J~

META~06RAPH"'i EUROPE

TABLE OF CONTENTS

CHAPTER

3 day programme layout

Microstructure & Sectioning

Encapsulation

Single Point Tools

SurfacePreparation to Integrity

Thin Film Measurement

Traceability to ISO 9000

Microscopy & Photomicrography

Group Questionnaire

Material Classification & Preparation

Methods

10

Own Preparation Method

11

Company Standard to ISO 9000

12

Much of this mataial basbea1takenfItBDthe boot 'Surface~~-aDOO &; Mia~

of MaItJiaIs'

B. BOUSFIELD, Buehler Europe Ltd. Coventry, UK

The first of its kind, this book is d~icat~ to the systematicpreparationof a

vast rangeof materialsurfaces,looking in detail at the problemof
microstruCtUral
traceability. Designedto be of practicaluse,the book hasbeen
written in two parts. In the first half, tile book systematicallydefinesthe
essentialproceduresinvolv~ in surfacepreparation. Havingestablish~ how
to preparea sampleof integrity, the secondhalf of the book illustratesthe best
useof microscopyby discussing,in depth.the different featureswhich
contributeto informativeanalysis.
Completewith over 100stunningcolour photo-micrographs
and fully illustrated
throughout,this book providesan essentialreferencefor researchers
and
technicianswho requirea comprehensive
overviewof microstructuralanalysis.

CONTENTS:
PART 1: SURFACE PREPARATION: Introduction; Sectioning; Mounting; Single Point Tools; The
New Concept; Grinding; Polishing; Grinding and Polishing LubricantS; Towards a Metallographic
Standard; Characterization: Auditing aOOTraceable Standards;Traditional Methods Only; Preparation
of Spray Coatings; Preparation of Composites; Preparation of Minerals; Preparation of PCB's aOO
Electronic ComponentS;Thin Film Measurement; Preparation of Soft Materials; Preparation of
Ceramics; Hardness; Training in Metallography; Supplementary Materials, TechniquesaOOMethods;
PART 2: APPLIED MICROSCOPY: The Microscope - A Resume;Microscope Types and
Nomenclature; Creating the Microscope Image; Objective Aberrations; Improving the Image;
MeasurementS;Illumination System; EyepiecesaOOCondensers; Introduction to Interference; Surface
Finish Interference; Contrast Interference; Video Imaging and Archiving; Polarizing Light Microsopy;
Fluorescence, Reflectance and Con-focal Microscopy; Photomicrography; Inverted Techniques;
Photomicrography in Practice

0471931810

100.00/$164.00

1992

356pp

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J"i.

METALL06RAPH:'/ EUROPE

CHAPTER 1

DA"'lONE- TUTOIUALS

roTORIAL

MET ALLOG RAPHY AND THE

W CROSTRUCfURFJSECn 0 NIN G

DISCUSSION

SEcrIONlNG OPTIONS

nJTORIAL

ENCAPSULA TI 0 N ISING LE PO)NT TOOLS

DISCUSSION

ENCAPSULAnON OPnONS

TUTORIAL

SURFACEPREPARAnONTO INTEGRITY

DISCUSSION

GRINDINGI POLISHINGOPriONS

TUTORIAL

THIN Fn.M MEASUREMENT I HA RDNESSI

IMA GIN G AND A RCIDVIN G

SLmE
P~ENTATION

PREPARAnONARTEFAcrs

roTORIAL

MICROSCOPYAND PHOTOMICROGRAPHY

SLIDE
P~ENTATION

EXAMPL~ OF WELL PREPA RED SAMPLES,

EXPLOITING THE OPTICAL MICROSCOPE

1.1

-PRACTlCALS

DAY TWO / DAYTBR

INSTRUCTOR DEMONSTRAT10NS

AM

PM

8.30 DELEGATES SPLIT INTO 3 GROUPS A.B.C.

1.00 STAY IN SAME 3 GROUPS

DAY TWO
W""IA~

I..

,
11.10

11~.

111~

I
1

11.-.

~TA~

12M

~~~~

1"-'
Is..

~~

-'8!'

~
8.30 to 1.00 am

DEIIoNS1RAmNC'~PLETE PAEPARAmN

1.00 to 3.30 pm

DEIIoNS1RAOON ~ ~PLETE

4.30 to 5.00 pm

REVEW IN NAliVE LANGUAGE

Otherperloda

D8cuSSlON
OPTIONS

PREPAAA11ON

11NGTO PAEPARATIOH UUG

A FLOW CHART WITH

DELEGATES OWN PREPARATION

DAY 3
Delegates split into 2 groups X I: Y
lAM
I 1.31

4.50

IPM
I 1.18

COURSE DIRECTORSOVERVIEW OF COMPLETED COURSEWORK

I
I

METALLOGRAPH\' EUROPE
CHAPTER!
MICROSTRUCTURE

MlCROSTRUC11JRE
&. SEtnONlN6
Metallography is both an understandingof 'material
sU"Uctures'
and the 'scienceof revealingthosesuucwres'.
The sttuctures of materials can be 'macro' (low
magnifICation- large field of view) or 'micro' (higher
magnifications - small field of view). The material
microstrucblre is the 'rmgerprint' of metallurgy Le. the
microstrucblre is directly related to the performanceof
that material. The materialstructure has a relationshipto
the physicalandmechanicalpropertiesof the material.
H the microstruCnlre is to be correctly interpreted it
follows that the microstrucblre must be a true and faithful
representation. Since most methods for the surface
preparation of materials involve mechanical working
(stress dislocation) which induce damage into the material
care must be exercised in conn-oIling this damage to a
minimum.
MACROSTRUCTURE

MacrostructUres are often visible to the naked eye, but in

general are aided by the use of magnifying lens,
stereoscopic micr~ope (double image) or the single axis
macroscope. Surface preparation for the analysis of
macroStIUCturesis generally confmed to fine silicon carbide
papers.

A macrostructurewould be usedto defme:

. FracttJremorphologyandgrains
. Dendritesin castings
. Weldingintegrity
. Porosity
. Cracks
. Exterior swfacecondition
MICROSTRUCTURES

Microstructures would be observed using a compound

optical microscopewith fields of view as low as O.18mm
and resolution of O.25Jjm. When resolution less than
O.25Jjmis required it is necessaryto use the electron
microscope. The two basic types of electronmicroscope
being the scanning(for morphology)and the transmission
(internal structure).
Surface preparation can be
mechanical,chemical (electrolytic) or chemomechanical
(chemicalsusedin con.unctionwith the rindin action.

Copyright 1994BUEHLER Ltd

2.1

MET AJ..L06RAPH"'i EUROPE

Fig 2.1 Microstructural

details

Figure 2.1 gives an indicationof the type of detail visible

down the microscope.In order to reveal informationsuch
as grain boundariesand alloying elemen~ it will be
necessaryto etch the sample. Strucmresnot visible in the
'as polished' condition can abo be revealed by optical
interferencetechniquesby depositingan interferencecoat
on the sampleprior to observation(anodizing)or using
differential interferencecontrast to highlight interphase
abrasiondifferentials.
1
2

3
12

10

4
5

i
8
7
6
Figure 2. 2 Possibl~ defects of through-hole platinr, (1, lack uf plating adhesion; 2, final plating fault.~;
3. prima~. plating void; 4. fi~ protrusion; 5, average platinr, thickness; O. laminate void; 7. plating void;
x. n(tdule; q, nail h~ading; 10, wicking; 11, knee crack; 12, J'Ot'r connection with rrsin smear)

Not every microsttuCb!re~ concernedwith grains and

material identifICation. Very often with an electronic
componentor engineering~bly
the cross-section~
carried out to observe component dimensional
compatibility. Compatibilityof platedlayer from laminated
boards and the cleanlinessof the drilled hole in printed
circuit boards (~B) are adeqUatelyillustrated in the
sketchin Figure2.2.

Copyright 1994BUEHLER Ltd

2.2

MET~06RAPH"/

EUROPE

FA 1THFm. REPROOucnON

Brief mentionbasbeenmadeto the n~ for samplesthat

are a faithful reproductionof the original materialprior to
~bani~-ti woIting. Samplesthat are a true and faithful
reproductionare often referredto as 'sampleof integrity'.
So what can 'go wrong' as we mechanicallyprepare
material specimens for microstructural analysis?
Elementscanbe:. Fractwed

.
.
.
.
.
.

Pulledout
Washed out

Etched
Smeared
Distorted
Enlarged
Transformed

Elements can also be affected by:-

Heat

-Pressure

Surface
friction
Forcedirection

Artefactsoccurby incorrect:. Abrasivetype/size

. Abrasiverakeangle
. Abrasivebacking
. Abrasivefunction
. Lubricant
. Surfacespeed
. Grindingsurface
. Polishingsurface
Resultsareaffectedby:Blunt abrasives
. ProlongedI insufficientpreparationtimes
. Chemicalattack
Cl~JiQess (lack of)
. Incorrectencapsulation
. Resincontraction
. Incorrectsectioning

Fromthe four ~ aboveit canbe seenhow an incorrect

approachto surfacepreparationcan inttoduceresidual
damageleading to an erroneousanalysis.

2.3

METALL06RAPIrl EUROPE
SEC"nON1N6

Before any sectioningtakes place the need to carefully

selecta representative
areacannotbe over stressed. The
microstrucmreover the entire component may not be
unifoml, therefore,decide beforehandwhat the object of
any sectionis for andwherebestthis canbe located.

Figure 2.3 Sampling Identity

Figure 2.3 is used to illustratea simple fonnat for

designatingthe samplingposition and the swface of
interestwithinthesample.

Figure2.4 SampleI SpecimenDefmition

The word sampleand specimenis often used to describe
the samething, with the conventionasshownin figme 2.4
this shouldnow be overcome.
Sectioningis consideredto be one of the most imponant
steps in the preparationof surfacesfor microstructural
analysisand before one can proceedfrom this point it is
wise to havesomeideaof the depthof damageresidualin
the sampleresultingfrom the sectioningstage.

Copyright 1994BUEHLER Ltd

2.4

MET ALL06RAPH'/

EUROPE

FIgure2.5 Depth of sectioningdamage

This Z axis infonnation is derived by resectioningand
preparingto integrity the surfaceadjacentto the original
cut (figure 2.5)

WHEEL

TRA VERSE

Soft Bond
Alumina Grit

RATE
Slow
Fat

Bard Bond
Alumina Grit

Slow
Fast

Hacksaw

Normal

DEPfH OF
DAMAGE
10

(fUD)

45
20
900
70 + 200

Figure2.6 Sectioningdeformation0.37%C Steel

Figure 2.6 gives the results from a series of different
sectionson a pieceof 0.37%CarbonSteel,notice how the
resultant deformation or structural damage varies from
10JUDto 9O0Jl1U.
Without this informationit is impossible
to 'tailor' the most appropriatesubsequentpreparation
steps. To put the 9O0JUD
damageinto perspective(A) 3 samplesof 0.37%C Steel,diameter25mm,when

usedon 8" diameter180 grit silicon carbidepaper,for the

life of the paper,would remove100JJIni.e. 9 sheetsof 180
grit paper would be required to remove the 900J1m
damage.
(B) 3 samplesof ~
C Steelunder the sameconditions
would require 18 sheetsof 180 grit silicon carbidepaper,
Le. 50~ per sheet (Thesefigmes are basedon optimum
cuttingconditions;silicon carbidepaperswill removetwice
the amount quoted but this extra material removal will
induceintolerablelevelsof residualdamage).

METALLOORAPm' EUROPE
WHEEL
METAL
BONDED
DIAMOND

METAL
BONDED
CBN
RaIN BONDED
sn.ICON
CARDa

SPEED
IpD

DEPnf OF
DAMAGE (JDD)

TIME
MINUTES

100

10

100

IS

11m

so

lUX)

2(XX)

~
2

Figure2.7 SectioningdamageAluminium Alloy.

The resultantstructuraldamageshownin figure 2.7 is used
to illusttate the relationshipthat exis~ between abrasive
type, bond, operating speed. cutting time and residual
damage.Take the diamondwheel in comparisonwith the
cubic boron nitride (CBN) wheel operating at the same
speed. The CBN wheel manifestsa reduced depth of
damageandcuts in lesstime. Whenthe CBN wheel speed
is increasedso does the damagedepth and cutting time.
Ftnally the abradableresin bonded silicon carbide wheel
reducescutting times dramaticallywithout an increasein
damagewhen the speedis high. This chart indicatesthat
thereis (I) an optimumcutting speedand (2) an optimum
abrasive
- resultingin (I) a minimumresidualdamageand
(2) a minimumcuttingtime.

Figure 2.8 - Sectioning Characteristics.

Sectioningcharacteristicshavebeenbrought together in a
singlechart(figure 2.8),illustratingthe effectsof lubricant.
speed, abrasive size and type, abrasive concentration,
wheelbond,wheelthicknessandmechanicalfactors.

METALL06RAPH'{

EUROPE

Figure 2.9 Characteristics- Metal Bonded diamond/CBN

wheels

This final chartis intendedto give guidelineswhen dealing

specificallywith metal bondeddiamondor CBN sectioning
wheels. Speeds, lubricity, operating speeds, wheel
dressing,abrasivesize andconcentrationare all addressed.

Copyright 1994BUEHLER Ltd

2.7

SECTIONINGOPTIONSGUIDE CHART
Reference the enclosed (reduced) Wall Chart. From this chart we are able to
select the most appropriate cut-off wheel to suit specific user needs. From
the 'legend' at the bottom of this chart, notice how abrasive concentration is
depicted by the number of abrasives (low and high). Abrasive bond strength
is related to the number of cross-lines i.e. single cross-line weak bond - multicross line strong bond. When dealing with expensive abrasives such as
diamond or cubic boron nitride then the bond/abrasive will be attached to the
'rim' of a circular metal disc, this is depicted by an extra semi-circle. This 'rim'
can be a resin or metal matrix. When metal matrix, the bond is shown as a
square grid. The type of abrasive is also designated by shape viz square =
alumina, triangle = silicon carbide etc. When different size abrasives are
used then a numerical system is employed i.e. 5 = small, progressing to 20 =
large. The first five wheel types are all intended for ferrous materials of
different degrees of hardness, the wheel abrasive being alumina. Notice the
8th wheel on the list, this is also alumina but is a much thinner wheel than the
previous alumina wheels. Being a rubber bonded wheel (as opposed to
resin) it is less likely to fracture when slightly flexed. This wheel is intended
for delicate cutting, it also finds many applications which induced cutting
damage must be kept to a minimum, viz sectioning of plasma coated
materials.
Silicon carbide wheels (6th and 7th) are offered for sectioning non-ferrous
materials. they can however prove equally successful when sectioning
ferrous materials though wheel life would be very much reduced.
The rest of the wheels in the range are of the non abradable type
(diamond/CBN). Much development has gone into these wheels to make
them very specific to the hard and brittle fracture materials as shown under
'Materials Applications'.

Copyright 1994BUEHLER Ltd

2.8

(!)

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. ~,",. CARS~

SECTION1N6
Wheels break for a variety ~ ~DS
FAULT: WgF:F:I.BRAKA6E
and can be frightening whell they CUr.
Abrasive wheelswhen manufacturm are
.,.
car8:ully tested to emure safe operating
speem, these operating conditions mlm
be adherm to in use. Wheelscan break
be(:aD-~they become jammed into the
workpiece, thk Is usually one ~ two
factors (a) the workpi~ (Spedmen)~
SAWPL!
moved, or (b) the whee) ~ wandered
(movedoff uis.)
To overcome(a) It win be ~ry
to
attribute the ca~ of any movement, I'
it is s~
caused by dampiug then
siugle pcXntdamps will be necessary. If
the s~
Is within the workpi~ and ~
releasedas the cut tak~ place then the
workpi~ shcx1ldbe 5treG relieved or
incrementalcutting adopted.

~...
;.-~ sontR
: Wt[L
.
1-_"

REf.
ONLY

~a.NAP

ALTERNATIVE
STRESS REUEVE
REDUCE COOLANT FLOW
REDUCE CUTTING FORCE

To oven:c:Mne
(b) a softer wheel is often
all that is required

FAULT: BURNIN6
Although burning can readily be
o~rved on the cut surface, what is I~
obvious is the depth to whim the
burning hM affected the micr~cture.
This depth for example an vary fnMn
2Oprn to 25OJIIDwithout a dramatic
change in the top surface burned
appearance.
Some materials are
adversely affected by thama1 shocking
whel'e It is not ~arlly
the
temperature mange but the Iocalised
shockthat occurs through im11ftJdentor
poorly directed coolanL Burning can
very ~
be overcome, ~ng
the
coolant k appropriate, by reducing the
traverR rate. Softer wheels, although
the obvious molce, mU give a reduced
wheellire.

~ ;~.
",

W.
,

. ."

..

"

..

~~--,

'

)---,
,
,

..

:_--~

Al TERNATIVE

-,-0

--I
: SOFTE
R
: WHEEL
..1

~~

REDUCE RATE Of' TRAVERSE

CHANGE POSITION OF'
LUBRICATION

Copyright 1994BUEHLER Lm

2.10

SECTIONING

Swarf pick-up is evideut wta merving

~ ~phery of cut off ~
after use.
This oolKlition is m<Xein ~
as ~
workpiece material ~PS
softer IDd
would ~ver be manifest wid! bittle
fracture materials. Alttnlgh ~ dnce of
a softer ~
will usually Dve this
troblem. ~ useof oillubricaots must ~
beovedooked
~
glazing occurs wIa
d:Ie blunt
abrasive is DOt allowed to break free fttXn
d:Ie surrounding matrix (resin), d:Ieremedy
is to use a harder amsive, softer ~
(X'
increase the pressure. When using baOO
operating equipment d:Ie aInsi ve can re
1:roken free by sudden contact of ~
to
workpiece.
This however is
tedlDically soond recommeOOation

DOt a

FAULT:

PICK-UP II. WHL 6LAZlN6

./,

'"
"i4
-..,

J.

.
:

.
..1

-' . sanER

:
-.I

"

WHEEL

WHEEL GLAZING

, -"T

- .,

.. -

SOfTER

.: WHEEl

-.1

AlTERNATIVE

INCREASE PRESSURE
HARDER ABRASIVE

FAULT: WIu. NOTCUT

When wheel penetration into dJe
workpece is difficult, yet tM ~
and
~
~tions
a~
to be ~--.miz~
ie. ~
speed, pressure, lubrication.
wheel rood. abrasive type; it will be
~ssary
to investigate ~ abrasive size
and concenttati on.
With very bard
materials a coOOition COJId be foooo
wIae too many abrasives are in contact
with tM workpece at <e time restricting
~ iOOividual f<rce ~ssary
to ~
and *ar
~ material. R~.l1I~-!!g dJe
IBlIDber of abrasives in contact 0V0'00IDes
this problem. Reducing ~ ~de
size man abrasive usually inaeases ~ ability to
cut We to ~ lower fcxces required. This
wiD also give a much ~~
residual
stress (structural damage), cuaing times
however, coold iocrease.

REDUCE
:A8RASIVE
CONCENTRATION

~y
. REDUCE
I

ABRASIVE

SIZE

,..

'9

ALTERNATIVE
CHANGE ABRASIVE

Copyright 1994BUEln..ER Lm

SIZE

2.11

SECTIONIN6
FAULT: CONTACTAREA
The contact area is a vitally imJX>nant
factor in the ability to successfully section
any workpiece or comJX>~nl
The
number of abrasives in contact relating to
the generated fttCes ~cessary. With this
in miOO it is always wise with abrasive
sectioning to take ~ least contact area
possible. This is oot always JX>SSible
with
a workpiece that changes the area in
contact as the cut ~
(circle), on
these occasions either iocremenW cutting
a: the oscillating headsystem will improve
cutting performance. S~en
rotation is
another m~
of ~~-!1g a constant
contact area, d1is facility also helps to
ensure
a parallelsedi~ romJK>nCn1i.e.
it reduces any ~
for the ~
to
drift.

s~

or workpiece
residual damage is

a factor often ovedooked yet in our field

of miaostroCb1ral analysis we must 00
more dIaD ju.\1 section ~ COInIX>nent,
we
must adlieve a sample widt ~
least
residual damage. Wtae d1is is a JX'ob1em
a thiDOC'blade (X' ~
wiD often suffice.
These d1in blades are often robber ~
and are also re~ficia1 f(X' sectioning the
more delicate comJX)~nt. Reducing d)e
abrasive particulate size wiD also reduce
defonnation (residua] damage).

Having selected~ 'best' abr3sive/0000

combination axupatible with efficient
sectioning of a particular material ~n
operating fcxcesmust be ~red to. To
use the ~
urm higrer than the
optimized pressurewill certainly reduce
the sectioningtime resultingin rapid wheel
wear, inaeaseddefcrmationand increased
generatedheal To inaease the matrix
bond strength of the wheel would also
reducewheel wear.

Copyright 1994BUEHLERLm

.t'
REDUCE
CONTACT
AREA

~J,.~

~
At TERNA TIVE

WHEEL
osc~nON
INCRE~AL

CU1TING

SPECIMEN ROTAnON

FAULT: RSWUAL DAMA6/

WHEELWEAR
FAULT-SPECIMEN RESIDUAL DAMAGE
HIGH DEFORMATION

f{

USE THIN

()

~1
\\

LOW DEFORMATION

WHEEL

ALTERNATIVE
REDUCE ABRASIVE ",
SIZE
f"AULT-RAPIf')
WHF"F"I WfAR

.""'~
'"
,"'"

. '.

"'"

1'--

--..

po

"v

- - -: HARDER

~
ALTERNATIVE

wHEEL

RCOUCEPRESSURE

2.12

SECTlONIN6
FAULT: SAMPLE BURN1N6
This ackIitional section 00 bIrDing is to
draw attention to ~ lubricant or c(Xjant
which infiuelx:es ~ eflideu;y of any
sectioning ~tion.
Cutting wheels wiD
~te
differeDtly as ~
tem~
affects ~ resin 1xmd Some wheels fcr
example are designOOto ~te
dry aIJd
~
~te
efficiently when ~ ~
temperamre rises. ~
wheels we are
ma:e familiar with are dX)5e which are
'jetted' with coolant to keep ~ sample
(XX)}or ~
totaDY ~
in axiant
avoiding thermal shocking. It is important
with these ~
to target, wIae
possible, ~ jet of coolant into ~ an aDd
arowK1 ~
sample and WOIkpi~
Targeting ~
coolant onto ~
~
thereby keeping it (XX)}wiD iIKhlce sample
OOming by effectively hardening ~
wheel. Heat must be g~ted
wbe:n
'working' any mIface. On this occasion it
is wise to cxmfiDebeat, where possible, to
the swarf and blade.

_R~~

w.~

~-1--r-;;TTR

~~;;,

--~~~~

-~T---

SAMPLE

;(;jATR

WHEEL BONO TOO STRONG

SAMPLE BURMNC

~EJtE~~
AlTERNATIVE
USE SOntR

BONO WHEEL

TRY LESS LU8R!CANT

TRY DRY CUT.SLOWER TRAVERSE

FA UL T: WHEL P R OFIL - IN CORR CT

USE

When coolant is used. even when taking

into consideration ~ {X)ints rdised atx>ve.
it will be !l~~
to wet ~~.
~
Bow onto ~ ~
must re equal 00d1
sides if unifcml ~
wear is to take
place. ~
~
pofile can also re a
clue to correct matrix tKmd as sIK>wnin
thesketdl.

USE
SOFTER
,

'"

" WHEEL
~

POINTED

CHISEl.

"
/""""""""'~~SUR COOlANT
BOTH SIDES or WHEEL

ALTERNATIVE
KEEP COOLANT FLOW
AWA"" FROM SlOES or
WHEEL

Copyright 1994BUEHLER Lm

2.13

SECTIONIN6

It bas been kIXJwn for ~ reflectivity c:t:

~ sediooed surface to re used as a guide
to ~famation
free cutting aDd fcx the
weD ~tdl~
surface to re rejected. This
in fact is an ~
assumption since it
is ~ OOrnisbing CX fXX'C cutting blunt
abrasive that causes ~ shiny roOOition.
Efficient cutting takes place ~
using
sharp abrasives and sharp efficient
abrasives leave wen defined saatches. It
is impcxtant thc'efore to recognise a gocx1
saatdl pattern sinre this wiD often JXOve
to re t1M::
time emcient mettxx1, but above
all t1M::
metIxx1that least alters ~ material
structure i.e. d1emost faithful.

FAULT: POORSCRATCHPA nRN

- ,~
,

SOF"TER
WHEr-L

RUL(CTMTY

HIGI

~..,:-~1fA~

rYLl

