently
granular manner. Intergranular
been associated with the precipitation
on the
primary (as-cast) grain boundaries (Refs. 1-5), but this is by no means
the only possible cause. Other factors which may result in failure of
this kind are the presence of a ferrite
network, extreme Type II
inclusions,
manganese sulphide
or small internal hot tears, all of which
favour preferential
crack propagation along the grain boundaries.
Chemical Analysis
C%
0.35
Si%
0.36
Mn$
1.11
P%
S%
0.022
0.033
Cr%
0.06
Mo%
<0.02
Ni%
0.08
Al%
(total)
0.053
Hardness
HV30 = 174 +3 in the as-received
A Company limited by guarantee.
condition.
Registered Number 516 791, England
Cu%
0.05
N%
(total)
0.018
S2
-A7Microscopical
Examination
Samples cold sawn from the mill housing were fractured

by slow
bending, and confirmed the coarse intergranular
three-point
mode of
(Fig. 1).
failure
Microsections
taken from a region near to the fracture
surface
fracture
showed no apparent reason for the intergranular
when viewed
In the unetched condition,
under the optical
microscope (Fig. 2).
the
inclusions
observed comprised Type III manganese sulphides,
and oxide
inclusions
from primary deoxidation.
It was not possible
resulting
to
but these are invariably
resolve any precipitates
of aluminium nitride,
very fine and can only be seen using electron
techniques.
optical
After etching in 2% Nital,

the structure of the as-received
be
to
a mixture of fine equiaxed ferrite
casting was shown
and pearlite,
suggesting that the component had been normalised.
There was no evidence
of a ferrite
network.
Samples were cold sawn from the fracture surface-and mounted
500X Scanning Electron
on aluminium stubs for examination in a Philips PSEM
Microscope.
In addition,
a polished microsample taken from a position
perpendicular to the fracture surface, and incorporating
the root of an
intergranular
crack, was also mounted for examination.
The fracture surface, when viewed at a relatively
low magnification,
revealed features typical of a "Rock Candy" fracture caused by the
(Fig. 3). The coarse intergranular
presence of aluminium nitride
facets
(Fig. 4), interspersed with
exhibited large areas of cleavage fracture
features
terrace-like
platelet
oriented on the
fracture surface.
Also in evidence, though much less common, were fine
dendritic
features, which can also be seen in Fig. 4. Energy dispersive
X-ray analysis of the fracture,
using a LINK system showed an increase in
the amount of aluminium on the surface of the platelets,
but unfortunately
it is not possible to detect nitrogen using this technique because of
atomic number limitations.
Examination of the polished microsection in the SEMshowed
into
the matrix ahead of the crack
extending
needle-like
precipitates
tip (see Fig. 5), and again these regions appeared slightly
enriched
in aluminium.
Positive evidence as to the cause of failure
resulted from the
of
the transmission electron microscope (TEM). Carbon extraction
use
replicas were taken from a freshly fractured surface, using an electrolytic
etching technique to remove the carbon film from the fracture.
Examination
in
these
a Philips EM301 microscope revealed networks of
replicas
of
precipitate,
a grey plate-like
which was heavily fractured,
presumably
fracturing
during
the
either
of the steel, or as a result of the replication
technique (see Figs. 6 and 7). These were identified
as A]N using selected
diffraction,
the observed "d" spacings being within 1% of the
area electron
for
(hexagonal structure with a=b=3.11.
values
aluminium nitride
publishe
C=4.99A).
-A8Also present in occasional

precipitates,
areas were grey dendritic
by electron
diffraction
again identified
as A1N (Figs. 8 and 9), and
in some cases these were continuous with the plate-like
(Fig.
precipitate.
9).
Discussion
From the results of the microscopic examination, it is clear that

fracture of the mill housing results from the
the coarse intergranular
(mainly
in the form of plates) on
nitride
aluminium
of
precipitation
the as-cast
grain
boundaries
during
primary
cooling
of the casting.
Although the aluminium content of the steel is not unduly high

(0.018)
is well above what would
0.053%,
total
the
nitrogen
content
at
for
be
a steel of this composition,
expected
normally
and it is likely
has been favoured by this high
that the aluminium nitride
precipitation
together with a slow cooling rate through the precipitation
nitrogen
content,
temperature range (between 1100C and 7000C).
Woodfine (Ref. 3) has described a method of removing intergranular

fracture by heat treating at high temperature to dissolve the aluminium
followed by rapid cooling to avoid reprecipitation
in the massive
nitride,
form. However, this does not provide a practical
solution in this instance,
dissolve
0.053%Al
to
the
temperature
required
since
and 0.018%N would be
(Calculated
from
in
1300C.
thermodynamic data given by
of
well
excess
Gladman and Pickering in Ref. 6).
Nbre preferable would be to prevent precipitation
of the grain
in future castings of this type, and here there are
boundary nitride
three possibilities:
i)
ii)
iii)
Endeavour to keep the nitrogen

Increase the cooling
range.
content at a lower level
rate through the precipitation
(-0.01%).
temperature
Use titanium,
as reported by Woodfine (Ref. 3), in addition
to aluminium to form the more stable TiN which does not
in
forms
massive
at the grain boundaries.
precipitate
Conclusions
fracture of the mill housing has
The coarse intergranular
boundary
from
the
of
a
grain
presence
network of aluminium
resulted
during
primary cooling of the casting, and probably
precipitated
nitride
in the temperature range 1100C-700C.
References
and A. R. Elsea.
Trans. A. F. S., 55,160
1.
C. H. Lorig
2.
B. C. Woodfine and A. G. Quarrell.
3.
J. A. Wright and A. G. Quarrell.
4.
W. J. Jackson and J. Bradshaw.
S.
M. p. Sidey.
6.
T. Gladman and F. B. Pickering.
J. I. S. I.
J. I. S. I.
(1947).
195,409
200,299
(1960).
(1962).
SCRATAJ. of Research No. ' 11, Dec. 1970.
Iron and Steel 40,269
(1967).
J. I. S. I.
205,653
(1967).
A9
-
Fig.
fractured
Macroscopic view of the freshly
bending.
broken by slow three-point
Fig.
Microstructure
from a section
taken near the fracture
fine equiaxed ferrite
and pearlite.
surface,
revealing
Mag X75
Etch:
2% Nital
surface,
A10
-
Fig.
Low-power
fractured
scanning
surface
electron
revealing
micrograph
of
"Rock
typical
a freshly
Candy" features.
Mag X80
Fig.
Scanning electron
micrograph showing the system
of platelets
at higher magnification.
Mag X320
All
-
`
''
`
i
;.
/
*
Fig.
Scanning electron
micrograph showing needle-like
extending beyond the root of the crack.
precipitates
Mag X320
A12
-
AWA.,
i.
I
if
. ,.
Fig.
Transmission
electron
micrograph of a direct
carbon
extraction
replica
of the fracture
surface,
showing
heavily
fragmented
the
plate of aluminium nitride.
Mag X22000
Y,
"f
,Y
L
+'t
}
'
,!
Fig.
Transmission
electron
micrograph showing the
aluminium nitride
plate in more detail.
Mag X36000
A1.
)
-
t.
f
. `.
46 "..
Fig.
Transmission
electron
micrograph of a direct
carbon
fracture
the
The
surface.
of
replica
extraction
form of the precipitate
dendritic
be seen.
can clearly
Mag X28000
,: 1'
1
.r
M,.
Fig.
Transmission
micrograph
electron
showing the continuous
nature of the dendritic
and plate-like
precipitates.
Mag X5900
U
0
O
a,
I-
0
O
0
z
U
QZ
OR
U,
OO
U
0
0ocoC000o
0
N
Co
r'
0
r'
of
I"
N0
r-
Co
e-
(wdd) N3DOa1IN
00N
A14
APPENDIX 3
Director:
J. A. Reynolds, B.Sc., Ph.D., F. I. B. F., F. I. M.
Steel
Castings
Research
and
Association
trade
Registered Office:
Your reference:
Our reference:
5 EAST BANK
Telephone: 0742 28647
24th June,
to
Foundry
'B'
SHEFFIELD
S2 3PT
Telex: 54281 S.C R. T.A. Sheffield
1980
Report No. '4/E

Report
ROAD,
134
on
Cracking of a 0.35%C 'Spider'
Casting
by
N. H. Croft
Introduction
Severe cracking problems have been encountered in the
These
region of the feeder head of a 0.35%C, 0.7%Ma spider casting.
in nature, and slow bend tests
cracks appeared to be intergranular
performed on samples taken from the casting revealed small areas of
faceting.
Moreover, chemical analyses carried out at
intergranular
the foundry implied a pick-up of aluminium near to the feeder head
(0.11%Al compared to a ladle analysis of 0.06%), suggesting JUN
as a possible cause of the cracking.
precipitation
The casting had a finished weight of approximately 8 tonnes,
having been made from a 16 tonne electric
arc heat. This was the
fifteenth
and was the first
casting in a batch of fifteen,
one to
exhibit cracking.
Chemical Analysis
The results
C
Ladle analysis 0.35

Centre of head 0.34
of analyses carried
Si
Mn
0.34
0.69
0.011
0.34
0.69
0.011
A Company limited by guarani".
out at the foundry were as follows: Cr
Mo
0.016
0.24
0.05
0.016
0.25
0.05
pS
Registered Number 516 791, England
Ni
Al
0.16 0.064 0.009

0.17 0.111 0.009
A15
-
In addition,
the AIN contents had been determined by the
Beeghly method and were found to be:
oAIN
%N as A1N
Ladle
0.0017
0.0006
Head
0.016
0.005
Check analyses (spectrographic)

were made at the Department of Metallurgy,
Sheffield thiversity,
on samples taken from the region immediately below
the feeder head and from the bulk of the casting away from the head: C
Si
Head
0.36
Bulk
0.38
MetalloeraDhic
Cr
0.010
0.016
0.23
0.011
0.015 --0.23
Ma
0.32
0.66
0.32
0.67
Nb
Ni
Al
0.06
0.17
0.11
0.06
0.17
0.12
Examination
Sections taken from the cracked region of the casting confirmed

the intergranular
morphology, (see Fig. 1), and micro-sections
revealed
the cracks to be extensively decarburised (Fig. 2), with some oxidation
having
the
occurred.
surface
of
exhibited
one cracked sample, broken open by slow three-point

intergranular
facets (Fig. 3).
large
several
bending,
Examination of a freshly fractured surface of the material in

the Scanning Electron microscope revealed features typical of "Rock
Candy" fractures caused by aluminium nitride
(Figs. 4 and 5),
precipitation
although much of the fracture was by cleavage (Fig. 6), as would be expected
in the as-cast condition.
Discussion
From the results of the chemical analysis carried out at the

it appears that the aluminium content at the base of the
University,
feeder head is no higher than in the bulk of the casting.
Thus, any
having
occurred as a result of the exothermic
pick-up
of
possibility
The most likely
topping compound used can be excluded.
explanation
had
been
be
to
that
additional
aluminium
added to the melt at
seems
some stage after the ladle analysis was taken, thus explaining the
discrepancy between the ladle analysis and the analysis of the
finished casting.
The fact that the aluminium nitride
content of the ladle sample
is so extremely low compared to the product analysis probably results
from the rapid cooling of the ladle sample which has not allowed
for
the A1N to precipitate.
The product sample, however,
time
sufficient
been
have
cooled at a much slower rate in the bulk of the casting,
will
figure will be the one representative
of the
and therefore this latter
It is noteworthy that the total nitrogen
true A1N content of the steel.
content of the steels is the same for both the ladle and product analyses,
in
first
in
instance
been
have
the
that
the
supernitrogen will
and
in
been
have
in
it
solid
solution,
the
saturated
whilst
will
product
the form of the nitride.
A16
Macroscopic and microscopic
have shown the cracking
examinations
from excessive aluminium nitride
to be intergranular,
resulting
Fig. 7 shows solubility
at the as-cast grain boundaries.
precipitation
in austenite(l),
data for aluminium and nitrogen
and it can be seen
that with 0.11%Al and 0.01l%N present, supersaturation

will occur at
temperatures below about 1400C. This, in conjunction with the slow
cooling rate in the region of the feeder head, has resulted in the
formation of cracks under the thermal stresses induced during the cooling
These will have been increased by the change in section
of the casting.
of the component near to the head.
From the extent of the decarburisation

of the crack and the
it
is
estimated that cracking has occurred in the
observed,
oxidation
by
900C
the austenite to ferrite/
and
was
accentuated
possibly
region of
phase transformation.
pearlite
Conclusions
1.
The cracking arose from a lack of ductility

as a result of aluminium
at the prior austenite grain boundaries.
precipitation
nitride
2.
The nitrogen content of the steel

aluminium content was high.
3.
There is a discrepancy between the ladle aluminium analysis and the

in
No
the region of the feeder head was
pick-up
analysis.
product
apparent.
4.
The apparent discrepancy between the AUN content in the ladle and
in the product arises from the rapid cooling of the ladle sample,
form.
A1N
does
time
to
the
The valid
precipitate
give
not
which
analysis is the one taken from the finished casting, i. e. 0.016%A1N.
was not high,
but at 0.11% the
Reference
1.
N. H. Croft.
Fracture.
Fracture Mechanisms in Cast Steels - Intergranular
SCRATAProgress Report No. 2012,12th March, 1980.
A17
-
t
)y
Fig.
Macro-etched
intergranular
section
path.
through
a crack,
showing the
Mag X0.75
--
________
Vv,
4`
-".
, lam
iJ.
fi'r'
O.r
IOF
jp
-'d.
Fig.
. -Wir'~r
"6. I''z
J
i...! rr
decarburisation
the
Optical
showing
micrograph
is
The
fine
ferrite
the
matrix
cracks.
with
210Nital
Etch:
...,..
iF
associated
and pearlite.
Mag X40
A18
-
Fig.
Fracture
cracks.
`,
surface obtained by breaking

Note the large intergranular
4:
.`;
Fig.
`s,
open one of the

facets.
Mag X2
}I
Low-power scanning electron

intergranular
fractured
surface.
morphology of a freshly
Ntag X40
A19
-
Fig.
facet in more detail.

Intergranular
Note the
dendritic
markings, normally
associated with
form of aluminium nitride.
the dendritic
Mag X640
Fig.
Scanning
fracture
electron
micrograph showing the main mode of
during slow three point bending, one of cleavage.
Mag X160
N
6
co
17
C5
ca
N
r
O
J
Q
W
J
m
r
CJ
0
to
o
Co
0
ca
0
6
t
0
'.......,
I=
101 1 iw
-A20-
APPENDIX 4
'Extinctions
The Measurement of
in the SEM
Angles
In the technique used to determine the angular relationships

on intergranular
between A1N plates
thder
before
until
tilt
the plates
circumstances
(see Section
were rotated
as
appeared horizontal
on the viewing
screen
as much as possible.
The additional
angle
they
tilted
were then
tilt,
these
disappear
to make the plates
always possible
6.2.1).
surfaces,
on the goniometer stage of the SEMmeant that it
restrictions
was not
fracture
disappear
to make the plates
a, required
and
of
was then calculated
as follows:
the apparent width of the plate
of maximum tilt,
In the position
(wl).
measured
the
was
viewing screen
on
By tilting
back
through a known angle $, the apparent width of the plate

to a value w2 which was again measured on the screen.
in Fig. A4.1.
shown schematically
to calculate
possible
increased
This is
By simple geometry it was then
a.
In Fig. A4.2, we have

(a + )
and sin
sin a=W
w2
ww
where W is the true width of the plate.