~~~~~

RE~

LOW

FAULT: STRUC11JRAL
DAMA6
SECTIONING

~
This sketd1 is used to reinforce ~
importance of m~1cingthe sectioning stage
~
most imP<X18nt ~e
in ~
preparation p'ocedure.
Not only can
inevocable damage re ~
at dlis stage
but In(X'e imlXJ1'taDtl
Y a gcxx1section can
p:1imina.tf":~
~
for some of ~
sumequent JXeparation stages.
~
damage aeated from a given size abrasive
is less when sectioning d1an ~
an
equivalent sized abrasive is used in ~
grindingmOOe.

t)

[~t:t~~~
L LOW ~E

20 M'CROMETR[
ABRASIVE

GRINDING

W////?&

I=~~~::::]::::::.~

AlTERNATIVE
INCREASE

SHOI:K

loBSI)ReING

SURfACE USE ':-":';;';[l-

Copyright1994BUEHLERLm

Ol~ CRINDlNi

~RA$!V(

2.14

SECTIONING

When sectioning coated layers such as plasma

coatings or materials with a friable surface it is wise
to direct the cutting force, first through the coating,
followed by the substrate, failure to do this can result
in delamination as shown. When dealing with a
friable material or a porous coating it is wise to
vacuum impregnate prior to sectioning. The vacuum
necessary will be dictated to a large extent by the
size of interconnecting paths between the pores.
When the specimen has been totally immersed it is
possible to use isostatic pressure to increase resin
penetration. A lower viscosity resin will also improve
resin ingress.
Irrespective of any protection
provided it is still wise to direct all forces in the
direction of resin coating matrix. Notice from the
sketch how not all pores are 'open pores'.

SEcnONlN6
FAULT: SAMPLE ORIENTATION

Copyright 1994BUEHLER Ltd

2.15

MET.AlJ.06RAPH\' EUROPE
CHAPTERS
NCAPSULATlON

ENCAPSULA110N

Specimensaremountedor encapsulated
to (a) protectthe
sample material. (b) produce a uniform dimensionally
stable size for subsequentautomatic machine operation or
(c) assist handling for subsequent band operated
procedures. The 2-types of mounting techniques available
are compressionhot mounting and castable cold mounting.
Additionally there are two basic types of resins. those that
once set will remain rigid even when subjected to heat
(Thermosetting) and others which once set can be
rendered plastic when subjectedto heat (Thermoplastic).
Castable cold mounting resins set after reaching the
exotherm temperature and can be thermoplastic or
thermosetting. These resins do not require pressure to set
and are simply poured into appropriately shapedcups.
Compression hot mountings are also available as
thermoplastic or thermosetting. This powder mixture is
encasedwithin a pressure chamber and requires a specific
temperature relative to pressure to set the resin.
Thermosetting resins 'set' at the hot curing temperature and
as such can be ejected from the mould chamber when hot if
necessary. Thermoplastic 'set' below the peak temperamre
and must therefore he ejected when cool.
HeatIng

Furin~

Cooling

~
"
~

Solid

t'
~

THERMOSETTING

Liquid

if.!'

Heating

CoolIng

Eject

THERMOPLASTIC

Fig 3.1 CompressionMoulding Conditions

Fig 3.1 illustratesthe heatingI curingconditionsfor both

the ThennoplasticandThennosettinghot mountingresins.

Copyright 1994BUEHLER Ltd

3.1

METALL06RAPHi EUROPE
RESIN REQUIREMENTS

Ideally we would like a resin to have nil contraction, to

adhere to the sample, to have an identical abrasion
characteristic to the sample and be easy to Pombo
Unfortunately this is rarely, if ever, possible to achieve
thereforethe object is to define the 'prime' requirementsand
relatetheseto the resin. From the point of view of a4hesion,
only Epoxy resins fully satisfy this requirement with the
Phenolicsbeingthe leastaccommodating.With castablecold
mountingresinscontractionis an important factor. With hot
compressionmounting the different coefficient of tbennal
expansionbetweenresin and mount also becomesimportant
As an examplethe coefficient of lbennal Expansion(crE)
for someresinsareasfollows:-

.
.
.
.

Phenolic3/4.5 x 10"
Acrylic 5/9 x 10"
Epoxy 4n X 10"
Metals 1/3 x 10-'

From thesefigures it is easyto seehow the resinswould be

shnmk onto a round samplewhencooled.

Figure 3.2 Reducing Contraction

Grindingrelief betweenmountingresinand sampleis to be
avoidedwhenedgeanalysisis to be carriedout To avoid
this sitUationthe abrasionratesbetweensampleand resin
must be considered.
Copyright 1994BUEHLER Ltd

3.2

METAu.06RAPH"l EUROPE

CLASS

MATERIAL

Hd.M~
Prek8d 1m-

~
~"-baIaIe
~yRaa
Aaytie

~
M-.iaII
Ccid Mmmtiq

M~

(JDD/miD)
.160
440
130
SXJ

f.paIy
AayIic
~yeIt
AayIio+AV

170
1040
1100
m

Cq.-ADoy
SIerJ(O.37)

35
12.5
142

A lIi.iIaII

Figure 3.3

ABRASION CONSTANT/If'AT

ADoy

-Abrasion rates grinding

Figure 3.3 gives comparisonrates betWeenvarious materials.

Two important points relating to this chart are (1) the
reduced abrasion rates on compression mounting when
compared to castable resins and (2) the reduced abrasion
rates of metals relative to the resins.
Phenolic

, "SteeI

Carbon/carbon
I /
Epoxy

(a)

(b)

(c)

Fig 3.4 - Relief Grinding

Figure 3.4 gives examplesof positive and negativegrinding

relief. Additionally at (c) is the example of differential
interphase relief. This is vital when ~ing differential
interferencecontrast,the heightdifferencehowevermust not
exceedthe resolutionof the microscopeobjective.
The following is a list of attractionsfor both compressionand
castablemoulds.

Copyright 1994BUEHLER Ltd

3.3

NCAPSULA TION OPTIONS 6- UIDE

CHART
-Reference the enclosed (reduced) Wall Char1. From this char1 we are able to
see at a glance the variety of moulding materials available and the various
characteristics relating to each resin.
In the field of materialography, encapsulation is via hot compression moulding
or alternatively the so called 'cold' castable method.
The word 'cold'
mounting is somewhat a misnomer since exotherm temperatures of 1202 C is

hardly 'cold'.
The least abrasive resins are the compression hot mounted variety which
also tend to be quicker setting and more dimensionally correct. From the
chart it can be seen how the various categories have been defined. The first
three are phenolics and are also available as pre-moulds. The abrasion
factor is important in trying to match, where possible, the abrasion of the
sample with the moulding material. This factor is related to micrometres per
minute under a given test parameter, this shows the difference between hot
and cold mounting.

In addition to the abrasiverate is the 'polishingrate'. From the legend at the

bottom of the chart it will be noticed how this has been designatedby crosslines, just one line for 'high' progressingto manyfor 'Iow'.
The hardness value (Hv) has also been quoted but at these low values they
must be for comparison purposes only. Note how the hardness value has no
relationship with the abrasion factor. The abrasion factor is the important
value. the hardness is of little importance and again is only quoted for
comparison.
With all these different resins it is important to address the question of
suitable specific applications, the columns starting from 'use' are intended to
help. The cleavage (gap between resin and sample on the inside of a
washer) and the relative grinding relief when comparing resin to steel (0.4%
C) are drawn schematically. .Take for example the black Epomet, this shows
no cleavage and nil relief; the black Edgemount on the other hand has very
slight cleavage still with nil relief. The major difference between the two resins
being cost. These two resins would be totally unsuitable when the sample
material is highly abrasive because on this occasion negative relief would be
created.

Copyright 1994BUEHLER Ltd

ENCAPSULATION OPTIONS GUIDE CHART

- COImHUED

Viscosity, the ability of the resin to flow into small areas, is very important in

particular when the sample is porous,when it may be necessaryto vacuum

impregnate. Notice with the hot mountshow the Epometand the Transoptic
have been given a 'start' towards being viscous. With the castable resins
rated from high with one drop to low with a continuousflow it is very easy to
match a specific resin to suit particularneeds.
Setting times have been generalisedbut as can be seen, vary from 5 minutes
to 12 hours. Thermosettingresins,those that set with heat and cannot later
be softened, are shown by shading the upper triangle in the box.
Thermoplastic resins, those that can be softened later by introducing heat,
are shown by shading the lower triangle in the box. Thermoplastics are
usually difficultto polish scratchfree.
Finally we have the peak temperature column for compression mounting
resins, these figures are only valid with a given pressure. The thermoplastic
for example could require 20~ C if the pressure was to be halved. The
quoted peak temperature for the castable resins is the minimum temperature
during the exothermic reaction, it will if not controlled rise above this figure.

Copyright 1994BUEHLER Ltd

3.5

CIIA

METAlJ.06RAP~ EUROPE

The gap that occurs betweensampleand FAULT: CONTRACTION

mould will always be a problem with
resins that exhibit a high degree of
contraction.
This contraction will
COMPRESSION MOUNTING
inevitably,be higher on the inside of a
CASTABLE MOULDS.
washer than the outside. With hot
compressionmounting it is the difference
in coefficient of thenna! expansion
between moulding material and sample
that createsthe greaterproblem.
SAMPl!
With hot compressionmoulding it is the
inside of the washer only where a fissure
is likely to occur. If, as often is the case,
a gap is noticed on the outside of a
compression moWlt it signifies an uncured

mould.
To reduce the area of resin in close
proximity to the sample will reduce the
effect of contraction and coefficient
differentials. To do this an insen can be
introduced as shown or alternativelyuse
particulates of ceramic.
Another
alternativewould be to sectionthe washer
giving a 'C' shapedsubject
The useof epoxy castableresinswill
overcomemost problemsascanbe seen
from the 'encaosulationootionse:uide'.

COtfTRACTKIN

AlTERNATIVE
COMPRESSION
CASTA&[

YOI.MINC

YOUlDS

INSERT

REDUCED COFFUHT

PARTCULAT[

or

THERMAL EXPANSOf RESW

LOWER RESIN COH1RACTOI

FAULT: MOULD CRACKlN6

When two different materials 'set' under

pressure such as occurs in hot
compression mounting there exists at
ambient temperawre, localised stress
points within the mould. This situation~
aggravatedwhen dramatic volwne ratio
changestake place suchasoccursat sharp
comers of samplesas illustrated. This
residual stress can be so great it
propagates cracks within the resin.
Removingsharpcomers or increasingthe
mould size will usually overcome such
problems.

COMPRESSION MOUNrJNG
CAST ABLE MOln..DS

~:.,
Q<~SAlm.E

REMOVE SHARP
OORNERS

~~I-~
I""

(0'"1"-

-01.
.,-

...,~

ALTERNAnVE

INCREASEMOULD
$1m

;
.,..

LOWER RESIN CONTRACI10N

Copyright 1994 B UEln..ER Ltd

3.7

@A

METALLOORAPHY EUROPE
FAULT: MOUNT UNCURED

Thennosetting moulding material can CO~ION

MOUN11NO . THERM~
RE.sIN
often look quite good from the outsideyet
.,.,
~ ,
be partiBlly uncured on the inside. This
~
:-CRAHU~TO
I
siblation can be confumed by cross
sectioningthe moulded unit Specimens
exhibiting what looks like contraction
I
betweenresin and sampleoutsidefaceare
~~
more often than not examplesof partially
uncured moulds. When d1is internally
t'_--'
""...:.:::-:...,
.
.
uncuredcondition increases,the specimen
when ejected from the mould unit, will
haveeither a burst on the oppositefaceto
the sample or alternatively the sample
~
itself will standproud of the mount This
condition is more prevalent when
thermosettingresins are ejectedhot ~
can be seen from the sketch it will be
~,
I
necessaryto vary pressure,temperatt1re
or
aMEPERIOO
cure period as appropriate

I~1\M(
.

~~

~
~ .f

~,,

--:0-

ALTERNAT1VE

USE THERMOPLASTICRESIN

FAULT: MOURTURCURED
COMPRESSION MOUNTING
THERMOPLASTIC RESIN

Clear thermoplastic compressionmoul~

often exhibit what is called a cotton ball
effect, this can be in evidenceon ejection
from the mould or can occur asthe mould
cools to ambienttemperature.
There are two types of cotton ball effects
and they must be addresseddifferently if
the problem is to be overcome. Firstly
there is the misty effect just below the
sample,this can usually be overcomeby
reducing the rate of cooling, prolonging
the period.When the misty or cloud effect
is replacedwith a distinct combinationof
smaIl bubbles then reducing the heating
period should suffice. Thereis a word of
warning however and that is, both of
theseconditions are temperature/pressure
related. i.e.,. lower the temperatureincreasethe pressure.Having established
a good working combination it will be
necessaryto retain a similar resin to
sampleratio to avoid cloud fe-emergence.

l- -

REDUCE

Of

...
\

-~lOUO

~~l
[MISTY]

~"~5~

r SAMPLE

/
--~~-Go
--~

REDUC(
HEATING

PERIOD

CLOUD [SMALL BUBBLES)

AlTI~NA11V(

USE LESS RESIN

Copyright 1994BUEHLER Ltd

3.8

METAu.06RAPH-{

EUROPE
FAULT: SAllPLEDISTOR110N

Delicate samp~ i~y

should not be
subjectedto compressionmounting, this
howeveris sometimesunavoidable.Some
users surround the delicate component
with a metal ring thus confiningpressure
to the longimdinal axis. If isostatic
pressureis to be used then thermoplastic
resins are best employed;the mounting
press pre-load being used until the resin
has softened. Since thermoplasticresins
can be moulded at much lower pressure
than the thennosettingresinsit is possible
to achieve satisfactory moulds at much
lower pressurethan recommendedby the
equipment supplier. It is important to
rememberthat thesemoulding resins are
pressureI temperaturerelatedand as such
any lowering of pressure must be
accompanied with a rise in moulding
temperature.

COMPRESSION MOUNTING
THERMOSETTING RESIN

DRYOUT
MOULDING

POWDER

SAMPLE
\...