W2
(a +
sin
sill
sina
wl
sina
=
hence
a=
and this
tan-1
+ cos a sill
a cos
cos
+ cot a sin
sin
W21
cos
tilt
was added to the angle of maximmun
'extinction'
angle.
to obtain
the
-A21-
Wz
W7
Max.filt -p
lilt
Maximum
Fig. A4.1
Measurement of wl and w2 on the viewing

the SEN. (cf Figs. 6.17 and 6.18).
screen of
B'
A
AA'= w,
BEY
= wz
S.E.M.
detector
Fig. A4.2
BA
Geometrical relationships
angles of tilt.
positionof max.tilt
extinction position
at the two different
A22
Appendix
Calculation
of the Microsegregation
Al and N during
in Section
As noted
during
2.4.2
can begin
Characteristics
of
Solidification
solute
redistribution
This
results
in the residual
liquid
solidification.
and N content
for
occurs
increases
of Al
of A1N
and precipitation
limit
once the solubility
in local
usually
A1N in liquid
is
steel
exceeded.
data used in these
The solubility
in Section
presented
is
for
(1978a)
Hner and Baliktay
GS-60 grade steel
The limit
4.4.2.
based on the empirical
therefore
log [Al] [N]
-8490
T
For the purposes of this

TS = 1723K. As will
due to
which were
in Fig.
of solubility
7.2
equation
+ 2.37
model, it
is assumed that TL = 1773K and
be seen from Fig.
insensitive
are relatively
are those
calculations
to slight
7.2, however, the results

in estimation
errors
of
these temperatures.
The local
concentrations
of Al and N in the residual
(C1 and CL) were calculated

and three starting
carried
out using
C11 = C
in
equation
as
The equilibrium
was taken
for increasing
fractions
compositions (C- and Co) .

the Scheil
in
equation'
liquid
(fs)
solid
For Al,
this
was
the form
kAl -1
(1 - fs)
2.2 of Section
partition
2.4.2.
coefficient
as 0.6 as determined
of aluminium
by Tiller2
in 6-ferrite
and Oeters
(kAl)
was
and
et a13,
-A23-
during solidification.
assured to remain constant

For nitrogen,
equation
this
which
does not
case,
is
an interstitial
apply,
since
CL was calculated
rl
CL = Co
alloying
back diffusion
rapid
using
element,
the equilibrium
the Scheil
can occur.
lever
In
rule.
-1
(1
kN)
fs]
-
kN was taken to be 0.3,
as determined by Oeters et a13, Chipman4
and SimsS and was again assumed to remain constant during

solidification.
These values
Fig.
7.2.
solubility
CLl x CL
were then used to plot

The points
at which
these
line
the value
of
gives
curves
vs
cross
fs as shown in
the maximum
fs beyond which precipitation
of A1N becomes possible.
References:
Z. Metallkunde,
1.
E. Scheil,
2.
W. A. Tiller,
3.
F. Deters
4.
J. Chipman,
5.
C. E. Sims, Electric
J. I. S. I.,
et al,
Arch.
Physical
1942,34,70.
1959,192,338.
Eisenhuttenwes,
Chemistry
1969,40,603.
of Steelmaking,
Furnace Steelmaking Vol.
AIN,, E (1951),
p.
632.
2 (1962) p. 99, Pub:Wiley.
TABLES AND FIGURES
TABLES
Table 2.1
See Text,
Page
Table 2.2
Nitrogen
of different
contents
steelmaking
routes
(Wright,
Nitrogen
Method of Manufacture
Basic Open Hearth
0.004-0.001'*
Basic Electric
0.004-0.010*
Arc
L-D
Content (wt. 06)
0.008-0.011+
<0.005*
Basic Bessemer - Air
Blown
02
Enriched
Induction
Speith
0.010-0.025*
0.009-0.012+
0.006-0.012*
0.003-0.006+
0.008-0.012+
'blted
Vacuum Melted
1962)
0.002-0.006
and Vom Ende
+ Kuhn and Detrez
Table 2.3
See Text,
Page 24
Table 3.1
See Text,
Page 37
Table 3.2
See Text,
Page 41
Table
4.1
Temperature dependence of the solubility

from various
austenite
temperature
for
a steel
sources,
[Al] [N] in
product
and the predicted
solution
0.1%A1 and 0.01%N
containing
Source
log10
Al
-7400
+ 1.95
Darken et al (1951)
0.1%C, 0.4oMn
-7750
T
+ 1.80
Knig et al (1961)
0.2%C, 1.50%Mn,0.5%Si 1342
-6180
T-
+ 0.725 Erasmus and Mech (1964)
-6015
T-
+ 0.31
Idem
0.15%C, 0.4 Ma, Q. 2%Si 1544+

3.5%Ni, 1.0%Cr
-9200
7-
+ 2.92
Hner and Baliktay

(1978a)
0.40%C, 0.8 h,
-7500
+ 1.48
*Gladp
and
Pickering (1967)
0.1%C, 0.8 Y
"Nban" solubility
prior
product
work.
+ i. e. above the liquidus.
Steel Composition
1221
0.2%C, 1.50oNa,
0.15oSi
incorporating
T(C)
1386
0.6%Si 1281
0.2%oSi 1401
the results
of
Table 4.2
Interaction
parameters eN" and eMx for some commonalloying
elements in liquid
Element
x
steel
eAl
0.091
enx
Temperature
(0C)
Ref*
1600
1600
1600
0.0547
1600
-0.02
1600
-0.047
1600
-0.01
1600
-0.0115
1600
1600
1600-1750
1600-1750
0.123
Si
0.056
Ma
Cr
Ni
Mo
Al
0.043
828
N
1602
-0.912
*Refs.
(1960)
1.
Wilder and Elliott
2.
Schurmann and Kunze (1967)
3.
Evans and Pehlke (1964)
-0.472
Table 4.3
Interaction
parameters eN" and ex
for some commonalloying
elements in austenite
Element
x
eN"
Temperature
(C)
Ref
1100-1300
0.125
1050-1200
0.0595
1000-1200
-114 40 076
r -1- .
1000-1200
32
.4 -10.0056
T
900-1200
-360 +0.136
1050-1350
-0.05
1000-1200
eAx
Al
-2.4
C
Si
Yn
Ni
Cr
Mo
*Refs.
(1973)
1.
Mayrhofer
2.
Schenck et al (1963)
3.
Matasova and 'Luna (1973)
4.
Heckler and Peterson (1969)
S.
Ichise
et al (1971)
Table 5.1
Details
Cast No. Practice
4169
of the Experimental Castings
Pouring
emp.
(e
1565
Si
hh
Al
Total
N
0.28
0.38
1.44
0.10
0.026
Comments
Extensive
porosity.
4176
1560
0.27
0.49
1.54
0.004
0.006
0.18
0.015
Used to examine
effects of heat
treatment.
4210
1560
0.30
0.51
1.76
0.005
0.007
0.17
0.017
Charpies.
4211
1565
0.29
0.49
1.65
0.005
0.006
0.07
0.017
High T heat
treatments.
4231
1560
0.29
0.46
1.55
0.005
0.007
0.08
0.008
Charpies.
4351
1565
0.28
0.38
1.56
0.005
0.007
0.12
0.014
Charpies and
high T heat
treatments.
4353
1550
0.42
0.48
1.55
0.009
0.009
0.20
0.018
Effect
of C
content.
4354
1540
0.56
0.51
1.68
0.010
0.011
0.22
0.020
Effect of C
content.
4355
1550
0.65
0.56
1.63
0.010
0.011
0.21
0.023
Effect of C
content.
4382
1570
0.30
0.42
1.58
0.005
0.009
0.08
0.014
Directional
solidification
work.
4383
1570
0.30
0.45
1.55
0.006
0.009
0.17
0.017
Directional
solidification
work.
46/1
1600
0.29
0.20
1.28
0.010
0.015
0.14
0.009
Fracture
toughness
testing.
46/2
1610
0.31
0.32
1.27
0.010
0.014
0.14
0.008
Fracture
toughness
testing.
46/3
1610
0.30
0.21
1.29
0.010
0.015
0.15
0.009
Fracture
toughness
testing.
46/4
1610
0.28
0.15
1.13
0.009
0.007
0.07
0.011
Fracture
toughness
testing.
Table Continued
Table 5.1
Details
Cast No.
Practice
of the Experimental
Pouring
emp.
(o
Castings
Si
bh
(Continued)
Al
Total
N
Comments
46/S
1610
0.29
0.17
1.23
0.008
0.011
0.22
0.015
Charpies.
46/6
1620
0.31
0.20
1.09
0.010
0.014
0.23
0.016
Charpies.
46/7
1610
0.29
0.26
1.46
0.010
0.015
0.21
0.017
Charpies.
46/8
1610
0.29
0.18
1.11
0.009
0.005
0.08
0.010
Fracture
toughness
testing.
46/89
1620
0.31
0.59
1.37
0.013
0.017
0.18
0.010
Fracture
toughness
testing.
N. B.
The higher pouring temperatures for Practice B and C were to allow

for a 30C temperature drop between the furnace and ladle.
Table 5.2
See Text,
Page 82
Table
6.1
Electron
Camera constant
Zone axis
Diffraction
Data for AUN Plate
R
= 25.4mm
: <0001>
d
(calculated)
dX
(observed)
3210
7200
1.018
1.008
0.99
1.347
1.344
0.20
1210
1.555
1.558
0.21
0220
1.347
1.351
0.33
1230
7110
1.018
1.016
0.20
1.555
1.549
0.39
1100
2.693
2.688
0.20
0110
2.693
2.688
0.20
1120
2020
1.555
1.568
0.83
1.347
1.351
0.33
1010
2.693
2.687
0.20
1010
2.693
2.687
0.20
2030
1.347
1.351
0.33
1120
1.555
1.568
0.83
0110
2.693
2.687
0.20
1100
2.693
2.687
0.20
2110
1.555
1.549
0.40
3170
3300
1.018
1.016
0.19
0.898
0.894
0.20
3310
1.018
1.016
0.20
1370
1.018
1.016
0.20
0330
0.898
0.897
0.02
1340
0.747
0.726
2.85
Diffracting
Planes
% Error
in d.
Table
6.2
Electron
Camera Constant
Zone axis
Diffraction
= 25.4rmn
Data for
A1N Dendrite
: <1123>
d
(calculated)
d
(observed)
7023
1.185
1.181
0.31
3122
0.943
0.937
0.56
4222
0.742
0.726
2.23
1011
7111
2.370
2.363
0.31
1.485
1.451
2.23
3211
0.997
0.996
0.14
X311
0.739
0.726
1100
'1100
2.693
2.688
1.77
`0.20
2.693
2.688
0.20
2200
1.347
1.344
0.20
3300
0.898
0.894
0.38
2111
1.485
1.451
2.23
101
2.370
2.363
0.31
0111
1211
2.370
2.374
0.16
1.485
1.530
3.07
2311
9T2
0.997
1.016
1.86
0.943
0.937
0.56
2022
1.185
1.181
0.31
1122
1.320
1.344
1.84
0222
1.185
1.187
0.16
1372
0.943
0.985
1.69
44,113
0.681
0.667
2.17
3033
0.790
0.782
1.08
2133
0.868
0.864
0.50
1233
0.868
0.864
0.50
0333
0.790
0.791
0.16
1433
0.681
0.671
1.35
Diffracting
Planes
% Error
in d.
Table
6.3
The Angles
between AIN plates
from Measurements
Plate
designation
(in
degrees)
Stage of the S. E. M.
in the Goniometer
53
108
68
39
53
109
31
74
108
109
76
70
68
31
76
71
39
74
70
71
Table la
Angle between plates
Angle between plates
1: 3
= 108
1: 4
68
3: 4
76
2: 3
= 1090
2: 5
740
3: 5
70
Calculated
Table 6.4
The effect of aluminium and nitrogen contents on the room temperature
fracture
mechanism of 0.30C - 1.50bh steel castings
Cast No. Practice
Al (%)
Total
N (%)
[Al]
[N]
Fracture
Dbrphology
x10-
4169
0.10
0.026
2.6
Extensive porosity,
but
remainder 100% I. F.
4176
0.18
0.015
2.7
100% I. F., 0% Fibrous
4210
0.17
0.017
2.9
90% I. F.,
4211
0.07
0.017
1.2
0% I. F.,
100% Fibrous
4231
0.08
0.008
0.6
0% I. F.,
100% Fibrous
4351
0.12
0.014
1.7
50% I. F.,
50% Fibrous
46/1
0.14
0.009
1.3
0% I. F.,
100% Fibrous
46/2
0.14
0.008
1.1
0% I. F.,
100% Fibrous
46/3
0.15
0.009
1.4
0% I. F.,
100% Fibrous
46/4
0.07
0.011
0.8
0% I. F.,
100% Fibrous
46/5
0.22
0.015
3.3
40% I. F.,
60% Fibrous
46/6
0.23
0.016
3.7
50% I. F.,
50% Fibrous
46/7
0.21
0.017
3.6
5011I. F.,
50% Fibrous
46/8
0.08
0.010
0.8
0% I. F.,
100% Fibrous
46/89
0.18
0.010
1.8
90% I. F.,
10% Fibrous
10% Fibrous
The samples had been quenched from 950C and tempered for
bending.
They were broken by slow three-point
ihr
at 600C.
Table
6. S
Sample No.
The Effects
of Heat Treatment
bhchanism
of Cast 4176 (0.27C,
on the Room Temperature

1.50h,
0.18A1,0.015N)
Hardness (Hv30)
Heat Treatment
Fracture
Fracture Mechanism
202
95% cleavage,
WQ
247
10% Fibrous,
90% I. F.
4176/3
900C ihr WQ, 650C Ihr WQ
254
0% Fibrous,
100% I. F.
4176/4
900C lhr OQ, 650C lhr WQ
227
20% Fibrous,
4176/5
900C lhr OQ, 650C ihr WQ
244
5% Fibrous,
4176/6
900C lhr WQ
504
10% Fibrous,
90% I. F.
4176/7
900C lhr air
cool
210
0% Fibrous,
100% I. F.
4176/8
900C lhr
furnace cool
161
60% Fibrous,
4176/1
As cast
4176/2
900C lhr
WQ, 650C Ihr
5% I. F.
80% I. F.
95% I. F.
40% I. F.
0
0
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M
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O
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O
O
O
O
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O
O
. -r
uQ
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e3
0
Cp
"
J-
nZ
c:r
\
"
er
L:.
\
Q
\
\
D
"1"
rt
FIGURES
Fig.
2.1
A breakdown of the areas of application

castings (Haynes, 1974).
of steel
"
i0
Fl
N-O"
i0
^f
ti
8,3
d s=
J
8 ea
8? 8
q=
an
mammas
s=
8 s3
an
2s=
----s
ry
tQ
nqn?
O
4-
Wz
r,
O
s=i
to
$
q
ao
8 s:
4d
0
u
rr
f)
"o"nn-o"a"nr-0
3ONY
4311/15 NI SLN31N0
N39O
C) Z
'"-+
OAN HUM S1V3M jO W3awnN
4.1 r+ J
"14
to
in
"wn-o"0"
a-
G)
og
E
C
W
~
a
a
9
saC
e
k
c
a
S
c
a
i
e !
e
S
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F
2
L
M====
mommma
Hf
VMN-O"WtmN-O
3ONVU 03. LVIS NI SJLN31NOON3OQ jIN HL M S1V3H d0 W39Wf1N
"
"=UZ
rd
a9
frt
U
CD 'n
Q
W
(D
s
a
lR
9$
;
u=
ocôv
CD
--
0.30
I"1
0.25
ATM
ATM
e5
10 ATM
ae 0.20
z
W
}
20 ATM
15400C
0.15
X
0
0.10
o,
o
0.05
0.2
0.4
ao
M6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
CARBON, %
Fig.
in liquid
Carbon/oxygen equilibrium
(Marshall
CO pressures
and Chipman,
2.3
iron at various
1942).
0.05
0.04
0.03
z
I
0.02
0.0I
i
oc
Fig.
2.4
500
1000
Degrees C
1500
The solubility
of nitrogen
gas at 1 atmosphere
in pure iron under equilibrium
conditions
(Darken and Gurry, 1953).
N 0-22
(%)
4.60
11
Al
220
0445
a;
18
o.
'
V
/
Nb
/
S
I
o
0
als
Cr,
0.16
14
a 1z
14
'
Ta
a08
Mn
06
a
W
0
-- --
Co,Ni
02
a
Sx
0
02468
10
-r
Fig.
2.5
12
1L
010j
The solubility
at 1 atmosphere N7
of nitrogen
iron alloys
in liquid
binary
pressure
at 1600C
(Pehlke and Elliott,
1960).
1100
'5
so
25
0
N
z
v
25
01
-el 5C
a
lS
r.
z
100
"'5
'50
Temperature(C,
Fig.
-7.6
Standard free-energy
vs. ternDerature diagram for
1(I55).
Ende,
(Pearson
the formation
and
of metal nitrides
I
---
F4
Z
W
23
NITROGEN
HYDROGEN
A
0.010
IND
z
8
2Z
W
REDUCING PERIOD
OXIDIZING
LADLE
z
0.006 W
0
ac
PERIOD
10
20
30
50 60 70 80
40
TIME AFTER CLEAR MELTED, min
Z3
90
101
}{
i
BATH BLOCKED
OXIDIZING
Z
W
LADLE
0
PERIOD
S,
i
10
Fig.
2.7
20
50
40
60
30
70
TIME AFTER CLEAR MELTED, min
80
in hydrogen content during