~
4

FAULT:

One of the most desirable features of

specimenmoWlting is to have the moWlt
material stick to the sample. This
condition is prevalent with epoxy type
resins and all other resins to a lesser
degree. Having establishedthis very
desirablefeatureit is not surprisingto find
the mount sticks to the metalwalls of the
moulding cylinder.
Lubrican~ are
available to avoid cylinder wall sticking
andshould be usedat intervaJscompatible
with the type of moulding resin in use.
Another type of sticking occurs m
compressionmoWlting and that is when
the moulding resin is squeezedbetween
the ram and cylinder walls. to rectify this
condition it will be necessaryto replace
the worn out ram

CIRCUMFERENTIAl
SPLIT

MOUNT ADHESION

C~SSION

MOUNTING

THERMOSffilNG RESIN
FAULT

SAMPLE DISTORTION

SAMPLE

:-i
,...:~~~'"
"-=-:'""~---"

DISTORTION

CHANCETO

THERMOPlASTIC
REDUCEPRESSURE
INCREASE

TEMPERATlIRf

"'--~~
ALTERNATIVE

Copyright 1994BUEIn..ERLtd

"

!!$E CAS1A8LE RESIN

3.9

J""

METALL06RAPH"i EUROPE
FAULT: MOULD ADHESION
SPECMN AOttCSOC

Lubricantsare availableto avoid cylinder

wall sticking and should be used at
intervw compatible with the type of
mouldingresinin use.

I.~

SPEa..:Nl

--~j~a.

Most castable~
exhibit a degreeof FAULT: POORDIMNSIONAL
contraction. d1is contraction leads to an
STAS nnY
irregular shaped mould dipping in the
CASTABLE RESINS
centre and not too parallel on the outer
diameter. In addition to this poor shape
there is the Jack of dimensionalstability
attributed to varying contractionbetween
~~-~
different resins. This problem can be
overcome by using an epoxy type ~
l_J~ ,(low contraction, low viscosity) or.
':'-~t
REs..
alternatively mould the sample within a
'ring form' asshownin the sketch.
PHENOLIC
SAMPLE

m 6H EX OTHRII

All castable ~
have a 'peat
temperature', this is the minimmn
exothermtemperatureneededto 'set' the
resin. (See encapsulatingresin guide).
This exotherm temperature is ~lf
generatingand will if not controlled. far
exceedthe peak temperamre. To control
the generatedheat (1) reducethe volume
of resin (2) increasethe samplesize (3)
blow the exotherm peat temperature
acrossthe settingresin surface.

Copyright 1994BUEIn.ER Ltd

FAULT

RING
FORM

HIGH (XOTHERM

1 C

JO'c

7<

REDUCE

At. TERNA flV[

BLOW JOoC AIR ACROSS

SPECIMEN SURrACE

3.10

11>4

METALL06RAPm' EUROPE

Associated with
improved resin
characteristicsis usually a price penalty
Le. better resins are usually .more
expensive. To compensatefor this price
increaseit is possibleto supportthe front
face of expensive resin with an
inexpensive resin such as standard
phenolicas backingmaterial.

FAULT: EXPENSIVERESIN
MOUNTING

COMPRESSION
COST SAVING

INEXPENSIVE

RESIN

EXPENSIVE RESIN

SAMPLE

FAULT: POORLCTRICAL CONTACT

Good electrical contact betweensample

and anode, for example in electrolytic
polishing/etching,is often required. The
approachcan be one of two ways (a) drill
a hole through the resin until contact ~
made with the specimenafter which an
electrical contact can be made or (b)
mount the sample in a conductingresin.
Conducting resim can be metal filled as
used in electropolishingor graphitefilled
for scanningelectronmicroscopy.

CONDUCTIVE MOUNTS
METAL CONTACT

OR

SAMPLE
NON CONDUCTING RESIN

Copyright 1994BUEm..ERLtd

METAL OR GRAPHITE
INCLUSION

3.11

(!)

E-1Jc.A~ULATIO).J OPT'O~
Mo~L. 'D ItJG

COMPee-SSlO).1
C...T

u.

\l

72D-3100

gUIDE-

D.5t:2rPT10,I

AMASlO'.'
~ACTO2

!L4C~ P~'Q.IC

I POL ISHiUG '

'I

Hy

RATE-

EEt'TIVf

0
0

5f.O

\JSe.

4'-

-W-3~

-&0

PllEUQ.IC

5(.0

~UQI 'I8IOL~

4(.
~

,~c-o
(,0

Gt~'ffAL
GE~ml.

PC~~
'PI~

4-40

DIAu,yL.
.PtfTHALATJC
PJfTHA~
DlALL'fL.

a!~~L
~E;
CQ.'-M~
CQ.UU~

~o

',...0

10-3380
ZO-33CO -aL~~
: !POMET

"0
130

w. SOlO

lto
lto

&LACI(
&I.AC"
ED"~"'Ou..""
E06!WlOIAJ'T

I'"

/50

150

'7

150

~- ~
~

..,

150

~
WM

"0

"7

150

"7

150

150

"

1f.0

..~

~.
--"~~

~
!

~o

~"71
~

"7

""J

--~

""$(OS,"y

~
,~~: -~A;~:

~:
~,
--'~~~

~
c.-.&

.
"ZO-mo

6f&.'f'r.4L
P\I~

to-noo

CLEAVAGe26""
/STEEL.

BUEHLE~
~~~ ~MD PUt:
T~.,

rMfMICAL

~15T

--:-y~

'

\"'Sf'ACf
\. 'fe FAce
ADJta.ou
Ao~esIOU

"71

..
...ow
J!'LI~~

"75

-~-

G2APJI~
5eM

I
,I

~~~

fLEC'T~O
.fOLI5~

---1~

C"-PA~
Mouv'TS

---~
~

"::li

.~
~j'

COLD
~-~o

zo-mo
*8"':>

~A5TfCH

,-cETLIC

!
I

1000

~::;;;;I-;:::MotTL,lt"~~ I
F"

MnS!,"f

1100

1~

'-ow
SM21UK.\Gt

t~

~PE r-D

I~

Po~ YfS"Te'~

ss-~I)I
to- 3570

to-el!O
to -ai"

ZO-CI40

~- CI41
.1"-0116

1100

UL~'T
'~'C

9~
RoGal4

EPO-T.-J m../IWfa.

"tPQ-

KNC~

~
I~
,

.or:

870

14

~. .

, l'
2&

&70

Ie;

~,o

1&

~"a~
4
\.OWA~OJ
IL'TN~
~esl~

V~'U\lM
lW2~'JaI

AOtteslOa,!
to

.".e-e-o

.fI1
- .
~WJj
y-% - .

L'E'~Pf,,"SIV[

lto

eo

--. -.

1/'!1S!T S'li
'Ot."(!!Te

!'.o"~

"EXP!I.'S\\/!

~~~

~ ~..-..
~~
. ..
---r .:ff1
.

"0

'1'5

40

'7

'"77

1-6 IllS

!eo

.
.

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11,.a

27

so

~S

@4

METALLOORAPH'i EUROPE

CHAPTER 4-

SIN6L POINT TOOlS (STRESS APPUCA TORS)

Removal of material by multiple singlepoint tools seemsa

strange subject to be included in a course of

metallography. In fact a knowledgeof how the material
removaloccursand the subsequentdamageresulting from
this 'woIting' is vital to our knowledgeif progressingthe
surfaceto integrity is to be achieved Materials fall into
one of two groups i.e., (1) Ductile materials where
material is removed by 'slip plane dislocation', such
materialswould be steel,brass,aluminimnetc. (2) Brittle
materialswhere material is removed by brittle fracmre
m~hani.an; such materials would be ceramics, bricks.
mineralsetc.

RES\A.
T:S1t[l \ ~~

OEF~M4TION ANa
R[5C)UAI. STRESS

RES\A.
T:CERAYIC\-rRAl

RtsIOUAl

C~AC..-S

Figure 4.1 - Material Removal Phenomina

Thesetwo groupsof materialremovalare shown in figure

4.1. Dislocationby slip planemechanismis shown to nm
along the shearstressdirection, this results in a defo1'JDed
structureand a potentialresidualstress. When material~
removed by crack propogation the result is a residual
crackedStI'tlcturewith little if any residualstress. The idea
in materialography
is to progressthis residualdamageto a
theoretical zero by use of smaller sized abrasivesand
different support surfaces to absorb the cutting shock.
From figure 4.1 it should be noticed how the cutting tool
front face has a different angle (rake angle) for the two
materials. Ductile materialsrequire a positive rake angle
(seefigure 4.2), brittle fracture materialsrequire a zero to
negativerakeangle.

Copyright 1994BUEHLER Ltd

.A

MET ALLOORAPH"l EUROPE

~ t:~] a 0
Positivelow
deformation

Negative high
deformation

Figure4.2 OptimumRakeAngles
This rake anglevariesfor different mate~ softer ductile
materialsneeda higher positive angle, harder materialsa
lower positive angle. The resultant defomation can be
related to the rake cutting angle. Le. a low positive rake
angle will induce greater specimenresidual damagethan
would the optimumlargerrake angle. This cutting action
is an exampleof single stressapplicators,in the field of
materialography
we aremoreinvolved with 'multiple stress
applicators'. One such exampleis silicon carbide paper,
this is shownin figure 4.3. The rake angle of the cutting
abrasivebaswhat is calleda 'critical angle'. Less than the
critical anglewill cut the workpiece(sample),greater than
this 'ploughs' and eventuallyrubs (to be explainedlater).
Silicon carbide particles, as they are electrostatically
excited on the adhesivebacking paper are randomly
orientated The result being a combination of different
rake anglespresentedto the approachingworkpiece.

Copyright 1994BUEHLER Ltd

J~

METALL06RAPH'i EUROPE
Steel

[:::j

l~

~=:J
Critical angle 900
< Cuts> ploughs/rubs

Steel

C:1

Figure 4.3 - Silicon Carbide Paperwhen new

~~~/

!~

Positivesbecome negatives

Figure 4.4 - Silicon Carbide Paper In Use

Figure 4.4 showsthe effect of theseSiC particlesas they

are used. The ideal positiveanglessoon becomenegative
by breakingor shearingat an anglenonnal to the front face
sheardirection.

Cut
Fig;ure 4.5 - Scratch Patterns

Copyright 1994BUEHLER Ltd

Ploughed

~4

METALL06RAPH"l EUROPE

Figure 4.5 shows the effect of using the various angled

abrasives.Sharppositiveangleabrasivesgive a cleancut.
sharpnegativerake anglestan to plough, causinga breakup from the clean cut: This u often accompaniedby a
material build-up each side of the groove as shown.
Negative rake angleswhen used with ductile mataeriab
will soon~ome blunt, from which point there is a greater
tendencyto rub than there u to cul The visual effect of
this last conditionis to shineor b~
the surfacegiving a
brighter appearancewhich to the untrained eye could be
interpreted as a better finish. Looking at the type of
scratch pattern is essential in u-~-~~g the residual
damage.Justaswith the surfacefinim after sectioningthe
conditionshouldbe a unifoI1Dseriesof cleanscratches.As
the scratchesdarkenso the cutting is lessefficient. beyond
d1is stage as the surface shines then residual damage
(deformation)can be gross. When assessinga scratch
patternfollowing a grinding processwhere the workpiece
hasbeenorientatedthen the scratchesshould havea depth
Le. not all on the same plane, some going underneath
othersandat a different orientation.

Figure 4.6 - Degrading Abrasive and Deformation Chart

Figure 4.6 bas combined the relationship between the

cutting abrasiveanglein useandthe resultingdefonnation.
The major point being, when using degrading abrasives
such as silicon carbide paper they should only be used
within the time o~ (T1) period.

Copyright 1994BUEHLER Ltd

@4

METALLOORAPH"{
EUROPE

Figure 4.7 - Factors Affecting Material RemovalResidual

Damage
There is an important material removal! resultantdamage
reJationshipthat occursrelative to a given factor. A list of
factorsaffectingfinal resultshavebeenshownin figure 4.7

COMPRESSEDCRYSTAL.

SLIP P! .\.t'Jf DISLOCATIONS

~~

J,.\

METALLOGRAPH'l EUROPE

DEPTH OF DAMAGE

If we are to progressthe preparation sequencetowards

sampleintegrity it is important to have an appreciationof
the total defonnedlayer (or heat affected zone) resulting
from a particularsectioningI grinding or lapping process.