Typical variations
furnace
heat
for
31
tonne
arc
steelmaking
a
(a) using double slag practice
(b) using single slag practice
(Stephenson, 1974).
90
Fig. 2. $ Transverse section of an as-cast structure

showing the chill zone, columar zone and
1958).
(Walker,
equiaxed zone
0
U,
0
CL
I
0
Fig. 2.9
FRAG ON
SOLJOJFIED
Schematic solute distributions

in a solid bar
frozen from liquid of concentration Co:
.(a)
equilibri
an freezing
(b) solute mixing in the liquid by diffusion Only
(c) complete solute mixing in the liquid
(d) Partial solute mixing in the liquid
(Davies and Garland, 1975).
MIMIWM
fA
m
J
H
W
-180
Fig.
3.1
0
-60
-20
-100
C
TEMPERATURE
-140
Impact transition
steel showing the
(a) is the curve
(b) is the curve
(Wright, 1962).
20
60
100
curves for a 0.26C-1.50Mi

fracture
effect of intergranular
for a steel containing 0.004N
for a steel containing 0.014oN
0
E
z
D
V
a
D
8"
W
N
N
6"
lZ.
."""
"
ti
LU
.J
d
D
2 .i
+K'"Z
0123
INCLUSION SIZE
Fig.
3.2
Graph showing the effect of

size of dimples observed in
electrolytically
pure iron
inclusions
(Kunio et al,
Di )im
inclusion size on the

fracture
ductile
of
the
FeO
containing only
77).
20pm
Fig.
3.3
NhS inclusions
Type I (spherical)
fracture
surface of a 0.30C-1.50'i
on the fibrous
steel.
dar
:1
20pm
Fig.
3.4
A190.,
inclusions
of"a')0.30C-1.5O
on the
h1 steel.
fibrous
fracture
su,
ice
2C}gym
,. W- 1L
Fig.
3.5
Type III
Fracture
fibrous
(angular)
inclusions
the
is
on
surface ofd a (). 3C-l. 5Oh steel.
2.0
q
Qe.
Spheroidal carbide
1.0
c
L
U,
Plate
lphides
su
Fig.
Elongated
sulphides
3.6
5
Volume
Rearlit ic carbide
10
Effects
of the type and shape of second-phase
ductility
on the tensile
of steel
particles
(Gladman et al, 1971).
20.U
Fig.
3.7
1a
ti
The formation of a shear band between voids at two

band
The
4340
in
AISI
appears
macro-inclusions
steel.
to contain a sheet of micro-voids (Cox, 1973).
f
?
Lattice
resistance
Ti
=
+-rjl
(b)
ce
d/2
d12
(al
Stress
zffo,
(T-Ti)
4k
tI
lllr
Fig.
3.8
The effects
and fracture.
of slip hands in yield
d
diameter
in
band
(a)
a grain of average
slip
(b)
Model as a shear crack (KII mode)
(c)
Stroh's
model for cleavage fracture
based on the attainment
value
of a critical
in
the unyielded
tensile
the
Qmm,,
stress,
of
(Knott,
1973b)
grain
.
Tensile
stress
p
b= z (1111
\\
,,
(101) Slip plane
b =a (OOtJ
(001) Cleavage plane
Length c for displacement

(101) Slip plane
b=2
nb
(111J
I
Fig.
3.9
Cottrell's
model for
cleavage
fracture
(Knott,
1973b).
/.
.\
V%
showing the nucleation

in pearlitic
cementite
Fib.
3.10
Photomicrograph
cleavage crack
1981).
(Knott,
Fig.
x. 11
Macroscopic view of a cleavage fracture

0.30C-l. SO:
hI steel broken at -196C.
of a
i1000
in a
Fig.
3.12
Scanning electron
micrograph showing cleavage
in a low carbon steel.
fracture
Crack propagation
has been from right
(Hertzberg,
to left
1976).
25Nm
Fig.
3.13
Quasi-cleavage,
typical
fracture
of quenched
of the low temperature

and tempered steels.
of a discrete
presence
second phase
exposure
bearing
presence
elemental
to a hydrogenenvironment
to
exposure
liquid metals
exposure
to
a corrosive
environment
exposure
certain
at highapplied
stresses
creep
temperatures:
o1 segregated
impurities
to
neutron
irradiation
high-temperature
fatigue
corrosion
and
stress-relief
cracking
embrlttlement
Fig.
Fig.
3.15
3.14
The various circumstances

under which steels
intergranular
known to exhibit
embrittlement.
The micrograph in an SEM image of a tempersteel (Banerji
1980).
embrittled
and Briant,
are
Schematic representation
of the cohesion between
two atoms as a function
of separation:
Go is the
equilibrium
separation,
to a minimum
corresponding
in the force-distance
relation,
and am is the
maximum cohesion beyond which fracture
should occur
(Hondros and McLean, 1976).
2200
5Ft-n
FSn
1800
`.
ppaC
"
11400
11000
Cu -Sb
s2,
c
.o-
Cu-l
600
0a0001
vwVI
0101
Sakiti
Fig.
3.16
eoncentrotlon
0-1
jC
atone ,o
A logarithmic
plot showing the dependence of surface
Grain
boundary
bulk
content.
solute
energy on
behaviour
(Hondros
thibit
similar
and McLean, 1970).
energies e:
Fig.
3.17
fracture
Typical
from a hot tear.
surfaces
Note
features
the dendritic
and the oxidation
the
of
The central
bright
surface.
area is cleavage
fracture
which has occurred as a result
the
of
samples being broken after cooling
xj
(Croft,
1979)
.
100pm
Fig.
3.18
The fracture
surface of an Fe-O. U8C alloy,
showing the interdendritic
morphology associated
with hot tearing
(Shin, 1981).
(a)
(b)
p to'Ogl
(c)
Fig.
3.19
(a)
(b)
(c)
A typical
solidification
cracking test specimen
The schematic layout for
measurements
resistance
The milled
holder
in
used
casting
a perspex
for resistance
measurements (Shin,
1981).
ac
Fig.
3.20
Schematic diagram of a partially

decohered particle
at a grain boundary (Hondros and McLean, 1976).
Frccture
Fig.
3.21
The mechanism proposed by Lorig (1952) for

between the intergranular
relaticn
fracture
and the ALN embrittled
grain boundary.
the
path
frrte
:ina
'tes
austnrte
grain
t)ounaary
0
0
v0
0
E
3'
O
scr
.
T2tIC
pho5onorus
tltstrbutton
II
! ractura
surtaca
Fig.
3.22
Schematic diagram illustrating

the distribution
of
in an
the phosphide film and NhS precipitates
At the surface of the
casting.
overheated
intergranular
fracture
casting,
was induced by
at the centre failure
grain boundary ihS, whilst
from an almost continuous
film of FeP
resulted
(not Fe3P) (Baker and Harrison,
19-5).
r4
4w
4:
.
Fig.
3.23
Transmission
electron
micrograph
from the intergranular
extracted
of a O. 22C-0.75Nh steel casting
(Hanner: et al, 1968).
of NbC plates
fracture
surface
Nb
0.
C7
containing
COOLING RATE C/HOUR