IrAl

SPECMH

-- -

~RY-~-~~~
Sl.-tPI,AWS
..:::/
(PLASTIC DlSLO~~,:E

-.,:---

--

-,

~:I;;;;~~~::::.1

~~~i~~~~~~~~~
PAP[R
8.c.c~

...~

RtSGuAl
HARD

METAL

son

METAL

STRESS2~~

50.

BRmL ~TU~
~
TOTAl

lOOK

~To.
OEF'ORMATION

... F"RAGWENTO

SIZ CO4T

L.AY[~

~Al~

COAT

Figure 4.8 - Plastic Grinding Using Abrasive Particles

Figure4.8 depictsthe Stn1cnJral

artifactsresulting from the
use of SiC or aluminagrinding papers. These papersare
produced with variable 'weights', heavy papers (thick)
offering more shock absorbing Oess defonnation).
Abrasivegrains adhereto the paper by the 'bond coat' as
shown. The working severity of the grinding paper ~
inf1~nced by the 'size coat'. The thin size coat being
intially more aggressive,thicker size coats low in material
removaloffering a longeractiveworking life.
The metal specimenshown m figure 4.8 shows two areas
of slip plane dislocationcausedby the abrasivegrinding
process, note the strain boundary and the visible
~fonnation depth. The visible ~fonnation is that which
would be optically revealed after cross sectioning the
ground surfaceand etching. This etchedimagewould not
~.re-.ssa.-rily
reveal these slip planesbut will reveal a
distorted structure m comparisonwith the parent or true
structure. Additionally to the visible defonnationis the top
surfacefragmentedlayer. When using sharp, optimum to
critical angle abrasivesthis layer will be extremely small
(2JJ1nto
nil). As d1esegrains chip and becometruncatedso
the fragmented layer will mcrease as will the visible
~fonnation.
Copyright 1994BUEHLER LId

4.6

PREFERENTIAL ET.CH AT
SLIP PLANE/STRAIN
BOUNDARY~"

",

PLASTIC DISLOCATIONS
FROM GRINDING

'-

METAl SPECIMEN
PLASTIC LAYER
ASSOCIATED WITH
POLISHING CLOTH
ABRASIVE PARTICLE_S/~-

\.:.
-'""'\

'.:z:~~.-.
CLOTH BACKING
ABRASIVE RESTRICTING SURFACE
CLOTH NAP

4
-""
--"
--.c--

DIRECTION

.
. "
,:.
.' ':' .~:;

ij:

:
~
.'.

.:

,: -.

~"";;.":
. ...';.:.;~

,I.. c',

'"

",..

'.. " -.
. ;

.'

.'

.A"-':'";-".'..~;;;,I;o""~_I~""",'::.'~'
j..-':.'~':"-:"-~';',,:,:~~"l'~-::';","~'.'.

..

'"

':',...'.~~:.r-,:,:-':

AFTER
SAMPLE INTEGRITY STAGE

~m
POLISHING STAGE

IMPRESSED GRIT/SWARF n
WATER

FINGER
,~
I

JET

~:::;;;~.

...~~~~~~
,

HOT AIR

.-

SOAP

- ~~T~~~N~C
-{)CLEAN

WATE
R JET

~EJC1.H~
~ (if

required)

~~::~~~:::J::~=:::::~:~

"""'",~

I'

18

ALCOHOL

',:

OPTICAL
-~

ANAL YSIS

~
SAMPLE
ENCAPSULATION RESIN

FIG

CLEANING

@)

iliA

METAu.06RAPH'l EUROPE
During the materialremoval processit is Hkely that slip
plane action has resultedin residualSttessbeing present
beyond the visible deformationlayer. In consideringa
potential total ~formation layer the depth of residual
StreSS
has to be taken into account. Figure 4.8 indicates
the additionalincrementsnecessaryto take this factor into
account.
Although this discussionbas been confiDed to plastic
grinding where material removal is by slip plane
dislocation.a dmilar adjustmenthas to be made when
material is removed by brittle fracture m~hani~
(ceramics.bricks.rocks. mineralsetc). From the chart this
is shown to be 100%of the visible depth. not becauseof
residualstressbut ~ause fine cracksare areasof further
crackpropagation.

Copyright 1994Bum n..ER Ltd

@A

METAlL06RAPm' EUROPE

CHAM"R 5
CONVlmONS

SURFACEPRPARATlOR1'0 1RT6Rm'
In the surfacepreparationof materialsfor microS1rUcUal
analysiswords suchas grinding. lappingand polishing are
used.To avoid any confusion the following conventions
and definitions are used throughout the book. (these
conventionshavebeenwell publishedandestablished)

Sample

':!:~::::~-

t::

Deformation

Fixedabrasive

Figure 5.1 - Grinding

This is the most aggressivematerialremovaltechniq~ we

shall use. Although it is efficient at removing material it
does, as shown, manifest a relatively high level of
deformationwith a ductile material. This is due to the
resultantshearforces(RJ acting onthesample.To reduce
this deformationwith a fixed grinding abrasiveit will be
~-~~
to progressivelyreducethe abrasivesize and/or
increasethe shockabsorbingcharacteristicsof the grinding
surface.Grindingis a quick operation.

Sample
Impre.ssed
L("""",.~
~

abrasveI"" I
00

~
II/ / /, Deformation
~
Compressed grains

8~~~~o 000
Rollingabrasive

Figure5.2 . Lapping
..Do

,."p

sorT

&.,.

,..,~TE~'~ J
A.Wt1,"~J1 M.M,C)

J~

METAUaOORAPHi EUROPE
'Ibis techniq~ ,-mli5esa flee rolling abrasiveand produces
a much reduced deformation layer in comparison with
grinding. 'Ibis ~ in part due to the changedresultantforce
(R,) and the shock: absorbing action of the non-fixed
abrasive.'Ibis technique~ highly favouredfor its extreme
planarity and ~ relevant as a possible techniq~ for an
brittJe fracnJremateriah (not d~).
If ~ technique
was to be used for soft metah then impressedgrinding
abrasiveswould occur as shown. Lapping ~ a slow
operation.

Sample
i

,...~"'4@\'""'.::.:"

Polishing

(note the deformationl

plucked grains, smear and cloth nap)
FIgure 5.3 - Polishing

Po~g
is the step used when scratches are to be
removed from the sample often resulting in a '~'.
Defonnatlonis relativelylow as shown (shouldbe nil) but
there is alwaysthe chanceof smearingthe samplesurface
if prolongedtimesor increasedpressureis applied

Figure 5.4 - Composite Surfaces

Grinding is quick, not so flat and leavesa relatively high

@A

METALLOGRAPH't{EUROPE

SAMPLE
PRPARATION
SPECIMEN
MATERIAL
SPECIFIC5.86 TO
5.42

It bas been shown. using the charts, bow operating

parameterscan be used to optimise a given preparation
procedure. It is aha shown in the 'options' cban for
grinding and polishingthe grinding surfacesavailableand
the severity rating in relation to each other. What ~
~g
from all this infonnation is a guide to the
appropriategrinding/polishingsurfacesrelative to specific
materials.
The following chIns are intendedto guide the user into
using the correct grindin1/polishing surfaces that are
specimen material specific. All too often a grinding
swface is selected'becauseit is available' and nowhere is
it stated in literature where these surfacesmust not be
used. Take for examplethe nickel coated diamond discs
(ULTRA-PREP), they are not intended as replacements
for silicon carbidepaper,nor arethey intendedfor use with
very hard materials.Thesediscs will 'clog' with swart' if
used with soft tough materials rendering them useless
within minutes. Thesechartsthereforewill indicatewhere
bestto be usedand by definition shouldNOT re usedwith
otherspecimenmaterials.

The material groups have been generalisedand will

inevitablybe incomplete,they will howevercover the
majorityof materiahlikely to beencountered
The Material groupsare:. Very bardmateriaJs
. Brittle fracturematerials
. Soft d~e materials
. Ductilematerials general
. Metal matrix composites
. GlassK::eramic
matrix composites
. Polymermatrix com~tes

Figure 5.36: This chart relatesto the use of fixed diamond

grinding surfaces.~
is the area where incorrect use of
grinding surfacesis most prevalent Very hard materia1s
obviouslyrequirea hardabrasivesuch as diamondin order
to abrade the specimen. This diamond must re well
protected againstimpact damageotherwise the diamond
will becomedislodgedfrom its housing. It is for this
reasonthe resinmatrix grinding wheel is used. To use the
nickel platedwheelfor thesehard materialswould rendera
much reduced life due to impact damage (see figure
5.36A).

J~

METALLOORAPH"iEUROPE
As the brittle fracwre materialsbecomesofterso the useof
nickel bonded diamond grinding becomes~
(A)
The diamondis depositedonto circular Mesashapedforms
adhering via the nickel to a resin fibre support. The
protruding diamonds are also nickel plated to initiate
efficient cutting. There are a series of these surfaces
allowing progressionto the secondintegrity stage. When
observingthe scratchpatternfrom nickel bondeddiamond
grinding a brittle fracture pattern should be observed. It
will be noticed from figure 5.36 how the Ultra-Prepdisc ~
iJx;luOOd
for planar grinding of MMC ma1erials; ~ ~
only possible when the ceramic particulate has a high
concentration. The swart' from cutting the soft metal
matrix will want to weld to the diamondcutting face, it ~
the ceramicparticulatethat will act like a dressingstick as
it is being cut and therefore stop the diamond from
becomingclogged.
This grinding surface can also be used for the planar
grinding of soft materialsw~ alternativemethodssuchas
silicon carbide or allDDiDiumoxide papers manifest
impressedabrasives.When it is usedfor soft materialsthe
grinding surfaceshouldbe waxedor oiled prior to use and
could additionally require regular dressing to keep the
diamondfacesclean.
Metal mesh discs (UL'I'RA-PLAN) (C) are very much
confiDed to the brittle fracture materia]s,in comparison
with the two previousdiscs, they induce ~ damagebut
are slower at removing material. ~~~u..~ the diamondis
'charged' onto the steel mesh,and requires the action of
the ~imen passingover to lodge the diamondinto the
meshsurface,ductile materialswould not be a candidate
for this grinding surface. This is confinned by reference
onceagainto figure 5.36.
Metiap Platens(D) which are compositesof metaJ/resinor
ceramic/resinrequire a chargedabrasiveand as such have
restricteduse when materialductility ~ high. They induce
a restricted level of defonnationor structural damageand
leavesthe specimenin an extremelyflat condition. There
are a seriesof platensoffering increasedshock absorbing
characteristicsfor systematicprogressiontowards sample
integrity. Note how the use of thesehave beenrestricted
to the harder ductile and brittle fracture materials thus
avoiding any impressed diamond abrasives from soft
me~

J~

METALLOORAPH"lEUROPE
ULTRA-PREPdiscs(E) havea very importantrole to play
in the brittle fractureseriesof materials.note bow they are
usedin the final integritystagesie. 2 and 3. The diamond
abrasiveis em~M~-rl into dome shapedresin spots on a
resin fibre support. When observingthe scratchpattern it
will be noticedbow the previousstagefracture mec~
has changedto what looks like a polished appearance.
1bis is due to the materialremovalmed1aDism
changingto
a type of slip plane dislocationfrom the previous brittle
fracture. This condition is in part shock absorbing
dependentaswell asparticlesiu - ie.

20pm nickel plated mIra-Prep disc would induce

brittle fracnue - material removal by crack
propagation.

30J1Jnresin bond Ultra-Prep disc would induce a

polishedappearance- material removal by slip plane
dis1 <x:ati on.

Figure5.37- Thisgroupof grindingsurfaces(H & 1) are

thosewhich due to degradationhaveto be replaced,as do
grinding papers,or have to be dressed,as do grinding
whee~, in order to present fresb/sharp grains to the
material to be ground. Grinding whee~ tend to be the
vitrified type as opposedto remnbonded. Alumina for the
ferrous materialsand micon carbide for the non ferrous.
Grindingstonesor ~~
are only to be usedwhere large
amountsof stockareto be removalor alternativelya quick
planargrind is requiredon a large area. Thesewheelsare
not intendedfor soft materials. Zirconia alumina papers
(K) would be used to planar grind these materialsif the
grinding wheel should not be available. The majority
applicationin this group is for silicon carbide papers (L)
they havebeenthe backbo~ of all grinding surfacesin the
field of metallographyand will continue to have an
importantrole to play, in particularwith routine materials.
Wid! polymer materiah and fibre circuit boards for
exampleit is possibleto reach integrity group 2 using
P4000siliconcarbidepapers. As a generalmle the softer
the material the coarser the final silicon carbide grade
shouldbe. This is reinforcedin figure 5.37 where general
ductile materials~ SiC papersto integrity group 1 and
soft ductilematerialsto theplanargrinding stageonly.

>4

METALL06RAPH"i EUROPE
Figure 5.38 - Grinding cloths are those fabric surfaces
charged with a diamond ~ve
and suitable lubricant.
usedin ~ grinding modein the sampleintegrity stage. In
the past these cloths have reen called .polishing' cloths
since no distinction was ~
between grinding and
po~g.
In order to carry out efficient grinding mese
surfacesn~d to havea reducedsurfacetensionand this ~
achievedby the weaveof the cloth or the porosity within a
resiningressedtextile material. The diameterof the weave
and subsequentmesh(denierby weight) dictatesthe ideal
grinding abrasive~. This is reflectedin me selectionand
subsequentpositioningwithin the chart Finally at the last
integrity stage the choice is influencedby the specimen
material abrasionresistance,hard materialsusing Texmet
2000 (N), soft materia]susingthe acetatesilk (Q).
Figure 5.39 - Polishingclothsareusedas the word implies
'to polish or shinethe surface'in orderto achievea scratch
free reflective surface. Those~en
materialsthat are
most prone to scratches.that ~ soft metals, should be
polishedwith a non-saarcbingabrasivesuch as Colloidal
Silica. The cloth equally should be soft and free from
abrasionsuch as Mastertex. Notice from figure 5.39 how
tbi cloth ~ used for slWTy polishing (SP) and not
diamond
Specimensthat smear or are 'gummy' will require the
addition of either an acid or an alkaline solution to cause
specimen ~lution
and in consequenceallow the
abrasiveparticlesto polish in a defonnation free manner.
To ~ end the COOmometcloth for soft materials ~
designated'AK' for attack polish. For general ductile
materialsthe Clemomet, when used, would be for slurry
polishing(SP).
Ceramic material, silicon wafer etc require a totally
differentcloth hencethePolimetfcr sluny polishing.
When dealing with general ductile materiab the use of
diamond polishing can abo be a choice, the Microcloth
(high nap)beingusedfor many~~~c1I!:-~.This ~ of cloth
could also be used on difficult MMC materiab where the
matrix requires an additiooal polish. Some ceramic
compositessuch as PODFA used in almninium casting
could require an attack or ~lution
polish hence the
Cbemometfor AK.

J~

METALLO6RAPH'iEUROPE

DlAM 0 lm &RIND IN 6

CLOTHS

Through the adventof the B~bler DeWconcept in

specimenpreparationa greater emphasishas been
placed in what is the specific fmK:tion of
grinding/lappingand polishing surfaces,and when
best to ~ them. Additionallyto this ~ the needto
~
the type of abrasivemost suitable for such
surfaces. Considering cloths for grinding tOOy
shouldbe without any nap and have somemeansof
retaining the grinding abrasive. Le. considerations
suchas

.
p

.
.
.

have a varying size meshstructure to suit large

andsmallsizedabrasives
.
Surfaceto be porous
abrasivesto lodgebetweenfibres
abrasivesto be forcedinto polymerbinder

Coths that are chemotexti1e

usuallyhavea graded
resin binder system based on hardness (usually
between70 - 90 shoreA). When the resin volume
is high it is re~.ssaryto 'buff' the cloth surfacein
order to retain the diamondabrasiveand lubricating
medium.
Examplesof diamondIliDdin&cloths are:Utra-pad
Texmet
PeIforatedTexmet
Nyloo
mtra-pol
AcetateSilk (qA~)

Polimet
Although an explanationof which cloths to use for
specific ~
is given later in the text, it ~
thought prudent at this stage to introduce the
subject
Consider the grinding cloth selection at the final
integrity stagefor thefollowing materia1s:Very hard(TungstenCarbide)
. MediumHard (0.4%CarbonSteel)
Very Soft (Aluminium)
. Brittle Fracture(Mineral)

.
.

J~

METAIJ.O6RAPH"l EUROPE
All thesefour materialscould be preparedusing a
Texmet cloth at the final integrity stage,the results
howeverwould be compromised.i.e.
. Soft materials would be severely
saatcbed.
. Deformation would be higher as the
materialbecomessofter.
. Surfacerobbing could cause phasepull
out
. Integrity would becompromised.
Taking the soft materlaJsfirst we ~d a cloth that ~
the leut abrasive(soft to the touch), in this casethe
acetate silk cloth would be suitable. This cloth
additionallyhasa cross-weavepatternwhich helpsin
removing surface tension during grinding. The
reduced smface tension by definition means less
surfacerubbing which is an addedadvantagewhen
preparingfriabJe~
(graphitein iron).
The mediumbard materialrequiresa mm,larcloth to
the previousexampleonly this time the cross-weave
~
to be more resilient Nylon cloths satisfy this
requirement
Hard materials n~d a hard wearing Oat surface
cloth. Cloth abrasionis not important at this stage.
High ~nsity laminAtecloths that are fused together
under heat and pressurecould be ~d.
The most
popular cloth throughout the world is the
cbemotextile 'Texmet', this cloth is not quite so
dense.Texmetmadefrom absorbentfibres in a ~
binOOrexhibitsporosity which is useful for trapping
grindingabrasiveandlubricant

I
;'

Finally,what is requiredfor brittJefracturemateJials

suchasmineraJs?Soft cloths are unsuitablebecause
of interphaserelief grinding and ~ffici~t material
removal rates. The Texmet cloth, although
marginally suitable, does suffer from robbing and
relief. The answerthereforeis to have a fine weave
low weight denim cloth such as natural silt i.e.
mira-pol
These four examples serve to illustrate the
shortcomingsin the traditional blinkered approach
with its 6JIIDTexmet and 1JIIDMicrocloth for an
materials.

@A

MET Au..O6RAPH'i EUROPE

DlAM 0 NO PO 1JSHIN 6

CLOTHS

Sincepolishingis the stepd1attakesplaceafter

achievingsampleintegrity.its function mustbe to
removetop surf~ scrau:bes.
improvereflectivity
andwherene~-~ry introducedie submicrometre
interphaserelief n~-~
for differential
interferencecontrast.The cloth will be soft (non
abrasive)andwill exhibit a shortnap.Oneexample
of diamond~llihin& clothsis Microcloth

SLURR"'l POlJSHIN6 CLOTHS The requirementof a slurry polishingcloth is

differentto d1atof a diamondpolishing cloth in that

it d~ not havea high densityvertical fibre nap.
Slurry polishingclothsarevery soft and~ fibres
arenon veI1ical. A goodexamplewould be the
Selvytcloth ~d for polishingbrassand copper.
Oneimportantfunctionis the retentionof liquid and
to this end someclothsencompassa foam
subsurface.AnotJr;rexampleof liquid absorbency
would be the felt type cloths. Absorbentfibres such
ascottonwill be betterfor examplethanman made
fibres.
Examplesof slurry ~~&
cloths are:-

J:

.
.
.

Mastertex
OM:momet

Polimet
Suitableslurrieswould be allIminaI magnesiaI
cerimnoxideI colloidal silica.
SLURR~ &RINDIN& CLOTHS

The thoughtof usingan abrasivegrinding particle as

small as O.OSJJInin a grinding modeat first seemsa
strangecombination.however,if grinding is
~~-~~ry to achieveintegrity then suchsmall size
abrasiveswill be n~-~~ry. If for examplethe
sma]1p-~t
elementor phasein the specimento be
preparedis sayO.5JIIDthena grinding abrasivemuch
~a11P:T
thanO.5JJ1n
will be n~-~~ry.
The dangerwhenselectingthe sluny grinding cloth
with suchsmallabrasiv~ is to ensurethe abrasive
follows the conventionfor grinding and not
polishing.i.e. the abrasivemust not ~ and fall at
the point of cutting.
Exampl~ of slUII'YeliDdin&cloths are:. Texmet
Utra-pol

VERY HARD MATERIALS

(tungsten

carbide)

BRnTLE FRACTURE MATER~S I

(ceramics/ minerals/ refractaries)

SOFT DUCTILE MATERIALS

(aluminium/tin/lead/
copper)

0
0

DUCTILEMATERIAlSGENERAL
(ferrous/non-ferrous)
METAL MATRIX COMPOSITE (MMC)
(high

particulate

concentration)

;0

GLASS MATRIX COMPOSITE

CERAMIC MATRIX COMPOSITE

LEGEND
(in order of severity)
HIGH
M=ULTRA-PAD hard woven cloth
N=TEXMET 2000 chemotextile cloth
I
O=NYLON soft woven ~Ioth
P=ULTRA-POL low denier silk cloth
lOW
0= RAM ocetate silk cloth
:

FIG 5.38 GRINDING CLOTHS- DIAMOND ALUMINA CH,A.RGED

MATERIAL SPECIFIC

~:"J. ~..'

i.",,-;';~~

VERY HARD MATERIAlS

(tungsten

carbide)

BRITTLE FRACTUREMATERIALS

POLIMET/SP

(ceramics/ minerals/ refractaries)

ULTRA-POl/DP
CHEMOMET/SP

SOFT DUcnLE MATERIALS

(aluminium/tin/lead/
copper)

MASTERTEX/SP
CHEMOMET/AK

MICROCLOTH/DP/SP
RAM/DP
CHEMOMET/SP

DuCTILE MATERIALSGENERAl

(ferrous/ non-ferrous)
MATRIX COMPOSITE (MMC)

POLIMET/SP

(high particulate

concentration)

CHEUOMET

/SP

/ At<

GLASS MATRIX COMPOSITE

CHEMOMET/SP

CE?;A~IC MATRIX COMPOSITE

MASTERTEX/SP
MASTERTEX/SP

POLYMER MATRIX COMPOSITE

CHEUOMET/SP

LEGEND
DP-diamond

polishing

SP-slurry polishing

AK-attack

",

polishing

CHEMOUET-hard materials-soft
MASTERTEX-saft materials-hard

5.39-POLISHING

mate-";;:ls when using high ar low pH attack polishing

mat~~ials when interphase relief is required

CLOT~S,/MATERIAL SPECIFIC

Cl\4

MET ALLOORA.PH"i EUROPE

Figure5.40- This cban givesan indication of the choice of
grinding or polishing abrasivebest suited to a particuJar
materialgroup. The questionof which type of abrasive,
shouldit be diamondand if so what type? Shouldalumina
or colloidal silica be used?- how can the pH be changed
andwhat effect will it have?
Firstly considerdiamon~ usually offered in two distinct
fonDS: monocrystalline (R)
and Polycrystalline (S).
Diamond can Wo be nabJral or manufactured.
MonocrystaIIineasshownin figure 5.40 A havethe blocky
sharpedgedform whereas polyaystalline are less blocky
andaremulti-facetedoffering morecutting points.

"""
8dw- of monocrystanlne diamonds in META-D!
SuSP8ftsi0n8 -clean and effic~
cutting
ection.
Particle size 45 micron. SEM - 450x.
, . .

DiamoM

Spherical 8h8ped polycry8tatline diamoftd8 ., ME:TAOI SUPREME

provide n_roU8
cutti". laceta on the particle surface.
P8rticle alze 45 micron.
SEM
450..

Figure5 4OA - Diamond Abrasives

m on cx:;rystallineJ pol ycrystaIlin

f1)A

METAu.06RAPH\' EUROPE

DEFINITIONS

deformation.lappingis slow. very fiat and bas a reduced

sttucmral damage. Compositeswfaces(resin matrix with
metalor ceramicpanicles)~n usedin the grinding mode
offer extreme flatt!ess and reduced deformation when
comparedto grindingandarequickerthanlapping.
'+ Grindin&: The abrasivewill be fixed (or stationary)at the
point of cutting.
Appearance:shiny andscratched
~ LaUl!in&: The abrasivewill be moving (or rolling) at the
point of cutting.
Appearance:dull mattfinJsh.
-+ Pol~hin2: The abrasivewill be allowed to 'rise and fall'
within, for example,the nap of the cloth at the point of
cutting.
Appearance:shiny without scratches.

MATRlAL REM0" AL
SURFACES

GaJlfRfGW88L
- .
~~~~
~~~~;~~6"
~r..

GRINDING..-c

~ .. VUlEDA8aA1IVE

~-.

faDA88ASI''E
~ALMAnIX

MCSELftA'ra
8NGi.BI.A.YD
IOMm'IDA8DIrt

8Di!CMAnIs:
t6S'rAJJCDAMICPAaT1C1LA'R
CBAaGEDAsusm

8DaP4CE
(MEn.4P)

. MEr AL OR GLA8
L4PP1NG
8[JU' ACE

GalNlHNG
~
a.OrB 8(JRJ'Aa

I:~-:d
-

~a~

I
~

~a.aIB
':0 D AAA8ft

FigureS.STypesof materialremoval
Figure 5.5 gives 5 examplesof different generic material
removalsurfaces.
Grindin&Wh~l
Grinding wheels cover the abrasive binder/matrix group of
surfaces where it is necessary to wear down the
binder/matrix during use in order to expose fresh abrasives.
Examples of this would be the resin matrix or vitrified
grinding stone which has a silicon carbide or alilmina
abrasive. generally used for planar grinding of ferrous type
mate~

S.3

AMET

Au-oeMPRY' EUROPE
What happens in practise therefore is the polycrystaJline
abrasive does more gentle cutting (Jess defonnation I
structural damage), the monocrystaIline being aggIessive.
An additional commercial factor infltJelK:ing the choi~ of
diamond is that polycrystalline is more expensive. From the
chart, figure 5.40, it can be seen how mon<x:rystalline~ has
been used at the planar grind for all materials, continuing to
conclude d1e"sampleintegrity stage' for vel)' hard materials
and earlier as the specimenmaterial becomessofter.

Alumina has been used in the preparation of fenous

materialsand othersfor manyyears,it is also an excellent
abrasivefor polishingmany materiah. It can be made by
addingwater, oil or alcohol to gradedaluminapowder or
alternativelyto usethe readymadeslurry. Micropo1isbn a

deagglomerated
versionis available,
duplicatingthe ~al1P;r
particle sizes;the advantagebeing a more unifonn scratch
panern. Very simply die choice is simi1arto that of die
diamondin that thereare two versions,the more aggressive
hexagonalalpha alumina m and the more gentlecubic
gammaalumina (U). It follows therefore that polishing
would be caIried out with the gammaand integrity stage
with the alpha, this is confirmed on chart figure 5.40.
Alpha alumina'sare shown as 5J1IDI IJ1IDI O.3~, these
are all high purity white alumina and can be levigated
powder fonn or as a slurry. Coarsergradesfrom 25~
down to 3JJJnare also usedfor lapping applications,d1ese
alpha alumina'sdo not ~
to be die high purity white
version.
Additionallyto this rangeof alumina's,which are ma(k;by
crushing from large particles, is the seededgel almnina
(Masterprep)which is grown. A conseq~ce of d1isis a
aggregateparticulate that is one tenth the size of an

equivalentcrushedalum;na Furtherto this the O.OSJ1lD

Masterprepis the harderalphaphaseand not the gammaas
the traditional O.OSJ1lDalum;na The net result is a nonagglomeratedharder abrasivewith a much reduced size
aggregatethat gives efficient material removal com~d
with a superiorsurfacefinish. Masterprepis also beneficial
when automatically dispensing due to the lower size
aggregate.
Many materialswhenpomhedhavea tendencyto smearthe
upperworked surface. Although almninais a very efficient
material removal abrasive. it will when used with a
polishingcloth exhibit this abemtion.

METALLOEiRAPH}' OROPE

(.
Finepowderaluminais restrictedto gammaO.OS~. When
~g
with materialsthat are in any way water solubleit ~
pos,gbleto make a sluny from polishing oil or alcohoL
AltOOUghall1mina does not benefit from dissolution
polishing (high or low pH). It does have the added
advantageof being cbemica1lyinert and when mixed in
slurry fonn can be neutral.Le. will not attackinclusionsetc.

t1
\:

J~

METAu.06RAPH"i EUROPE
COOVeI!elyto die situation above where a high pH could
cause 1D1welcomematerial surface dissolution there is a
n~ for a c~r.ai1y inert almnina suspension. ~ ~ the
Micropolish C which is a I JIIDIK:xagonal gamma alumina
(U). Additional to this range of alwnina' s is Masterprep,
d1isis an alumina made by a seededgel process where the
panicles are grown as opposed to die nonnally 'crushed'
and sized particle method. This process allows a nonagglomerated suspension to be used with automatic
dispensing systems (Metlap 2000 dispenser), the particle
size confined to O.OSJ1ln.Note Masterprep is not shown
on die chart, but would be in place of 'U' when
automatically dispensing.

Colloidal Silicais the most importantpolishing abrasiveto

be added to the metallographersrange of polishing
abrasives.The particle size can be as low as O.OlfJlnbut
for generaluseO.OSJ1IDis recommended.The interesting
feamre of this abrasiveis its shape, unlike diamond or
alwninawhich aremulti-facetedcolloidal silica is spherical
Resultingfrom this shapedabrasiveis a surfacefinish that
is devoidof scratches.~ with the alum;",.. the pH of the
81mI)'is extremelyimportant, Mastennet (W) has a high
pH of about 9 which helps when surface dissolution ~
required. When comparedwith alumina as a polishing
~nsion
it is not so aggressivebut gives an improved
scratchfree finish. Colloidal silica can usually be diluted
with water to a ratio of one to one without any loss of
performance.
Whenit ~ requiredto lower the pH an ammoniastab~d
versioncan be usedwhich allows die addition of a dilute
acidagaincausingdissolutionof specifICmaterials.
Supplementing this range of polishing abrasives ~
Masterpolisb (Y), ~ combiIa the efficient material
removal qualities of alumina with the ex~llent surface
~
resulting from using colloidal silica. Figure 5.40
depicts the material specific applications for this
suspension.Finally there is Masterpollib 2 (Z), again a
mixture of aluminaand silica with an additional ingredient
which createsa ~mical reaction with ceramic material
enablingmoreefficient cutting.
Figure5.41 - Lappingis a gentlefonn of materialremoval
that is less aggressivedIaDgrinding and usually gives an
extremelyplanarsurface.

~
~

VERY HARD MATERIAlS

(tungsten

carbide)

BRITTLE FRACTURE MATERIALS'

(ceramics/ minerals/ refractories)

.-

*
#

-* -*
#

#
-.

*
#

SOFT DUCTILE MATERIALS

(aluminium/tin/lead/
copper)

DUCTILEMATERIAlSGENERAL
(ferrous/non-ferrous)
METAL MATRIX COMPOSITE (MMC)
(high

particulate concentration)

GLASS MATRIX COMPOSITE

-.

- -

_.

CERAMIC MATRIX COMPOSITE

POLYMER MATRIX COMPOSITE

LEGEND

-SiC

SLURRY

* -ALUUINIUUOXIDE

-DIAMOND

FtG 5.41-LAPPING

ABRASIVES 'MATERIAL

SPECIFiC

GLASS MATRIX COMPOSITE

CERAMIC MATRIX COMPOSITE

B D
R
~

.#

1.
POLYMER MATRIX COMPOSITE

8 D
R

I - /I
.
.i L
R

N
D E
S (,.,Ar, P $

- '*

s u
w z

L N

N,O

R T

0 S

LEGEND

A-ULTRA-PREP
DISC

m~tol bond
e-OIAMOND GRINDING W"'iEEL
C-UL TRA-Pl.AN metal mesh
D=BUEHL[R METL.AP PLATENS
E-UL TRA-PREP DISC resin bond
F'
G
H-VlTRIFlED ALUMINA WHEEL
I
J-VlTRIF"IED SiC WHEEL
I<-ZIRCONIA AlUMINA PAPER
L-SiC PAPER

=SIUCON CARBIDE SLURRY

* =ALUUINIUUOXIDE SLURRY

M-ULTRA-PAD hard wov.n cloth

N-TEXMET 2000 chemotextile cloth
O-NYLON soft woven cloth
P-ULTRA-POl
low denier silk cloth
O-RAM acetote silk cloth
R-D4AMOND monocrystoln
S-DIAMOND polycrystalline
T=MICROPOUSH A/hard hexagonal alpha alumina
U-MICROPOlISH B/less hard cubic gammo alumina
V-MICROPOUSH C/hard hexaQonal chemIcally inert alimina
W-MASTERMET colloidal silica high pH
X-MASTERMET 2 colloidol silica low pH
Y=MASTERPOLISH colloidal silica/alumino
suspension
Z-UASTERPOLISH 2 colloidal silica/alumino/iron
a.,de solution

-DIAMOND

~fG 5.42-THE

COMB~NED CHART - MATERIAL SPECIFtC

.A

METAIJ.06RAPH"! EUROPE
Its applicationis specificto brittle fracturematerialsas can
be observed on the chart. Also notice how lapping
techniquesarenot usedunderthe polishingcolwnn. When
observinga lapped finim it will have a matt appearance
with brittle fracture materials. From figure 5.41 observe
no lapping is to be carried out on materialsexhibiting any
ductility.
Figure 5.42 - This chart is a compilation of all the
infonnation given in the previous chans. B~hler issue
specific DIALOG methods, these are methods that
confonn to the concept of 'sample integrity' prior to
polishing. The representsampleintegrity in the shonest
time. The idea of the combinedchart is to compile this
infonnation as shown enablingmethod coDSttuctionover
the whole rangeof materials.

GRINDING
POUSHIN6
OPTIONS GUIDE
CHART

This guide is intended to assist in ( I) compiling a

preparationprocedurefrom first principlesor (2) to modify
an existingproceduregiven the severityrating wid1ineach
group of grinding I polishing swfaces. It will be
recognisedfrom the previousinfonnation. the importance
of selecting the correct size abrasive relative to the
induced residual damage.'Ibis choice must be made in
relation to the severity of the chosensurface. From the
chart it will be noticedbow ~ threeimportantstageshave
beendefinedLe.
1) Planargrinding (wherenecessary)
2) SampleIntegrity
3) Polishing(not alwaysrequiredwith hard
materials)
A suggestedabrasivesizehasbeenindicatedfor the 3
stagesi.e.

.
.

Planargrinding > 300m >P320

Sampleintegrity - group1 < 300m< P320
group 2 < 9um < P1200
group 3 < 30m
Polishing - < lum

When selecting grinding/polishingsurfaces be aware of

their severityrating from 5 to 1. '5' beingthe most severe,
'I' being the least severe. Also notice how a grinding
surfacein one group has a different severity rating when
positionedin anothergroup.viz:-

5.33

J~

METALLOGRAPH"iEUROPE

\.,

Texmet"9' in sampleintegrity stage

. Group 1 - severityrating 1
. Group2 - severityrating 3
. Group3 - severityrating 4
So bow doesthe systemwork? From any given procedure
it is possibleto selectupwardsor downwardsin severity
from a given position. Takefor examplethe following
cases:Fault 1

Sampleshowsgrinding inteIphaserelief

Remed~1

Usehighernumberedsurfacesin die sample

integrity groups,if severity 2 tty 3 etc.

Fault2

Samplegiving high porosity levels.thought

to be preparationinduced

Remedx2

Uselower numberedsurfaces

Fault 3

Grindingscratchesvisible after the polishing

stage

Remed~3

Usehigrer nwnberedseveritypolishing cloth

~rationa1 Checkmt for success

.
.
.

.
.
.

Optimise platen/specimen head rotational

speed.
Select grinding surfaces relative to residual
damageafter sectioning
From the options in each group select the least
severe (1) for perfection, the most severe (5)
for speed and high material removal rates.
NOTE it ~ not ~ssary
to use a grinding
surface from all three groups at the sample
integrity stage.
Use only one polishing step, select the m~t
severe (5) for planarity, the least severe (1) for
reflectivity.
Use vibratory polisher for scratch free,
deformation free or controlled differenbaI
abrasion polishing (explained in the microscopy
section).
Use COn'eCt
extender to reduce cost.

J~

METALL06RAPH'i EUROPE

.
.

,.-

Use not only the correct sizedabrasivebut also

its correctshapeandtype.
Do not prolong polishing times wmeressarily
( S minutesmaximom).

".':
C!)

BUEHLE

C;rUIDf;-

UL.T~- P'2'f"P

'D'SC (U) 1DI/O..~ PAPe~p~-.ACfD

YrT~IFIf'D AtA

AlUMILJ.(PA~

'~EL
I~2~1L.!'i

WIlEtL

'Df.N.4O1JD
(Psoo)

"'~ltE'D
t+".;EL.

'5tc'
PltO

, ~I~~
.

rM~

FZI

V1..T2.A-PAb;

PItO

I "DIAMOlJD(P!%~)

'54.ICCJJCA26/DE:-I JJ"( LO~

UL.T~A-PtZ!'P
"'DISC f..:) 'TO~.

UL~'CISC

0 L. J~1e-,.

"'e-XA1ET'W

PREP
(2)~.

U1.i2A

- f"R'P

MIC20CLOT~

':>I5c. (2) !-CQ...

~L.ICOU C~e.ICf
PApe:~ P3tO-~:>O

MErLOAP

,,-t. 4:

TEX~T

Mrn.AP IJ8I e l'

TfXMET

'H'

ULit.A - POL

'H

C,14EMOMfT

~fL I(OJ! C,AR!u)f'

PA~
P'~!I.AC

.3

2.12COJ.J
IAjAUlMD.'A , UL1R.( -

PAPC- ~

PL.Ao:JoJ

POLI~ ~I

P8'J/J80

"UL'TeA - PAD

ULTe4-:-PLAU

I~T

JJYLO

CAST~
L,~
p~ -aoo

T~J.4ET M"

~ETLAP .~I. ~o

j
CAST I~

PC2F. ,E?<.Mf"

LAP

CA5T~ 12qJ LAP

p,~o

Te.,<J.AE'T'W

M!CE'OCLOi ,.

!':"_7-

POL

(YI82.CIIffT)

~A~

io-

-"-'-0

PAS~.. ,,-

~-

.
,~:-.
.
c._.
.!-~
,.-.olAoOOAl8
.
S-. ~
.
SOM~_..
~-

~Oo
~.:..~
a.4S-~
OL. ~
~~O_!
.

MASTEeT~
(\'16~O~ET)
UL.7E.A

-SEYE2JTY2AT1~'G - 5 MIGM
ft LOW

~~
.10 -

~i~ - POI.

'RAM

P3lD

~~O_.
s- ~

j MAS'TE2TfX

d~

f~::
:
~==:
t~00Ae4DU8
w.a.
~-- ~
f~__.
.~ ,,-.

,~_..
IS_~.

- ..:-.
-.

So~-~'-"
~

..

~~-

.
.

~_.
r.~_.

011..
SIOr'. .,

i:=

,.

p...,.-;
.

.
--~
:
W8.-

.
.

~- .

s__.

1M-.-.~..~~.
3=~~~
A
,
3_~
.,..~
1
.

--.

~
~_.
I ~--

~~".",..-"~

-~

.'IS-.
'0- --

o'u-.

".0-

...
- -. - '...r,
. -.

-'00 _..~~
.

0...s.- 0."_.
-

"-.
- A;i

. --."

,--

-- - - --, .'

~..

~~

- -.'

--

--

-"

~~~~~
Ji;o-_~---::==~

iliA

METAlJ..06RAPH\' EUROPE
Additionally, this stOnewould be used for 'more d1an
normal' materialremoval. When grinding hard materials
such as tungstencarbidethe grinding wb~l would be a
diamond, me~
matrix. ~ wb~l would not be
suitablefor softer materialswhich would not wear down
the matrix, it would however be most suitable for an
brittle fracturemateria1s
GrindineDiscs
Singlelaid abrasivesare bondedto a rigid suppon, often
metal. Whendiamoodor albic boron nitride they tend to
be nickel plated onto the surface,the backing when not
metal can be fibrous which improvesthe shock absorbing
characteristics.
To aidswartremovalthe abrasives
tendto
be in uniform clusters. Thesediscs could be used for an
brittle fracture materialsbut it must be rememberedthe
abrasivestandingproud of its supportrendersthe disc less
robust than the ~uiva1entgrinding wheel If for example
very hard ceramia or tungstencarbidewas to be ground
on d1is surface its life expectancy would be grossly
reduced.

Com~siteSurface
These engineeredcompositesare made to satisfy the
deman~ of ~n
flatnessand sampleintegrity. The
chargedabrasiveis intendedto imp~ into the composite
surfacematrix (epoxyresin) as the sampleunder pressure
passesover, therebycausinga aiDdin& effect The rate to
which the compositesurface wears, is governed by the
particulatematerialandthis mustbe matchedto the sample
materialLe. steelsampleswould requireiron particulatesin
the composite surface. Brass samples would require
copper particulatesin the compositesurfaceetc. These
platen surfaceshave appJicationswith all brittle fracture
material and ductile materialsexcludine soft metals Le.
non-alloy,copper,tin. lead,aluminiumetc.
La!J!'in& Surface

Lappingis slow and gentle,an abrasiveslurry is 'dripped'

onto the, often cast iron, platen. The specimenunder a
~
pressureis lappedas the platenslowly rotates. This
operation can be done by band as is the case with the
geologistwho thins his sectionsdown to 30JjJDusing 600
grit powder (silicon carbideor alumina)on a glass plate.
Lapping is applicableto all brittJe fracture materials but
must not be usedon ductilematerials.

~A

METALL06RAPH"/ EUROPE
Grindin&l.fg1ishin&Cloth Surfacr.

It may seemstrangeto call a materialremoval action on a

cloth a grindingstage,but from our 'defInitions' this is
what happenswhen the cloth or fabric is ingressedwith a
resin. We thereforehave cloth surfacesthat can be used
for grinding or polishing. With the high matrix ~
surfaces this can readily be appreciated (Perforated
Texmet). With the resin partially ingressed cloth the
samplepressureresists the tendencyfor the abrasiveto
'rise and fall' during cutting, ensuring a grinding action.
With the softer nap type cloth and reduced pressurethen
the abrasivewill 'rise and fall' during cutting giving a
polishingaction. Thesesurfacesare employedwith nearly
every materialand thereis a great variety availablespecific
to particular ~imen requirements. The' great variety'
can by itself prove very confusing hence the reason for
further explanationsto follow.
PREP AKA nON
TECHNIQUES

\
~
~
6
I~

,,
~

~~~--/

\~:::=~
~

'~..IT~~
~c

"}
:.

STACB
~DIAMOND
- HARDa.om aJNDlNO)
DIAMOND
I~
- SOfTa.om ~O)

Figure 5.6 - Hand Preparation

Figure5.6 givesthe informationnecessaryto cany out the

preparationof materialsby band. On this occasionfour
strips of silicon carbidepaper are used, the samplebeing
traversedbackwardand forward. The specimenis rotated
through900as shown.

5.5

@A

METAu.06R.APH"i EUROPE
After P1200 grit the ~imen requires two polishing
stages,one using 6J11nabrasivethe other 1JIm. Both
grinding and polishingare .wet' operations,grinding with
water,polishingwith an extenderof lubricant. From figure
5.6 notice how the polishingaction takes the fonn of a
figure eight.with practisethis is madily ~hievabJe.

Without much skill. specimens

are rarely flat from this
technique
~

~ ..-,

t6~

IS~'

S'fC"~

'.0

~~M~
~co.,-.

~~

Sl..:K'I. T u:ss ~
p~
GRwCI ~

~~D

Figure S.7 Rotating Platens

Three examplesare shownin figme S.7, the first being a

simplebandtecbniq~ where the sampleis ~1d againsta
rotating platen having the appropriategrinding/polisbing
surfacesattached. In order to use all the platen surface
and to avoid directionalgrinding/polishing,the specimen
will requiremoving,if possiblein somesonof rotation as
shown. Specimenspreparedthis way can be much flatter
than by the stationarymodeabovebut lack the control of
machineautomationasfollows.
In the next example,three specimensare clampedinto a
specimenholder, the pressurebeing directedvia a central
spigotasshown. For a moreuniform fon=ethe specimen~
driven in a complementary
directionto the rotating platen.
For unidirectionalpreparationthe relative motionswould
be contra. This systemhas many advantages.The one
draw backhoweveris ~ ~ty
for planargrinding.

/1)4

META.IJ.06RAPm' EUROPE
Planargrindingis ~~~-~~'Ybeca~ the action of clamping
the specimensin the specimenbolder dictates a position
which rarely is planarbetw~n all specimensin ~ bolder.
The last exampleis where the three samplesare ~ to
move within given constraints and although driven as
before haveindividualloads enablingeach specimento be
plane with the rotating platen. Planargrinding not being
~
allows the samplesto be preparedon the exact
surfaceneededrelative to specimenresidual damageLe.
after sectioninga component(sample)the residualdamage
was so small (lOJ!ID)that one grinding cloth sUlface~g
3J!IDwas all that wasrequired.

SURFACE TENSION

SURF AC[

TlNSION

HIGH

CUTTING LOW

.~

D .8

""~;//':?//I

SURrACE TENSION LOW

CUTTING HIGH

Figure5.8 SurfaceTensionI Water

Surfacetensioncausedby the specimens,platensurfaceor
lubricating mediumwill adverselyeffect material removal
from the workpiece(specimen).The sketchin figure S.8 h
representativeof aquaplaningwhen flushing a grinding
surface with water during im operating cycle. The
operator of any grinding equipment where water h
employedis askedto listen to the grinding 'sound'. ~ the
water flush increasesso the grinding decreases. Under
certainciICtlm.-~~ vibration will be createdthrough dJis
surfacetension.this often is totally eliminatedby reducing
the water volume. Soapsolutionscan break down surface
tension.

S.7

@4

METALL06RAPHi EUROPE
Compositeplatensurfacescan ~ be affectedby surface
tension, this is why porosity is so vital in the
resin/particulate combination. Surface tension will
inaease as the specimensurface centre line average is
reduced.,i.e. as the specimensurfacesmoothes. To have
an emul~~er in the lubricant can ~
help in reducing
tension.
Grinding/Polisbingcloths are also affected by surface
tension.Developmentwort bas shown bow cross-weave
clothsremovemore materialthana smoothcloth ~g the
samesizeabrasive.