120
260
0.04 t 0.06
0.08
400
540
0.0
2 0.016
O
O
Z
0.012
0.008
0.004
0.02
1 lb/ton
0.10 0.12
0.14 t 0.16
2 lb/ton
0.18
0.20%
3Ib/ton
% ALUMINIUM ADDED
4.1
Fig.
Graph showing the effect of aluminium content,

nitrogen content and cooling rate on the susceptibility
Compositions above and to the right of
for. T. F.
be
likely
(Lorig and
to
susceptible
are
curve
each
Elsea, 1947).
0.10
oG
1%
..
0.05
uni
0
O
eG
Z%
1350C
0.05
ALUMINIUM (%)
Fig.
4.2
0.10
The nitrogen content of alwniniun-killed

steels
1200C
1050C,
equilibrated
with nitrogen gas at
in
slope
the
and 1350C. The position
change
of
denotes the formation of A1N (Darken et al, 1951).
0.15
T CC)
1000 1100
1000 1500 1400
1300
1200
1000
1100
10
uauio
10.1
2
AUSTENIT
10i
as
6.0
5.6
7.0
7.5
8.0
'IT (x 10'4 K')
Fig.
4.3
0.04
0.02
Fig.
The variation
of A]N solubility
product with
temperature for liquid steel and austenite.
The upper lines are for pure iron, and the lower
GS-60 grade steel
lines for GS-40 steel.
(0.40C, 0.80Mn) lies between the two (Honer and
1978a).
Baliktay,
4.4
0.06
The solubility
temperatures.
and Pickering
0.08
0.1
%SOLUBLE AL
0.12
0.14
0.16
0.18
of Al and N in austenite at different

Plotted using the data of Glaciran
(1967).
0.2
Ar
0-th
10
tr- -A,
W1
or
V
Fig.
Fig.
4.5
.6
Transmission
electron
micrograph showing plate-like
precipitates
of ALti extracted
from the intergranular
fracture
surface of a 0.26C-1. SOjNisteel
X3500
(Wright,
1962).
Transmission,
form of ALN
electron
micrograph showing the dendritic
X1000 (Wright,
1962).
1050
1000
ZQ
950
900
Z cc
wQ
2V
850
8009
0
02 04 06 .08
.
.
.
10 12 14 16 18
.
.
.
.
.
%- ELEMENT
Fig.
4.7
The effect of titanium,

aluminium and zirconium
on the grain coarsening temperature of En5 steel
(Halley, 1946).
(0.25-0.35%C)
A SMALL
KEEL BLOCK
25mm
(b) FROM 75n,
SQUARE CASTINGS
75mm
Fig.
5.1
The position
of samples taken for impact testing
from (a)
the small keel block castings
and
(b)
the '5mm square castings.
OM SMALL
213,11
KEEL BLOCX
_r
I
I
tII
III
II
I
IA1 FROM
JOCmm SQUARE
"I
CASTINGS
Ir
iWII
NI
NII
xU
x7I.
YOW
WI?
'
1''
I `
rJ
/II
uV
ij
il1lyl
M
20mm
2Omrw
_/
loomm
Fig.
3.2
The positicn
of samples taken for fracture
from (a)
toughness testing
the small keel
block castings
the 10Om square
and (b)
castings .
C)
GW
t1"cl)
'4-)
Akil
:
dl l1 lI it li il
y.
. fit
1111 li ii
c:
pf
7B
O
TV
C
r,
W
W
^`
C.
4)
)
u:
'
uLv:
c '
:.
:
r
Vn
J
VZ
V,
MACHINED
W1
FATIGUE
NOTCH
CRACK
C.0 D.
APPARENT
CENTRE OF ROTATION
(Wal
Fib.
5.
Idealised
sanples.
notch
profile
during
the bend testing
of COD
K
J
G
F
C)
O
O
J
Fig.
;.
Schematic view of the specimen assembly and

the directional
solidification
apparatus.
Key:
A
B
C
D
E
F
G
H
I
Gas and sample exit port

Lower service head
Alumina tube
Graphite susceptor
Silica
tube
Sample tube (altmiina)
Heating coils
Gas and thermocouple
access port
Stainless
steel tube
J
K
Brass stopper block

Hook attachment for drive
unit.
+
'"
''
Fig.
-). b
Overall
vier
apparatus.
of the directional
solidification
`,
`1
Fig.
6.1
intergranular
A typical
fracture
room temperature
The sample was taken from cast 1176
surface.
by
broken
bending in the
slow three-point
and
Note how the
quenched and tempered condition.
delineates
fracture
the columnar grain boundaries
(X2)
of the casting.
Fig.
b. 2
facet
Optical
fractograph
intergranular
of an
showing the crtivstallographically
orientated
The bright
surface markings.
areas all reflect
features
can
simultaneously,
and the dark linear
'families'.
also be seen to occur in parallel
Surrounding
areas have been masked with lacquer.
(X50)
-"
Fig.
6.3
""-
Scanning electron
micrograph showing the intersection
of several grains on the fracture
MIacrosurface.
is brittle
the fracture
scopically,
and follows
the columnar grain boundaries.
The surface markings
to those in Fig. 0.2.
(XSO)
are similar
VU
"U
J
-,
et
.:.
'n
--
U
:7
Ln
is
o3
"^)'O
C)C)o
c_..
:0
+- ^J " ,-
.-
C) 0
'J
Q)
n C/) C)
ICJ
C)
_CJ
o
+ UO
'U
'--a
+..
CJ 0_
_
C) """' `"r0.,
iOc
rA
C)
n-
C)
U
'I
C) O
s1; 4".+
CJ
."
U
Ur
V7 --
- f.
H
Q)
C CJ '"
:. C
+-A
"!:;
=
.
Fig.
6.5
feature
in more detail,
Plate-like
X-ray map for Ali-Ka radiation.
with
a corresponding
(`G9CC)
TE
N
O
.,
1r.
1.1
"
U
U
C)
C
ct z
^.
.
if
0"
CC
r -C
"=p
v,
EN
.L-i
+-+
"*
O-
<
C)
-Of
-rn
V; Gi -' -'
CCU)L---cC
CL C*
CC
Cl)
_
E aL
W
cy Q)
_ +-' (1)
o
_=
t
0
U
CC
C!
EG
C.)
F-"
cC 4- U0
c" U
ct-.U
. _.. Ct r11
(l)
Cil
"Ij
C) S
C4-z
C)
4-+ o CC-
<
--q
-1 4- C- I--
CC CL"r-..
0
r. " r,
4J
C) C) LO
GL x+-
C) -
.-
CC
Cil Q) O
O C) C) +0 V)
UC
C)
cy 4-.+ 1- -4
E
Z
u
c0 3C
+ r cn CC C) O CC
e) L,4
v, cC v, C..
v;
tt
-
O\
CJ
C) t
UO
r^
<
UO
O
Uc4.
"
s.
bG
C)
/V
U7, ^ v,
-G=
4- C)
C> C) U + 'C3
V,
G cc
r
C) U
U
Cv.
.C
.
Cq
(a)
5Nm
J,
Fig.
o. 8(a)
is a scanning electron
form of :\1N on the
imprint
of the dendritic
fracture
surface of sample 416/1.
Fig.
6.3(b)
been
has
dendrite
ALN
shows a similar
which
of
of
extracted
replica
onto a carbon extraction
(dark field
the fracture
transmission
surface
electron
micrograph).
KON
Al
Nln
Fig.
b. )
Fc
'iFe
u
MI
Scanning electron
micrograph showing the same
halves
feature
on
mating
of a room
plate-like
fracture
intergranular
surface.
temperature
Energy dispersive
reveals one half to
analysis
be Al-rich,
the other half shows no k1
whilst
fracture
has
be
It
that
can
concluded
peak.
A1N/matrix
interface
by
decohesion
the
at
occurred
being
in
ALN
retained
on only one
results
which
half of the fracture
surface.
i0plil
Fig.
b. 10
in
Similar
feature
to
that
plate-like
shown
Fig. 6.9, again with Al being detected on
only one half of the fracture
surface.
1
`f
i
Fig.
6.11
40
Scanning electron
micro; raphs of a plate-like
feature with a central
'spine'
of ; lobular
inclusions.
%hS
One
half
fracture
the
of
,
the inclusions
surface contains
and the imprints
of these inclusions
are visible
on the mating
surface.
40
`%\
(B.F.)
%',
We\\\
P,
#,
(D.F)
BIrigllt
electron
faulted
replica
surface
LlC1d
Lind
heavily
a
showing
micrographs
inclusion
of NhS. Carbon extraction
fracture
intergranular
from
the
taken
WO)
(XlO2
4176/3.
of cast
o,'
F t. r
r'
:. ;
9040
Wl-
. 12tilt
O.5um
Fig.
b. 13
electron
micrographs
.\ series of transmission
showing the effects
of tilting
on the apparent
thickness
The thickness
of an AN plate.
was
a minima ii with 39 tilt.
if
j,
Fig.
b. 14
High magnification
transmission
micrograph of
the same ALN plate with 390 tilt.
The thickness
is measured to be 65nm (650 ).
e*
.0f
Fig.
6.15
The optical
goniometer used for preliminary
measurements of the angles between plate-like
features
surfaces.
Fig.
6.16
in the auxiliary
A charpv sample in position
holder used for angular measurements in
tilt
the S. E. M.
/T
i%%',
! i) Rotate until olate

is horizontal
(ii) Tilt until plate
disappears
N
(iii) Plate disappearing values of R and T
define
the
uniquely
N.
plate normal
Fib.
c .1
Schematic diagram illustrating,

the techniitue
employed to determine the direction
of a plate
normal in theS. E.,\i.
.,
4,
50--Nm
Fig.
b. lS
A
of sCaulnng
elect-on
micrographs
features
showing plate-like
on an interfracture
granular
surface
which correspond
described
to the stages
in Fig.
6.17.
---
///
"3
"4
"5
"2
Fig.
6.19
Stereographic
projection
which
direction
of the plate normals
surface at the
of the fracture
numbering of the plate normals
to that in Table 6.3.
the
relates
to the position
The
centre.
corresponds
014
-I'
0
Fig.
6.20
.1
Scanning
fracture
electron
surface
micrograph
of the intergranular
from cast 4210, showing
the
line of intersection
of three columnar grains.
Two of these grains are contained
in the mating
half of the fracture
The A1N plate
surface.
.
in the centre of the micrograph extends
across
indicating
the discontinuity,
that it has an
orientation
relationship
with the prior
austenite
grain being observed.
Fig.
6.21
As Fig. (O,
but showing a1N plates terminating,
abruptly
at the line of intersection
of the
three grains
This indicates
these
plates
that
.
have an orientation
relationship
with one of
the to
austenite
grains on the mating half of
the fracture
surface.
24 tilt
2Opm
Fig.
b.
--
Two intersecting
fracture
surface.
on an intergranular
plates
`-
"'
45tilt
11(2
:: un
j)1; 1te<
IS
tilted
to the point of simultaneous
extinction.
The angle between the two
normals to the plates
is ?10 + 10.
IL
A
it
i
"Transmission electron
micrograph of a thin foil
taken from the prior austenite
grain bowldarv
Plates of ALN have nucleated
of sample 410/1.
in the grain boundary and grown into the adjacent
( `35 000)
to ferrite)
grains (now transformed
.
II'
`L
_(JST"1
4y
.,
.'"
r .
`=4 `
S+L
Fig.
6.25
TL
fIi
_"2
Longitudinal
section showing the position
of the
liquidus
in a directionally
solidified
sample of
(X50). Etch: 4, picral.
Optical
micrograph
cast 4383.
.:
r
+,C,'
fr .
1L'
Ai
1w
or
Fig.
6.26
Fine dendritic
liquid
region
structure
of the as-quenched
of the D. S. satimle.
Etch:
(\35).
-') picral.
r1
L
L+S
i
S (Y)
sWY)i
Fig.
b. 27
The variation
of fracture
morphology with position
along the directionally
castings.
solidified
The macroscopic fracture
morphology was the same
for casts 4382 and 4383.
;4
Fig.
Fig.
b. 28
0.29
for
intergranular
the
Ferrite
responsible
network
in
6.27.
Fig.
The
failure
seen
remainder
mode of
is
(X50).
Etch: 4 picral.
martensite
the
microstructure
of
'Fpe II
fracture
%hzSinclusions
on the interdendritic
surface of D. S. cast 4332.
9
r%
AIN
Sm
ti
Spm
Fig.
6.30
Dendritic
fracture
AIX precipitates
surface
of D. S.
on the interdendritic
cast 4333.
.a
T,
p
O
cpX
CMxOt.
U
vx
c^
iMM
L, U
fl +- '
.
r'
J-C
aC
F"+ U
U "-
Ci O
r'
rr.
"H
U+
NU
C)
. U
MUZ
r<
Sar
,.
P-
1.
''
w-
Y
rt
S
,
.
'
Fig.
6.32
Micro-hardness
impressions
used to identify
the
for
scan path
electron
probe microanalysis
of
4210.
Etch: Marble's Reagent
cast
(X150)
(a)
Fig.
6.33
(b)
Fracture
surfaces of three point bend specimens
in the quenched and tempered condition
taken from
a) Cast 4354 (0.56C)
b) Cast 4353 (0.12 C)
.
KEY:
900C 1hr WQ
900C 1hr Slow Cool
900C 1hr WQ
650C 1hr WQ
900C Ihr
Air Cool
As Cast
900C Ihr WQ
650C'/zhr WQ
As Cast
900C
900C
1hr OQ
650C 1hr WQ
Fig.
6.34
1hr CQ
650C'/ihr
WQ
Fracture surfaces
from cast 41
after
various heat treatments.
(Actual size).
1250C
Cast
4'10
Cast
4351
for
1350C for
Fig.
6.35
High temperature
heat
casts 4210 and 4351.
ih r
Ihrs
'4hrs
water
ihr
4iirs
'-ohrs
Slow cool
furnace
treatment
schedules
for
quench
in
2pm
pp,
,0
Fig.
4k
Scanning
micrograph
electron
of cast 4210
followed
by a water
24hrs
12S0C
after
at
The
quench and temper at 600C for lhr.
A1N precipitates
coarsened
are clearly
visible.
6.36
The superimposed trace is an X-ray scan for

A1Ka radiation
across the line .1.', ' .
10 HM
Fig.
6.37
As Fig. 6.36, showing the plate-like

ALV which has begun to spheroidise
.
some niicroductilit':.
form of
and exhibits
.,
(a)
"5
(b)
Fig.
b. 38
Optical
(uTletched) of cast 410
micrographs
heat treatment
showing
after high temperature
(a)
fom. of the AlN and
the plate-like
(b)
the coarsened dendrites.
Fig. a. 38a
(X-00)
.
(X1200)
Fig. b. 3Sb
S. E. Image
lOpm
._-,
01
AI Kit trace
lpm
Fig.
0.39
Scmning electron
micrographs of the coarsened
AlN in a polished
section,
using secondary and
backscattered
imaging, and energy
electron
dispersitie
analysis.
S
t
i
i
i
O/
1
0
0
m
/
\
X
\
iI//I
\
X
N
U
O
IX
w
/0
cr
w
3-
O/
i
LL. j
/0
/7C
X/
O/
cri
1/
Lt
/O
/X
/
v
O
O
0
0
CO
b
N
L
a)
:%i V
0
0
0
-C)
0
uI
"+
.;
(a)200C
(b)125C
(r) 250C
Fig.
b. 41
fracture
Typical
from tensile
test
surfaces
specimens broken at different
temperatures.
gis
is
increased,
fibrous
the
temperature
a
:
becomes more favourable.
mode of failure
11JO
CAST 4231
(0.03%D.1, O.008%N)
X
X
x
30
FIBROUS
xx
30
}
(.7
W
i- s30
v
CL
20
! CLEAVAGE
"100
"200
5.42
Fig.
00 r-I
300
200
100
TEMPERATURE CC)
0
Impact transition
curve for cast 4231, containing
0.0810.1 and G. 0C8N. Quenched from 950C and
tempered for 1hr at 60CC.
CAST 4210
(0. i7%A1,0.017N)
60 h-
(
100% F! BPCUS
560
X
zx
z
40
XxX
20 r
)C
\1! XED FIBROUS/