~~~~~~~~
CR c ClO",
INICR!I" CROuPNo .

9-'~ "'<'-'~

---

~7/7

;~~~

CR~
C'-O'H
NTECRITYr.Roc.. No J

, - 3 nIic-'re

~--:;-;~j-~-;-/
~~:-:-;~

~;;-/;.,,-;-~-;,,:~~

~
CLO11t
w1tCAfTY CR()JP No 2

POI.IS.-.CC1.O1)C

J-9 ...c,-,.

-~

~-1 "OC,_I,. 0"-

FIgure 5.9 - Grinding I Polishing Surface

Figure 5.9 shows a series of aggressive cloths. Those
cloths intended for grinding with 9 to 15J1Inabrasive, have
a course ~nier cross-weave pattern. These aggressive
grinding cloths are cla.c.~fiedas integrity group I (to be
explained later).

As we move to a Jessaggressivesurface(integrity group

2) the denier becomes~
to be compatible with the
reducedabrasivesizeof 3 to 9}JIn.
The last grinding cloth in any preparation procedure will be
an extremely fine denier weave or the resin ingressed type
as shown in figure 5.9.

I1JA

METALLOORAPH'i EUROPE

Finally, the polishingclodl with i~ densenap surfacefor

diamond polishing or the soft 'selvyt' type surface for
oxideisilicapolishing. The surfacetensionin this case~
more relatedto the specimensmoothness.If the specimen
is polishedbeyonda particular smoothness,dlen rubbing
rather d1anpolishingoccurs, resultingin a loss of sample
integrity and with soft materialsthe 'orange ~r effect.
To overcome the surface tensio~ emn1.~fierscould be
used;the prefenedroute is to ~ a high or low pH oxide
or silica polishing suspension.

THE CLASSICAL
APPROACH

Europeangrit designatednumbersare different to those

numbersquoted in the U.S.A. To avoid confusion~
using Europeansizes the letter 'P' ~ placed before grit
numbers.Comparisonof grit numberswand J11Dsize ~
shownin figure S.lO
USA
European
Grit
40
80
120.
180
240320400.
600800
lCXX>
1200

Averase me
(.-In)

Averasesi%.e
(,.D\)

428
192
116
18
53
36
23
16
12
9.2
6.5

Figure 5.10 Grit Comparisons

412
197
127
78
58
46
35
2S
22
18
15
6.5

Grit
P40
P8O
P120P180
P2408
P320
P400P6(X)P8OO
P1(xx)
P12(X)P23OO
P4(XX)

Figure 5.10. the grit comparisonchart. givesa comparison

betweengrit nmnbersalongwith theequivalent~ size

yNiAc.

Figure5.11TraditionalPreparation

.A

MET ALLOORAPH\' EUROPE

Figure5.11 is a graphicdisplayof the traditional approach
to specimen preparation where the manifest residual
damageis removedby subsequentsteps,progressinginto
the sample.Notice the termsusedat eachstageLe. Rough
grinding,fine grinding,rough polishingand final polishing.
The methodof pro~ng
the samplethrough the various
steps(7) is to o~
the surfacefinish at eachstage and
ensure scratchesfrom the previous stage are not in
evidence. At the completionof all the steps the sample
will be shinyandwell polished.

THE NEW CONCEPT

With the knowledgethat each ~tioning/grinding/lapping

or polishing stage manifests residual damage to the
workpiece (sample)and that a particular combination of
abrasivesand abrasivesupport would 11~, independent
of time, leaveat besta specificdamagedepth.This Z ~
damagebeingthe criteria to specimenpreparationand not
surface ~
It wu also realised that the abrasive
backing or the ability to absorb shock during grinding
would alsoreduceZ axis damage.Thesethoughtslead to
the questions(a) What damageexismfrom the ~tioning
stage? and (b) How can we progress this surface to
integrity without ~y
creating deeperdamage?

Figure 5.12 Traditional preparation within the New

Concept
Figure 5.12 graphicallydisplaysthe philosophywhere the
same number of steps (7) is still employed. but the
undamagedportion from the sectioning stage remains
throughout From this displaythe questionthen foremost
in our min~ is 'Could we omit someof thesesteps?'.

>4

METAu.06RAPH'/ EUROPE

Figure5.13- Selection
Figure 5.13 having addressedthe question of abrasive
selection,bas concludedthat three of the steps could be
removed without re~~rily
oompromLgng the total
procedme(sampleintegrity in the shonesttime).
As bas beenshown in the sectioningpart of this manual,
the residual damage can vary from IOJllD to 9O0JllD.
Considerthe materialusedin figure S.II/ S.12/ S.13now
to be sectioned under optimised controlled conditions
giving a Z axisdamagedepth.asshownin figure S.14

Figure 5.14 - Preparation Without Logic

To progressthe samplethroughany of the previousstages

would be totally illogical. As shown from the sketch the
240grit abrasiveinducesrather than reducesthe Z ~
dimension.

From this simplified explanationit can be seenhow vital

the sectioningstageis to any preparationprocedure. The
knowledgeof residual damageis the factor that dictateS
what the proceedingstepswill be.

<1>4

METAJJ..06RAPH"i EUROPE

Figure S.lS - Preparation with Logic

figure 5.15 completesthe procedureby baving a single

step only. The assumptionmack:in this discussion~ the
absenceof anyplanargrindingrequirements.
Z AXIS CURVES

When 'working' a materialthere will be a given depth of

residual damage relative to a given grinding
surfaceJabrasive
size and shock absorbingcutting action.
'Ibis depth (z axis) will vary with different materials;an
exampJe
for 0.37Steelis shownin figure 5.16

Figure 5.16 - DatabaseChaIt for 0.37 Steel (for

comparisononly)
Damagein micrometersis given for a whole series of
silicon carbick: papers and diamond polishing cloth
combinations.To selecta procedureusing silicon carbide
paperthe choicewould dependnot on surfacefinish of the
sampleto be prepared,but the estimatedor documented
residualdamage. On dJepolishingside it will be noticed
how the abrasiveparticle size is followed by 'PS. then a
number(9JJ1n
PS2). PSis shortfor 'polishing surface.the
numberindicativeof the polishingseverity.2 being low in
polishing(abrasive)- 8 beinghigh in polishing (relief).

5.12

J..i

METALLO&RAPH"/EUROPE
WbtJ1 progJeSSing a preparauonprocedurefrom

a known
damagedepth.what arecalledZ axiscurvescan be created
as the residual damagedecreaseswith 1ime. This ~
displayedin figure 5.17

Figure 5.17 - Z Am Curve Sequence

Notice how some of the steps improve then degrade

(1/213) this is ~~~~ silicon carbi~ in use develo~
tnmcatedparticleswhich eventuallyinduce damageback
into the sampleastheyremovematerial. StepNo.5 is also
degrading,this is the final polishingstep which utilises a
nappedcloth in orderto achievea shine,resultingin a slow
degradationof integrity. Step No.4 is a chargeddiamond
abrasiveonto a ~abric
surfacewhich will continueto

.aiDd without degrading from its 'best ~tion

' . This

graphic display bas beenrelated to O.37%Csteel and ~

shownin figure 5.18

,.K
-~

asc

~,
\\=:::~~~==
-

.-

I_~~

TFigure 5.18 Preparation Method for 0.37 Steel

OIM: of the major advantagesof depicting preparation

methodsby graphicdisplayis the technicalbe~fiu derived
from alternativemethods,figure 5.19is onesuchexample

J~

METALL06R.APm' EUROPE

3 SiI~

C8tIide p.,efS

1 PoIistW'D .

..
~
g~
..

",--

3 Platen ~
surtaces
1 ~-,
--ow

O' Time
Time .

',

----

'~--' -.~

~--:-'I

.
r.uh

Reduced
lime
greaww.egrttr

Figure 5.19 - Integrity ChaIt for Material MMC

A four step (3 SiC. 1 Polish) traditional method ~

comparedwith an alternativefour step mediod utilising
composite platen surfacesand a grinding cloth. The
grinding cloth ~ a 'polishingtype' cloth usedin a grinding
mode. Thesetwo methodsarebasedon the preparationof
a metal matrix composite. The important aspectof this
graphicdisplayis the informationthat can be derivedfrom
it. Viz.
Dotted line method(accordingto the ~play)
. Exhibitsgreaterintegrity

Takeslesstimetoprepare,
and

Doesnotdegrade
with time

Continuousline method

.
.
.

Doesnot achievethe samedegreeof integrity

Takeslonger. and
De~
with time

When comparingthe surface~

at the 'best position'
with both methods.they were consideredto be identical.
Figure 5.20 sumsup the two approachesie. surfacefinim
V s residualdamage.

METALL06R.APB\' EUROPE
TRAomONAL

"

L
Lx-

SECTtONING
MOUNTING

NEW
SECT10NING

r;~;~G-lX_.uJ=~~

I ROUGH

yRINDING
I FINE
GRINDING

'GRIND

I~ I ~ I ::::fTY
I

ROUGH
IPOUSH

cL

FINAL
'POUgH

IX

.
IHTEGRrrY IN THE SHORTEST TIME

.
,
HIGHLY POUSHED
Figure

--

I.:L.

5.20

- Surface

Finish

or

Integrity

In comparingthe two approaches

it will be noticed that a
changeof terminologybastakenplace. The ~ of words
such as 'rough grinding' and 'rough polishing' are
mimomers m the new terminology. Since all samples
would be ground or Jappedto integrity (i.e. we would
ne.Br polish a sample prior to achieving a faithful
structure)this group of stepshave been clA~fied as the
'sampleintegrity stage'. The only polishing that takes
placethereforeis after achievingsampleintegrity, this is a
~
stepandmust be kept asshott as possible.

FIgure 5.21 The Concept in use.

@4

METALL06RA.Pn EUROPE

MA TR1AL REMaV AL
MECHANISM

Figure 5.21 brings together all the be~fits of the ~w

Concept in surfacepreparationincluding the terminology
of eachstageand the appropriateabrasivefor each stage.
Notice how the sampleintegrity stagebas been split into
three groupsas the sampleprogressedto integrity. Within
thesethreegroupsthe ab~ve sizebasalsobeenincluded.
A severity rating, from 5 the greatestto 1 the least, bas
beenintroducedfor all grinding/iapping/polisbing
surfaces
used. This rating will apply to planar grinding, the 3
groups in the sample integrity and the polishing stage.
(The sketchonly showsthe rating for the 3 groups in the
sampleintegrity stage). The choi~ of surfacesand its
effect on progressing the sample to integrity will be
~ussed later under'preparationoptions'.
The two modes of material removal are by slip plane
dislocation for ductile materlab as a result of the shear
force from the abrasive. The other mode of material
removal is by brittle fracture which is the result of
cracking. Thesecracksemanatingfrom the shearstress
point having a major crack nmning along the shear axis,
odlers of lesser severity at angles from the major axis.

Figure 5.22 - DeformationI StructuralDamage

Relationshipfor Brittle FractureandDuctile Materials
If we observethe reductionin defonnationwith the steel
samplesasshownin figure 5.22, materialremovalis totally
by plasticdislocation. The upperpart of this sketchshows
what happensas a ceramic material is progressed to
integrity. Firstly, materialis removedby brittle fracture.
Towards completion of the preparationhowever, notice

METALL06RA.PH'i EUROPE
how ductile slip plane mechAni.clnc
occur until slip plane
disl<x:ationis the only mode of material removal. This
change..over
point is relatedto the fracttJretoughnessand
abrasiveparticle size and can be influencedby the shock
absorbingeffect of the cutting abrasivesupport.

.-r

II'"

Figure5.23 Preparation Sequencefor Ceramic Materials

Figure5.23 is an exampleof a preparationprocedurefor a
ceramicmaterial(reactionbondedsilicon carbide)showing
the two typesof materialremoval.

EFFECTOF
LUBRICART

We have mentionedthe materialremoval differencesthat

occur with changesin surfacetension,different lubricants
havean effect on this. In materialography,three different
lubricant types are available. These are, in order of
efficiency:-

1. Alcohol
2. Water,
and 3.0il
It doesnot alwaysfollow howeverthat this order will sti11
apply when combiningthe variablesof grinding/polishjng
surfaceswith differentmaterials.Oil for examplewould be
requiredfor soft materim in order to lubricatethe cutting
abrasive. The combinationof material/grinding-polishing
surfacemust be carefully considered.The following four
examplesareusedto illustratethis

Copyright 1994BUEJn..ERLid

S.17

METALLOORAPH"iEUROPE
.
""TrAil.!.
R[WOI/A:.

20

.~
I,

I
I
I

.A~

I
I
I

'5

..

-40IwOI"

I
I
I

'~I

I
I

10

-,

,oIcOflol

I
-oi

--

10

1~
20
(mnutes)
-IO(UTICI.L.POlISH..c CLOTH(T[x~
-SAMPlE UATERIAl0.4%C STEtL
-~ASP.'

~-

25

RS
(restort)

2000)

OIAUONO

Figure5.24 - Effect of LubricantI IdenticalOath (Steel)

-'[~

~~...
:~

t\

..

X'

.
,
I

"""7':

'k

.~
.

...

01..I

10

.
.

I
.
.
.

.
:

.
~

10

-UJlfCAL ~
-~
*1-.

~~

,~j'..

:
.

.
I
.

.
.
. -

.: - - - - :. - - - ;";

_Co-i

.-.COQ..

IS

20

(-)

.
.
I
.

~.. (T[X'" ~)
C-.a.: ;.eg:)

.
I
.
.
I

-.
,

2S

RS

(rntort)

6VIP.DIUIONI

Figure S.2S - Effect of Lubricant I Identical Ooth

(Ceramic)
A cbemotextilegrinding cloth. dosed with a controlled
amount of 6J1Jndiamond at set intervab when grinding
steel and ceramic specimem,was checked for material
removalat intervaJsof 5 minutes. Figure 5.24 showsthe
results from working steel - figure 5.25 the results from
working reactionbondedsilicon carbide. The first point of
interestfrom thesefiguresis the compatibility of the Water
baseddiamondsuspensionwith both the steeland ceramic.

Copyright1994BU~R

Ltd

META.u.06RAPm' EUROPE
the low figure and faIl off when using alcohol was
surprising. These results would abo show how the
reramic is more prone to surfacetension as the specimen
surface'SIDOOthes'.On the right hand side of both these
figmes is the restan (RS) dimension.this is the ma1erial
removalfigure after 5 minuteswhenthe specimenhasbeen
reUJrnedto its original ground condition. This restan
figure is what would be expectedin real life use. From
these ~
water is by far the most efficient with this
combination.It doesnot follow howeverthat theseresults
would be identical if for examplea nylon weave grinding
cloth wasto be used.
The 'smoother'and planarthe grinding surfacethe greater
will be surfacetension,figure 5.26 and 5.27 are examples
of material removal still using the steel and ceramic
samples,only this time using composite platen surfaces
(metal/resin).

10
t

~
~

PLATmfItJRPAa (~6)
WA1DJALo.4~ ITEm.

ABRASIVB 9 pM aAA*D

Figure5.26 - Effect of LubricantI CompositeSurface

(Steel)
Copyright 1994Bt~R

Ltd

J~

METALL06RA.PH"l EUROPE
...I(~

R(~...
.)0

2S

Ji/LH
: "~
/i:' : :
'/:
: .

20

1O

II

~~

-0

,~

:
I~

:0

\-"""",
-c~
~Tt..
Sij$J'A(( (~~
~
WA1t~ Ct~;
(R6SC)
-.aAASN( I
~:O

.)

Figure 5.27 - Effect of Lubricant I Composite Surface

(Ceramic)
With both thesefiguresthere ~ a tendencyto peak, after
which time materialremoval decreases.this is thought to
be causedby surfacetension. Alcohol ~ better for both
materials;attributedto surfacetension break-down,there
areproblemshoweverusingalcohol (Surfacepick-up and
vapour). Taking the first 5 min~ which ~ a real-life
figure then water ~ nearly as good for the ceramic. oil
beingslightly betterfor the steel

A&.O"\
MAT~~
ee...O/AL

~
IIR"~L
~A.L

Figure 5.28 - Use of Extender

Copyright 1994BUEm..ER Ltd

eA

METAu.06RAPH'l EUROPE
When using automatic abl3Sive dosing devi~ it ~
possible to monitor the dosing period and also the
economicdosingamount.It doesnot follow that the more
abrasivedispensedonto the grinding/po1ishing
swfacethat
an ~uiva1ent improvementin material removal will take
place. Increasedabrasivedosing can impede mate.ria1
removal. In generalthere is a point where funher dosing
of abrasivewill give little if any benefit, this is shown in
figure 5.28. From d1iseconomic dose the interval then
must be de~.d. It was found empirically that a loss of
effici~
was not encounteredif the abrasivesuspension
wasalternatedwith a compatiblesolutionof lubricantonly.
thereby reducing consumable costs by half. The
explanationoffered for d1issiUJationis the extenderwill
'clean' the abrasivesurf~ extendingits usefullife.

DIFFRENT CLOTHS

The experimentsused to define lubricant efficiency was

also used to illustrate how different cloths give totally
different results. Seven different grinding cloths. an
recommendedfor steel were tested for material removal
~~.
From figure 5.29 it can be shownhow 3 at the
bottom of the graph are so ;nPffi~P:Dt
u to be considered
W1Suitable
for this ~~lication. The efficiencyof the other
four varies from 20JJlnSto 28~s (figures taken from
restartposition).
WA18AL
8BI8OVAl.

I
.
.
.
.

'._#

/ /~-::l~~J'
1
I

~ . 20

,1"
.
.
.
.

:'

.:

'
-.::,. .-;..::.-:
I
,.

.-1

'-j-

--- -

.
.

1
.

-..

r
1

.
.
.
.

.
.
.
.

.
.
.
.

.
.
.
.

t'

.','

,---'-.,
.

~
v ARE'tT ~ ~
a.ontS
SAWPLBWATDIAL o...c
SIB&.
ABRASVB 6)aMw..a.ID
WA18. BAlm) UJBmcAHr

t
.
,
,
.
,

..
.

.""t

/ ",;:,"""""'r .

"

.
I
.
.
,
.
t

~.".l'
I
.
.
.
.
.
I

.'

. ''" "
','
.
I"
.
.
.
.

,,~
-;.
I
.

I
~

1O

I~
l-e5)

20

-~,
2~

-lM
(-..Wt)

Figure 5.29 - Grinding using Different Cloths

Polishing cloth selection is covered in the grinding

polishingoptionsguide.

Copyright 1994B~ER

Ltd

.
1

);~---:~:=:=i:::::~'
.
.
r "

,~

li>A

METAIJ.~RAPH'l EUROPE

6R1NDIN6AND
POUSHIN6

HIGHum:6RIn'THIN

SC110NS

Thin sections are now being made for much wider

applications than the traditional requirement of the
mineralogists Thin sections of bone, ceramics, teeth.
JK}lymers,refactories, implant materia]setc., have made
extta demandson the thin section- that of high integrity.
Implicit in this ~rement is the suggestion that the
mineralogism'thin section was 1ackiI1~in integrity i.e., it
was not a faithful representationof the true structure. To
someextent this is true, the mineralogism'thin sectionwas
howeverfaithful in revealingthe requiredinformation. It is
our expectationsof the d1insection that has changedand
as such the mediad of preparing the thin section must
reflect this changein expectations.
The c~~cal approachto dUn sections would be to lap;
ming silicon carbide or alurni~ powder, the material
smfaceprior to sticking down on a glassmicroscopeslide.
The abrasiveparticle size would be to 600 grit prior to
bonding the chip onto a glassslide. H the chip was to be
observedin reflectedlight, experiencewould tell us it has
not beenpreparedto integrity.

aD

1;'1 []

II~ ~~~
PStJLA:1D
c:=J

I-j

)-

-~.

il',.;--.,
SUPPLDefTARY

-J

~DeKnm DIPI1I~ naucn8AL ~ ~

Figure 5.30 - Thin Section Protocol

C~yrigbt 1994 BUEIn..ER LId

@A

METALLOORAPH}' EUROPE
Figure 30 shows the two different approaches.where the
primary working with the c~cic;:-cIlapproach means the
resultantthin section will ~est
d1isStructW"aldamage.
The targetthereforeis to achievesampleintegrity with the
primaryworking in advanceof any bondingoperation.
The methodof preparationof ~ first surfaceis identical
to that required for any other material. From our
grinding/polishingoptionsguidewe must make a selection,
notice how lapping has reen accommodatedin ~ chart
(PJanargrind severity 1 - sampleintegrity group 2 severity
2/ group 2 severityrate 2). Shouldlapping be the chosen
methodit must be followed by a grinding surfacein group
3 of the 'sampleintegrity' stage, polishing would n,Q1be
~.&-~ry. The useof diamondgrinding discs (Ultra-Prep)
have proved most soc~-eS8-ful
in dramatically reducing
preparationtimes.
0Ix:e the high integrity bas been bondf"..d to the glassslide
(Epoxy resin 2SO Cps) care should be taken when thinning,

not to Ie-introducea damagedS1J11ctme.

~ --- "'R(SSuR.
,
--.
I
,

'"

I
I
,

,
,..-

'.

,.
;~::;,.-f~~
~",,'
I

'

!.OI!R BLOC"
~L
SP[CIMEr~

-"""'"

ARE LMl

'r;;~;;;
=:f ~

I",," ~~~

~
-

1:\
~I
-- ClAWP

SCRW$

,
~-

::::!---:--::~

Q)

- ~~,
~ ~

UhTtl
Ct"!PS

THE" CL"MP

~TATION

.SPEC'MLHaLOC~ ,,~~

~-

SPtC"'~N ~OCI(
I SPECIMN CMP
BONOtD WItH lAKES'O "D

Figure5.31AutomatingChip Grinding
The medlodof preparationwhen lapping varies from that
of grinding,in that for grinding, the specimenrequiresto
be fixed This is done as shown in figure 5.30, where the
specimenchip of varying shapethe thicknessis temporarily
stuck to a specimenblock. The s~ens
can then be
1e\Ielled prior to clamping the blocks in position.
c~

1994BUEIn.ERLad

1114

METALLOORAPIf"{ EUROPE

Preparationandoptical observationis canied out with the

specimensremainingin the specimenholder. When
satisfactOrilypreparedto integrity, the specimenscan be
releasedfrom the specimenblock (by beating)prior to
fixing ontO a glass slide.

6RINDIN6&.

CAPITULATION

POUSH IN 6

Figure 5.32 graphically shows the various stages of

preparationstarting with the sectioning and its induced
damage. This strucUJraldamagebeing gradually reduced
by a riDdin& or Jaal!in& process called the 'sample
integrity' stage,until a faithful Structure~ achieved. This
structureis revealedafter carrying out the polishing stage
and~ accomplishedby one of the listed methods.

The machineoptimisedoperatingconventionsmust be
ob~ed in achievinggood resultsand thesehave been
listedJJnderoperatingconventionsfigures 3 - 5.33I 5.34/
5.35 (at the end of chapter)
In consttUctlnga method the choice of abrasivefunction.
be it fixed. loose, charged or OOgI'adingmust first be
addressed,
this is shownin figure 5.36.

OPERA.T~ TECHNIQUE:
MATt:R1Al

LAPPING

GR1NDING \ POUS"NG

I-~

,
,

METAL
"~ERAI-

OPERAl1NG METHOO

MATERIAl
""ERAI,.
\ HARD M:rAL
I ~,:,M
METAL

ILOOSEA8ASIVt (~

) I CHARCD.
ASRAS~ (GR!~)

,
,

,
-

DE~ING ~

-(~ PAPER~

HARD

MEDIUMson
METAl..
Y8Y -.r .
Mm'ALa

I.

.4 LARGE SIZE (3um)

, lARCESIZE(w..)

I NTIAUY

Figure 5.36 Method Construction

With all ~ infonnation and the "grinding/polishing

options gui~' it should be possibleto construct a
technicallysoundprocedurefor the preparationof all

@4

METAU06RAPH"l EUROPE
materials. From ~ derived procedureit should aha be
possible to fine nme the procedure given the severity
ratings for the operating procedure. in order to ~hieve
SAMPLE INIEGRcrY

SAMPLE
PREPAM TION
USINGTHE
CHARTS 5.32 TO

5.35

Figure 5.32 shows graphicallythe progressionfrom the

sectionedcondition to completionwhen the microstIUcmre
needsto be observed. In manycasesthe microStIUCblre
~
mble without recourseto etchingtechniq1ESas indicated.
When this is not possible men some fonn of chemical
etching or staining is required.
Figure 5.33 'Operating conventions for planar grinding',
this and subsequentcha1Ucan best be illustrated by using a
given method for example, in chapter 10 of this reference
manld1 Take 0.4% Carbon Steel MFJIAIM using a
2OOmm(8") 0 macltJDe.

Planargrind 180g SiC: from figure 5.33 ~ giv~ a

headspeedof l2Orpm and a wheel or platen speedof
200 rpm operatingin a complementarydirection with a
force of 5 Ibs (22.N).

Sampleintegrity takenfrom figure 5.34 - Metlap 6

with headspeed60 rpm and wheel speedof 150.
Texmet2000with headspeed120 rpm and a ~l
speedof 300. Texmet1000alsowith headspeedof
120rpm butwheelspeedof 250.

Polishingtaken from figure 5.35 - On this occasionno

polishingstep is quoted. If ~~-~~.
sluny po&bing
would havea headspeedof 60 rpm with a wheelspeed
of 80. Diamond polishingwould be at 120 rpm head
speedand a wheels~d of 200.

Attention is drawn to the note where contra motion m

recommendedin retainingslurry, this of course would not
be possible with softer materials. due to directional
polishingeffecu. Also note how the force is reducedfor
polishing, the ~ty
for this is greater with soft
materials and is often ignored as the sample hardneM
increases.

C~yrigbt 1994BUEIn..PR LId

TURE BY: I
HING
ING

- - - -,.

DIFFERENTIAL
INTERF'ERENCE

SECTIONING

INTERFERENCE
COATING

ELECTOL
YTIC ETCHING
CHEMICAl. STAINING

STRUCTURAL
DAMAGE

'.N
I

GROUP , I GROUP 21GROUP 3

I
I

I PLANAR
TGRIND

, SAMPL INTEGRITYSTAGE
1-

"

I
-

FIG 5.32- THE TRUE STRUCTURE-BY STAGES

",'

I
I
I POUSHINGI
~;A~E -i

CONTRAST

~BLE

STRVCWRE-BY 1

'CHEMICAL

ETCHING

>-e~'

..

DWTERENT~ INTERFERENCE CONTRAST

INTERFERENCE COATING
ELECTOlY'TICETCHING
CHEMICAl STAINING

~
SECTIONING

STRUCTURAl

DAMAGE

'

,GROUP 'GROUP
2-~'GROUP
'- --- 3
,

PLANAR

SAMPLE INTEGRITYSTAGE'

I,~OUS~INGI

OPERATINGPLATEN SPEED rpm

GRINDING OR LAPPING
SURF'ACE

ULTRA-PREP DISC
VlTRIFlED WHEEL
DIAMOND GRINDING WHEEL
SlUCON CARBIDE PAPER
ZIRCONIA/ ALUMINA PAPER
ULTRA-PLAN
METLAP No 10

CAST IRON LAP

so
H

~rol
PUfP9~t
HEAD rpm
120

200 1250,300 2
I
. - -

-1-

12501300;200 1250~

mm
-

Imm

Imm

PLATEN

PER

I DIRECTION 25mm2
I

t-11~

300
1?75
2
IC M
- -1'*
- T17~l:0"~~

. ,..Q:"\.1.

t- --:J

r"K

+ -

-t -

-1-

T -

-t -

-t

..~~

1'.~--

~1,,;1U

.JVU

"t

- tt--"t- "t~Q.IZ2}

~Q9-'t)

I
150113Q1?01:
* - -1- + - -t - -,-1 - t- - "t40-1'0T~-I==

.',

t--"t--

- -.. - -=

:~::

~T

I:

1 -T
5~
~vvl r27S
,~ '"250-'1 u I
- t- - "t-M
t-

.. - -,- - - -t - -,. - _1- - T

+--t- -t - -'+--t

rORCE

- - - 11- - - - - II- - .

HEAD

- -

..
-:

- Ii
-

..: - - ..; _
;

I
=-==--===:'

:J::

-.
NOTE: CONTRA-DIRECTIONOR LOWERHEAD SPEEDS FOR INCRE}.SEDMATERIAl REMOV~
W INCREASES MATERIAl REMOVALDIF"FERENCE
(MRD)
GRINDINGVIBRATION-THIS CAN OCCUR WHEN GRINDING
SOfT MATERIAlS
OR ALTERN4TIVEL'
WHEN SPECIMENSURFACEBECOMESSMOOTH
REMEDYUSE LOW PLATENSPEED WITH 120 rpm HEAD SPEED OR 30 rpm
HEAD SPEED WITH HIGH PLATEN SPEED
SOAP OR EMULSlnER WILL ALSO ALLEVIATETHE PROBLEM

FlJG 5.33-0PERATING CONVENTIONS FOR PLANAR GRlf-J(;ING

NOTE US{ CONTRA F'OR WORt AGGMSSr.'E WPROACH

GRINDING ~BRAT~-MS
CAN OCCURWHENCRN)I': son WATERW..$
OR AlTERNATNELY
WHEN SPEC...o. SURFACE BECOMES SWOOTH
REMEDYUS[ La. PlATEN SPED wnH 1~
HEAD sPEED OR Pm
HEAD SPEED WITH HIGH PLATEN SPEED
~
OR EMVLSIFlER
WIlL AlSO Al1VIAT[ THE PRO8lW

C'

G 5.34 OPERATI~G J:,O~VENTIONS FOR THE SAMPLE INTEGRITY STAGE

~-l~

B:f:J
-

OPTiCAl STAINING
DIFFERENTIAL INTERF"ERENCE CONTRAST
INTERF"ERENCE COATING
ELECTOl YTIC ETCHING
CHEMiCAl STAINING

- - - -.,
SECTIONING

=-

STRUCTURAL
DAMAGE

I
I
I
I
I
,GROUP 1 I GROUP 2 'GROUP 3

I
I

I
~

I
I
I
I
J POUS.tt!NGI..

SAMPLE INTEGRITYSTAGE

I. PLANAR

OPERATING PLATEN SPEED rpm

SURFACE

HEAD

ff~ ~~o~ r ~~ ~:jo I~~.~

FORCE

PEP;

;1 P!.ATEN

25mm21
\mm'2001250~300~
200-'250; 300;200 Ti56~300
Imml mmlmmllmml.mmlm~I,"!!,1
mml
" ".-,
- & to".,.~ - .. T -- - ~":'""
- - - - .. ~ ---- ---I--- --- T --- .,..-- - -.- - - - - - - - - - - - - - - - - - - .-.,. -. - I -:- T -. - I- - "- - - - - - - -- --I,-- -- T -- ~ ---. ---I.I;.:
-.- to-.,. - - - - - - -"-- - - - - -- - to- .,.- - -". - - - I- - - - - - - . - -- --,- - - - - .". - - - - ."-,- -- -- -.,- --,--.-- - -- --1- T- -.- - - - . _ . - - DIRECTION

"

POUMET
TEXMET 1000
t.4ICROCLOTH
CHEMOMET
MASTERTEx
ULTRA-POL 1000

,m

;'

~
"

1"

---1"-~

I 7"

a\

I.

I:

,..

to

.,.

I 17-

"I.

"1~

...

'-

.,.

to

.,.

to-"'

I"

I "

to

I"'"

"I"

"I

..;.

to

T"

I.

I'~

NOTETO RETAIN SLURR'r ON P~1[N

USE CONTRA
CONTPA CAN BE "ORE ErF'ECTM WITH SOME: MATERIAlS

FIG 5.35-

OPERATING CONVENTIONS FOR THE POLISHING STAGE!

J~

METALL06RAPH'l EUROPE

CHAPTR6

THlRmMlfASUREIIEBT
//""""
'
.

--,I
I
I

. lARCE'R
,--- .

I
I
.

"'\

son MATERIAL
OVER POLISHED

-DUCTILE MA!;RIALS SWEAR (OVERSJ~)

Figure 6.1 - Polishing soft materials,in particular when

somefonn of pressureis used, will often result in a top
surface smearing or burnishing. Although this ~
exaggeratedin the sketch it will take place and be more
pronouncedif uni-diroctional polishing is used. This
smearedsurfacewill 'lid' any pore or hole that is present
thusdisguisingor reducingthe visible size. Apparent size
of a smearedlayer will also suffer from size interpretation
asillustratedin exampleNo.4.
A solutionwould be to avoid any rubbing and use non-nap
type cloths, even if smaIlscratchesare visible - avoid the
bigblypolishedfinisb

2-BRmLE _MA1ERIAlSCRACK tUNDER:S.;

Figure6.2 - Brittle fracturematerials,as the word implies,

are worked by fracturing small particles from the top
surface in order to remove material. This fractured
damagemust be reduced,eventuallyto zero, if realistic
Copyright 1994BUEHLER lid

J..\

METALL06RAPH'i EUROPE
measuremen~~ to be expected. When dealing with a
ductile substratematerial, as shown in the sketch, this
damagefactor can inadvenentlybe overlooked since the
substrate and mounting resin would look perfectly
satisfactory. A solution would be to use shock absorbing
grindingsurfacesandsmallgrindingabrasiveparticles.

/- /"~--~-~~~'"
- - ~ ~LH~~E~ "'
I
II
.

I
/

son METAl
F1LLD
SPACE

v
~-SOME

RESINS CONTRAC~ (OVERSIZE)

Figure6.3 - Resincontractionmustbe avoidedor reduced

to an absolutem;nimumwhen the desiredcoating bas an
encapsu)ating
resin interface. The dangerwhen optically
observingthe preparedsampleand not seeingany fissure
at the coating/resininterfaceis to assumetheremust not be
any resincontraction. Whengrindinga soft materialit will
deform to fiB any vacant space causedby contraction.
Additionally, the swart removedwhen grinding the soft
elementcanbe depositedinto any othervacantspace,such
asa pore,giving an erron~ousmicrostructure.

rocus

LEVEL

-or--

'- - -..I-

"

f ~GER

\ I
\ - - - - -~-

I
I
.

R(U(F

4-.~_~~~~E_N!ERRORS
INTERPRETATION

DUE TO OPTICAL

Figure 6.4 - The apparent size of an object when observed

Copyright 1994BUEm.ER LId

J~

METALL06RA.PH'i EUROPE
down the mi~pe
is not alwaysa true size. Various
factors affect the image size such as aperture diaphragm
position (see No 5). A factor affecting the size from a
swface preparation point of view is grinding relief.
Polishing relief at the resin/coating interface causesan
angledfacerather d1ana planarfaceto be presentedto the
microscopeobjective. Due to the diffraction of light the
imagesizewill increaseasthe lower surfaceincreasesfrom
the focus level asshownin the sketch.

5-MEASUREMENT ERRORS DUE TO MICROMETER

EYEPIECE POSITION

Figure 6.S - Every subject bas a specific line size, if we

considerthe simation as shown, then the filar micrometer
line (or graticule) can be placed at either edge or in the
middle of this finite boundary between the measured
subjectand its two interfaces. The end result of this being
a variabledimension.To overcomethis error the operator
must makehis testingposition U'aceable
to somestandard.
i.e. cb~k a known dimensionfrom a stage micrometer
before sinng any component This e1iminAtP_~
operator
en-orby checkingto a known standard

Copyright 1994BUEHLER Ltd

6..3

J~

METAu.06RAPH'l

EUROPE

"

../

LARGER
~- - ~-~40REACCURATE
I
I

\
,)#

I
I

.4

NORMAL THICKNESS

6 ~tJREMP:NT

nRnR.~ n~

m nR)pT S~

Figure 6.6 - Angle grinding is an establishedmethod for

introducing accuracy into ~-sec1ion
measurements.
angleinsertsare suppliedenablingcomponentsto lie at a
given angle. This inclined angle dictates the increasein
sizethat can be expected. Figure 6.7 shows the expected
increasein size from 9QOwhen it is 1:I to 00 where its
increaseis infinite. The ~ful working area from this
graph is between40 degreesfrom the horizontal and IS
degrees maximum. Lower than IS degrees to the
horizontalis too sensitiveto a given error ie. 91/2- 100is a
greater error than 291/2- 300

REDUCING ERRORS

Figure 6.7 - Taper Sectioning

Another methodof achievingan angled ttacea.blesubject

which overcomessomeof the shortcomingsof the above~
givenin figure6.8.
Copyright 1994BUEHLER Ltd

6.4

J.\

METALL06RAPH'l EUROPE

Figure 6.8 - Angle Ratio

Figure 6.8 dependsupon havingtwo identicalcomponents.

one as the reference.the other. angled. It canbe seenhow
the actual thickness is derived from the three other
dimensions(A.B &; C).
The methodslisted previouslyhave all beendestructivein
that a cross-sectionof the componentis required. This ~
not always possible or desirable and therefore an
alternativemethodmustbe found.

1--"-""

l
-'-.
~'Li;" - -.(Ri':ii;

Figure 6.9 Spherical Ball Method (Plan 2:1)

Figure 6.9 illustrates the principles behind the spherical ball
method. The rotating sphere when dosed with 3J.1In
diamond will grind into and through the plated layer. This
dome shaped hole can then be optically observed and the
plated thickness calculated from knowing L. & La. The
fonnulae is shown in the sketch.