LEAVAGE
I. F.
x
100% 1.F.
200
-100
0
TEMPERATURE
Fig.
o. 43
100
200
300
(Cl
: rznact transition
curve for cast -121C, containing
0.1; 'Ai and -3. CH-jN.
Quenched from 9S0C and
tenroered for lhr at (;OOOOC. Note that the true
upper shelf energy is not attained
Lmtil
in excess of _OOC because ;f the
temperatures
interjranu:
ar fracture
regime.
CD
0
0
a
O
cc
C3. Q
CD J
^y
7
U, w
F2
ze
CC
p
4
N
C)
6
wr
r0
Cc
w
2
w
OO
co
oTo0
n
(C)a3GUO V A9a3N3
^ti N
0
N
0
us
x
U
Ln
"
c^Z
\
u
O
U
o_
U
o
"
00
E
\X
V
U
0
0
UO
> "O
ch
9
Lo
8
(r) ADa3N3 13VdWI
cd c3
v.
'^
oc
.
8
N
04
"
r- "-
(a)
i.
(b)
Fig.
. 46(a)
(b)
Scanning electron
micrograph showing coarse
dendritic
features
fracture
on the fibrous
(X80)
surface of cast 4351.
A dendritic
feature
in more detail
showing
has been initiated
that fracture
in the normal
(X540)
way, by void nucleation
inclusions.
%hS
at
t'
(a)
(b)
F'ig.
b. 1;
Scanning electron
micrographs
showing the change
in fracture
testing
morphology with decreasing
Intergranular
temperature.
facets on Chlarpy
impact specimens taken from cast 4351, fractured
61
C;
(`:
at (.a) -S00C and (b)
-125C.
Fig.
o. 48
Scanning electron
micrograph showing cleavage,
fracture
low
temperature
mechanism
typical
the
(\^)
for all the (harpy s.7irples.
"i<
O F.
p
Ln
C>
n
lI
xOp
O
lfl
13
}OQ
CL
Ll
Ov0 O,
Op
.D
91
14
0
Un
i
ccc<rcy
P4xQ
u-j
0
0
i
I'D
Ln
o000
CI-4
{I) AodN3 l? b'dNI
r,
cn
--+
CC)
r--
CC)
(rC)
C-
Lr
C
E-
Oll
ON
C)
W. -
U
0
0
OU
U
CJ'-"
.0-,
ON m
o>
-TV)
L/)
W
Z
M
LO
CV L.
U
C)
OU
Lr
m
LiJ
4+
U
0
Ln
I'D
N
U-)
In
o
C)
Ln
(-
o000
Lr)
fV
In
(D) 3dn1dd3dW31 DNIJS31
oc
tl(i
C
cam'
4C
LU
Q)
r'
--
---
--i,
---
O
f
1 c-
c3 o
fx.
i
o
0
--
wij
Y
il
CD
Ln
ix
o_
w
cc
x ) ." ,
Q
w
CL
LLJ
i
t
,.
OOpOOOOO
C'
OOoOOOOO
u1
fr1
L-
t-j
r-
C)
L'n
r--------r--
---
-----;
------
- -__.
.-
---
C)
;-n
:J
0
0
r--
^
+J
U
"î
4)
0 v,
U c7
5
L,
nv
Uc:
C> w
Cw
U'c
0
"^ U
V. V,
Q
Lfl
f`]
L
r
^
G:
-
`"
u1
111
pOOEO
Ò
'OS
L
b
r'
O
Lil
r-
toad
C.G.displacement
Fig.
6.53
Schematic load/di-splacement
cui e associated
failures.
This behaviour was
with brittle
typical
temperature
of all samples at a testing
of -100C.
yam:
.
v
rlr;
y'x
t?
Iced
"-
+.
_
,-
,.,
_ __.
. iu.
C.G. displacement
Fig.
6.54
Schematic load/ displacement

cur: e associated
failures
fibrous
(LLQT material).
load
C.G. d sptCC2Tient
Fig.
b. 3S Schematic load/ di-piacement curse associated

with mixed 11.F. i fibrous failures
; I-f:QT material').
Note the discontinuous
steps after the attainment
of maximum load.
4t
IJ
h
Fig.
0.5o
The fracture
surface of a IHIQT sample slowing
being preceded by fibrous
crack growth.
I. i.
Fatigue
crack
SLowfibrous
crack growth
changeof
plane
Intergranular
fracture
Omy
Fig.
o. 5;
Scanning electron
micrograph at the root of a
fatigue
crack showing a region of slow fibrous
crack growth prior
to intergranular
fracture.
In order to propagate
along the grain boundar`v,
the crack had to deviate
from it's'
ts original
plane
by 1.3rrm.
z
W
..
TEERGRANULARSTRENG,
Y1_LD
: TRENGTH
us
TEMPERATURE
is.
Schematic diarar
showing the variation
d
intergrmnular
stren-ths
and vie?
At a given temperature,
.
follow
the weakest ;math.
of cleat ae,
te: pe: ature.
0
0
LO
O
I
O
u
z
U
x
ZE
p0 LO
U
0
xO
QH
LL
C
~
Q
C u
U
U
x
r'
`c +c
0
U
_O
f
~\
RG
UZ
c-
=nC"
=G:
C; " r,
2
OO
Co
r'
O
v:
_)
ZE
W_
T
ice.
-i
v,
nC
"-!
-
+
+- O
Oy
Z
O
co u.
U
O
J
U
c, -"
ZO C) <
JUU
z
:
r
n
LA
le
CN
(-L X) N10 X IV 13
rQ
x
C)
:G
C
C)
^. r
r
C
.J
OG
. 71
0U
UO
c
"n
Z_
d
dC
V.
Z-
<
,; u
.r.
"
- -4
r- i r1
0
i. J \
bC
,.
KEY:
(111)v
Fe
on
"
atom
0 Mo atom on (0001),.,c
(a)
[11201/t
[1101r
KEY:
10-
-'
,-
v.
--
'
!
tit
Fe
(11'')
atom on
"
0 Al atomon (0001),
(b)
Q
7-i-
;
-
--
[11201a/
110
.
Fig.
7.4
a)
The Grien tation

determined by
relationship
Raynor et al (1966) for h. c. p. Mo2C with
a stenite,
with <1120>.,b C //
<110>
b)
The arrangement of Al ana Fe atoms for ALN

in the same orientation
(i. e. with <1120>ALV /, ' <110>. )
.
Note the large misfit
in the <11-20>aLN directions.
200
150
Si
For steel containing O'4l%
1-S%Mn
a
cz.
SQO
0
1300C
so
""1 )r
Fig.
7.5
005
010
N
ALUMINIUM
0.15
0-20
The effect of carbon content on the solubility

Plotted using the data
of A1N in austenite.
of Glas an and Pickering (1967) and using the
interaction
coefficients
presented in Table 4.3.
r
NSF.
(a) high matrix strength
CII.
F.
TEMP.
C= cleavage
F= fibrous
a--
Tc L
(b) intermediate
matrix strength
i
1
1
I.F.
TEMP.
'i
;c) tow matrix strength

I
l
Fig.
TEMP.
Schematic strength
diagrams
temperature
the effects
f T`.) on
of matrix strength
intergranular
fracture
behaviour. '
showing

Fracture in Steel

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Fracture in Steel

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FRACTURE

Thesis submitted in fulfilment

described and a review has been made of the fracture

The problem of A1N-induced intergranular

of two forms of A1N

form) has been confirmed.

(I. F. ) has been

work has shown that the dendritic

forms in the residual

and the existence

form and a dendritic

0.30C-1.50bh castings with varying

has been studied

Al and N contents, and commercially-produced

has been considered.

role of alinniniwn nitride

stage when the casting

grains with an orientation

have been examined.

IF is favoured by a high Al and N content

with quenched and lightly-tempered

A model has been proposed which is based

on a comparison of the relative

A programme of mechanical testing

has shown that different

value of the crack opening

The C.O. D. at maximumload,

is decreased and the implications

This can be used to

behaviour with testing

in Charpy impact energy as a result

Although there maybe a considerable

Niobium Carbide Precipitation

Boride and Carboboride Precipitation

ALUMINIUM NITRIDE IN CAST STEELS

A1N as a Cause of Intergranular

Grain Growth Inhibition

Impaired Hot Ductility

Ingot Panel Cracking

Surface Break-up During Hot Working

Fracture Toughness Testing

Measurement of the Temperature Gradient

of the Specimen Assembly

Results of the Directional

Aluminium and Nitrogen

The Results of Mechanical Testing

The Effect of Processing Variables

Aluminium and Nitrogen

Pouring Temperature and Cooling Rate

CODfor Crack Initiation

COD at maximum load

The Measurement of 'extinction'

economic method of producing

Complex geometry and difficulties

in hot working often

economic grounds casting

that some components can only be made by casting,

the more favourable,

of the cast product with

doubt is often expressed about the

and surface quality.

Indeed, a wide range

and the heat treatment

tend to be more isotropic