Copyright 1994BUEHLER Ltd

@4

METAU06RAPH\' EUROPE

CHAPTR 7

THE METHOD

MICROSTRUCTURAL
TRACEABwn'TO ISO9000
The idea behind microstroctural traceability is to
implementa system of operations based on referenced
standardsthatcanbe defmedand audited. Thesereference
standardswill wherepossiblebe statistical. The objectives
thereforewill be to
. Produce non-empiricallyderived surface preparation
methods.

Designatestatisticaland visual parametersfor each

.
.

stage

Define a standardprocedurewith auditing and

traceablereferences
Carry out a quality control audit

It is imponant to stress the point that it is not the 'method'

that is traceable to ISO 9000 but the manner in which the
method is caITied out. monitored and recorded. Any
surface preparation method that gives the desired result ~
acceptable.providing visual and statistical data can be used
and audited.

To developa non-empiricalmethodalong with the desired

visual and statisticaldatawill be pursued. Considerfigure
7.1

I
STR~
~

~J-mIE
,
,
Figure7.1 ProcedureConstructionI The Best of Three

Each grinding I sectioningstep has been displayed as a

triangle. the verticalaxis being the reduction in structural
damage.the horizontalbeing time. The ideal triangle or

Copyright 1994B~R

Lid

~A

METALL06RAPB"iEUROPE
step thereforewould be to have a long vertical direction
with a short horizontal. The preparationstagesas can be
seenare sectioningand sampleintegrity. the latter having
thr= groups. The principle is to select from the
'sectioningoptionsguide' thr= suitablesectioningwheels.
1bis will be followed by three suitablegrinding surfaces
from each group selected from the 'grinding/polishing
optionsguide',
The four selectedsteps chosenfor the standardmethod
have cross-hatch
uiangles. Notice how the choice in
group three takes the preparation to integrity, other
surfacesin thh group would be quicker, but without the
high degreeof integrity. In the real world it could be
necessaryto go for speed,the choice will vary with the
needs.

STATIS11CALIIlm
NOTE: The polishing Stage is not included in the
\'IsUAL PARAMTRS procedureconstructionsincethis is a supplementarystage
asandwhennecessary.
[Reference:Towards a MetallographicStandardSuitable
for ISO 9000Approval. MicrosnucturalScience- Vol 21]
The procedureconstructionrequiringvisual and Statistical
data~ shownin 7A/B~
and ~ basedon three surfaces
in each of the four groups. (one sectioning - three
grinding). The informationrequiredat the sectioningStage
ultimatelyrequiresthe time takento cut (Inins) be divick:d
by the cut length to give tan Theta. This then allows the
constructionof the trigons. From thesethree tests it will
be ~ssary to select the least damaged This surface
choicewill be noted on the sheet7A and caIried over to
7B. The threetestsin 78, which ~ the first in the sample
integrity stage,will be basedon the preferred sectioning
surfaceandall surfacesmustcommencefrom this position.
With the SOkg Hv indentit will be necessaryto note the Z
axis materialremovalnecessaryto progresseachgrinding
surfaceto its 'bestposition'. The bestposition~ whenthe
samplewill no longerimprove. Material removal (J1ID)B
then relatedto time to derivethe thetatrigon angle. Once
againthe surfacechoice~ notedand carriedover to 7C as
the 'reference'surface. The three swfacesare then Olx:e
again related to the referencesurface,the trigon created
andthe surfacechoicemade.
At the final sampleintegrity stage(7D) the new reference
swfaceis usedin againcreatingdie three1rigons.
Copyright 1994BUEln..ER Ltd

>4

METALL06RAPH'i EUROPE

Z AXlS 6RAPHlC
DISPLA""
From the twelve trigons it will now be relaJively easy to
construct the graphic display as shown in figure 7.1.
Starting from the best position (that which most closely
manifests sample integrity) and working upwards using
material removal to position each trigon. From the graphic
display a method must be constructed that satisfIes a
particular industrial requirement of cost, time and integrity
level required
STANDARD AUDIT
PROCEDURE

TRACABL
STANDARDS

The 'standard audit procedure sheets' are included in

7E/F/G/H, the information necessaryto complete such
sheets bas already been compiled in the relevant
'procedure constructionsheets'. Once the sheetshave
beencompletedan audit cantakeplace.
What has been achieved so far is:An acceptablesystem for defining a preparation method
A means of relating the chosen method to statistical and
visual standards

Providing the documentationis in the form of a closed

loop i.e. every process or check is carried out in
accordancewith the audit requirementsand is suitably
documented,then ISO 9000 requirementshave beenmet
If however d1iswork is to mean anything, it bas to be
traceable to some standard and d1is can be done as
follows:1. A SampleMaterialStandardmustbe identified

2. The 'SampleMaterial Standard'shouldbe traceableto

a traceableinstitutionor failing this an agreedindmttial
body. ~
body could be your own companyif DO
otherindustrialstandardexis~.

3. There should be traceablereferencema1eria1with

documentedlocation.

Copyright 1994B~R

Ltd

J~

METALLOOR.APH'i EUROPE

4. Additionally.thereshouldbe audit material,takenfrom

the traceablematerialthat is to be usedfor eachaudit this will alsorequirea documentedlocation.

s. The audit inlCIYll must be ~ignated

and this applies

to firstly the machine!'ter8tionparameters.that is ac~t
is made at given intervaJs to confmn the
equipment/consumable
combination has not changed
ie. If the materialremovalrequiredat a given stage~
4OJJmS
and that 10 minuteswas allocatedat this stage
thenthis rateof removalmust be confinned Secondly.
the surface prepamtion conformance must be
approved To do this the audit material will be used
alongwith the samplematerialand checkedagainstthe
audit proceduredocuments.

6.

The audit Jevel must be de~d for both "machine

operation parameters' and "surface preparation
conformance' Le. Select from the audit procedure
documentsthe minimum number of checks thought
necessary
to confIrm conformance.

7. Non-confonnance
wheneverit should occur may

requirethat a

audit takesplace.this mustbe

fuJ1

recordedin the documentation.

II Location

R&D

Audit Internal

Buehler UK

MachiDeoperatioap8P~
lb8tcb
~
---

--

I QC

- the start of eYery--

Surface preparation coaformance - First Monday or each

Audit Level

--

- :

I MadaiDe operation parameters . Check Z aD in group 1

and 2 of the sample Inte2rltv sta2e
SurfKe preparatioD confm'maDce . Check Z uIs aud
I Ytlual lafm'matiOD In group 1 aad 2.. Check Yisua1

conformance or 2r'OUP 3
NOD.Conf~
J

I Surface Pl"epantioD conformance. total check against aU

standard audit procedure laformatiou

Figure7.2 TraceableAudit Procedure

Figure7.2 is an exampleof how sucha ttaceableaudit

procedure could be consU'Ucted.

Copyright 1994SUEIn.ER Ltd

7A
PROCEDt JRECnNSTR.UCT1nNi:.~nNrNG

Oplimised machineparameters
SAMPLE mENTITY
SAMPLE

-Z-AXIS

LENGm

mETA (deg)

-'

TESTNo

WHEEL
mENTITY

SEcnO~G
~(minr

lum)

rt

ITest1

Porosity
Depth ofPorosity
InterfaceRclief
ResidualDamage
Remarks
.'.."

'.'."""

""."...'

Micrograph

%
J1ID
J1ID
J1ID
'.".""".'

MAG/NA

ITest2
Porosity
Depth
Residual
Remarks
Interface

of

Micrograph

Damage
Relief
Porosity

J.ID1
J1n\
J1n\

MAG/NA
I Test3-Depth
Porosity

-I

of Porosity

Mcrograph

..%
.~

Residual
Interface

Damage.
Rdief

...~
...~

Renwks

. ""

MAG/NA
SURFACECHOICE TEST No

~I..I

7Ba

\.

PROCEDtJRF:. CONSTRUCTTnN
PLANAR GRINDING

Optimisedmachineparameters
SAMPLE

mENTITY

RESmUAL DAMAGE

REFERENCE SURFACE No

III

soKg Hv n-mENT mEN

Surface I Measuring IInitia1

I sequence I ind~

~ 4No
Test

L~ REMOVAL

Final Material Combined Z-Axis

Indent ~ova1
Time( min ) Theta

roD0

ITest4

,I

Porosity
Depth ofPorosity""."'
InterfaceRelief.""""
ResidualDamage'

Micrograph

%
J1D1
J1D1
J1D1
"""""'.'"

Remarks

MAG/NA

ITest 5,.1
Depth
Porosity

of Porosity.

Residual

Damage..

interface

Relief

Micrograph
%
...J1n1
J1n1
J1n1

Remarks

MAG/NA
Test 6

Micrograph
Depth of Porosity
Porosity

...%
.~

Residual
Interface

Damage.
Relief

~
~

Remarks

.'.."'..'.".'...

7B2
PROCF-DI JR.:F-CONSTRUCTION

1st SAMPLE mTEGRITY STAGE

Optimiscd machineparameters

SAMPLE

mENTITY

RESmUAL DAMAGE

J!m

REFERENCE SURFACE No

'Test7

Porosity

Micrograph

OJ.

Depth ofPorosity
Interface Relief

J1!D
J1!D

Residual Damage

J1!D

,...

Remarks

MAG/NA

(Test8

Depth of Porosity

Porosity

...8f.

..JJm
JJm
JJm

Residual Damage.
Interface

Micrograph

Relief

Remarks

MAG/NA
'Tell 9-')

Porosity
Depth
Residual
Renw"ks
Interface

of

Micrograph
Damage
Porosity
Relief

,...

%
JUn
JUn
JUn

7C
PROCEDtm.E CONSTRUCTION

2nd SAMPLE DIlTEGRITY STAGE

Optimised machineparameters
SAMPLE
m ENTITY .
RESmUAL DAMAGE

J!Jn

REFERENCESURFACENo I:iA so Kg Hv n-mENTmEN LIP REMOVAL

Surface MeasuriDI
LD.
~u~

Test
No

Final
Ind=

Initial
indent

Material
Removal

Combined Z-Axis
~

Tune( min )

m
'Test 10

I
MIcrograph

Depth
Porosity
Interface
Residual
Remarks

of

Damage
Porosity
Relief

J1D1
J1D1
J1D1

MAG/NA

ITest11

Depth of Porosity
Porosity

Micrograph

...0/,
..J1nt

P~dual
Interface

Damage.
Relief

J1nt
J1n\

Remarks

MAG/NA

ITest12 .-:Depth

Porosity

of Porosity

--:3
..0/.
.JJ.In

Residual
Interface

Damage.
Rdief

...JJ.In
...1Jm

Remarks

Micrograph

7D
~nNSTRucrlnN

PROCEDUR~

FINAL SAMPLE nolTEGRITY STAGE

Optimisedmachineparameters
SAMPLE

mENm"Y

RESmUAL DAMAGE

J1ID

REFERENCE SURFACE No
-

~ T est

IS~
II.D.

No

13

Measunng

!~ence

soKgHvINDENTmEN m
-

1:

I~terial
I Removal

REMOVAL
-

Combined
T Jme(min )

Z-Axis
Theta

(JLII!!! 13

Porosity
DepthofPorosity
InterfaceRelie(
ResidualDImIIC

Micrograph

%
J1D1
J1m
J1D1

Remarks

MAGmA

'Test14
Porosity
Depth
Interface
Residual
Remarks

.'.""'

of

I
'...'

Damage
Porosity
Rdief

Micrograph

%
J1In
J1In
J1In

".

MAG/NA
I Test IS
Remarks
Residual
Porosity
Interface
Depth

of

Damage
Relief
Porosity

.,

%
J1In
J1In
J1In

7E
STANDARD At mTT PROCF;ntJRF-(From Z Axis GraphicDisplay)
SECTIONING

SAMPLE mENT1TY
FUNC110N
-

--

SECTIONn-lGWHEEL
mENTITY

AUDIT
ScRATClfPATInN

M/C

~.n.tfEiF

-PARAMETERS

ACE

~-

LUBR.ICANT

-~

I W-mUALDAMAGE- -

REMARKS .

MICROGRAPH

MAG/NA

7F2
STANDARD

AtmlTPROCEDURE

1st SAMPLE INTEGRITY STAGE

SAMPLE m ENTITY '
FUNCTION
-

IPi.ATEN
IS~A:.~

--

IM/C
PAR AMETF.RS
,

--.

ABRASIVE/
SEOUENCF.

LUBRICANT

m..m

AUDIT
-

Saatch
Pattern

POrosity
%

Material
Removal

REMARKS

MICROGRAPH

MAG/NA

7FI
STANDARD AUDIT PROCEDURE
PLANAR GRINDING

SAMPLE INDENTITY..
FUNCTI ON

I PUTEN
I

PARA .METERS

!SURFACE

ABRASIVPJ

M/C
I

SEQ~"cE

lumRICANT

Tn.(E

AUDIT
-

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S:TANDARD

AI mIT PROCEDUR.B

2nd SAMPLE OO'EGRITY STAGE

SAMPLE mENTITY
FUNCTIGN

I ABRAsrvFJ
M/C
I SEQUENCE
l_SURFACE PARAMETERS
. PLATEN

LUBRICANT

TIME

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-

Saatch
IPattem

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Porosity
Depth

Interface
Relief

Lux
Value

IF:dained
I Phases

Material
Removal

REMARKS

MICROGRAPH

OPTICAL TECHNIOUE

MAG/NA

7H
STANDARD

AUDIT PROCEDtJRE

FINAL SAMPLE INTEGRITY STAGE

SAMPLE mENTITY ..
FUNCTION

PLATEN M/C
SURFACE PARA~

ABRASIVFJ
SEOUENCE

!LUBRICANT

TnvfE

AUDIT
Scratch
Pattern

Porosity
% --

P:oio$ity
~-

Interface Lux
Value
Relief

Retained
Phases

Material
Removal

REMARKS

MJCROGRAPH

OPTICAL TECHNIOtJE

.I

MAG/NA

01\4

METAlJ.06R.APH"l EUROPE

CHAPTER6

MlCROSCoP\'AND PBOTOMlCRO6RAPn

MICROSCOPE
n'PES

The metallographerwhen analysing specimens usually

requiresa 'Macro' (low magnification-large field of view)
or a 'Micro' observation(higher magnificationsmall field
of view). Figures8.1 and8.2 areexamplesof 2 'micro'
scopes. Figure 8.1 is an 'upright' compoundmicroscope,
8.2 an 'invened' compoundmicroscope.

Figure8.1
UprightCompound
Microscope

Figure8.2
InvertedCompound
Microscope

The word 'compound' is usedto signify a double optical

imaging system. That is an objective which createsthe
primary image and the eyepiecewhich further ma~jfj~~
the primary creating a secondaryimage. If just one
magnification occurs then the microscope would be
describedas 'simple' (i.e. magnifying glass). Invened
compoundmicroscopesare often called Metallographsor
Projection microscopes. The advantageoffered by the
invenedsystemis that no specimenlevelling is necessary,
the objectjust sits on top of the microscopestage.

COPYRIGHT 1994BUEln..ER Ltd

8.1

METAu.OORAPHY UROP

Figure 8.3 - (Macro)

Figure 8.3 is an example of a Macroscope(sometimcs
called a macro-microscope,althoughthis is a misnomer).
This type of scope can be consideredas a camera lens
system with various sized projected images. It i~ a
'simple' scope in that it dependsupon a primary image
only. The most obvious example would be a 35mm
camera. The illustration in figure 8.3 shows a bellows
exten.~ionsystemwherebythe field of view can he varied.
The image being reflected via the upper mirror onto a
projectionscreenor alternativelyallowedto pa.~ upwards,
with the mirror tripped out. Once projectedupwards it
(;an ~ imagedinto th~ large format cam~rdplane. Both
cameraplane and projection screenarc par-focal (at IhL'
sameimagedistance).
St\."r\."osrupicmicr()sco~S (figure 8.4) are unlikl..'any 'If tht.'
flrevious example.1\m that they have a d()uhl\.' ()flti..: OL,j.'.
Thl..' angle of thc.~ two separate image.' i.'i d\.'~ignl..'dt"
I..'mula~ thc avcragc J'Crsons intcrocular di.'\tant.'1..'
wh\.'n
viewing an object at the least distance of distint.'t vi~i()n (II)
inchl.'~). It is becauseof these two separate rdY.'ithat wc
fl\."rcciv\.'the imagc in three dimensions (st\."re().'iCoflic).
MICROSCOPE IMAGE

1111.'
micm~co~ is u~d basically becau~ thc ~uh.ic~tWL'
wi",h to ()hservc i~ .waller than the human I.'ycc.:anrl.'~"v~.
In ordL'r to ~c thi~ .wall ohject we havt.' to magnify an
imagl.' of tht.' ohjl.'ct that is within the vi"ihlL' limit, ()f thl:
~y~.

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MT:Au.06RAPH\'EUROPE

Figure8.5Man's limit of Resolution

Figure 8.5 is used to illustrate the limit of mans vision
when observing an object at the least distance of distinct
vision (10"). This limit as shown is IOOJ.1In.
We therefore
needto magnifyany objectless than IOOJ.1In
in order to see
and resolve. For example a sOJ.1In
object would have to be
X2 magnified in order for the eye to see.

Figure8.6 illustratessomeof the important elementsand

positionsof the compoundmicroscope. Four conjugate
planesare shown; the lens principle focus, objective back
focal plane, primary image plane and secondaryimage
plane. Notice how the mechanicaltube length is fIXed.the
optical tube length will vary with different lens
configurations(objectives). Figure 8.6 depicts a finite

J~

METAlJ.06RAPH"l EUROPE
optical systemof l6Omm mbe lengdL ~
dimension
changeswith metallurgicalmicroscopesto a higher value
in order to accommodatethe reflected light illuminator.
Objectivesmust be correctedfor the operatingmbe length
and shouldnot be usedat other mbe lengths(objectivesof
numericalaperturegreaterthan 0.25 will manifestcloudy.
images).
The alternativeto finite tube length systemsis to have an
infinite systemincorporatingparallelrays along part of the
optic axis. This systemis n.o.1
superiorto a finite system.
It is however, more convenientwhen a combination of
different ~~~~ries are to be used. Once again the
microscopeobjectiveshave to be speciallycorrected for
this infinite tube length and must not be used with other
objectives.

BRI6HT FIELD
MICROSCOPE
TE. C HNl Q US

The most commonmicroscopetechniqueis that of bright

field. The micr~pe beingset for what is called KOhler
illumination, this is shown in Figure 8.7

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Light illuminatedfrom the lamp filamenttravels along the

illwnination axisincidentto a semi-reflectingmirror. Light
reflectedfrom the mirror passesthroughthe objective and
is focused onto the object An image of the object ~

COPYRIGHr 1994BUEHLERLtd

8.4

1IT:ALL06
RAPH"i
EUROPE
imageplane. The eyepiecefurther m~
this imageto
give a secondaryimagefor observationor photographing.
To satisfy KOhler illl1m;ftArionthe lamp filament must be
imaged in the objective back focal plane. the field
diaphragmin the object planeand the apermrediaphragm
~ in the objectivebackf<x:a1
plane.
Microscopeaccessoriesshownin the sketch are filter and
polariserI analyser.
The specimenwhen observedin bright field very often
requiressomeform of chemicaletching in order to reveal
micros1ructUIaldetail
Dart Ground(Dark Field}

(8)

(bt

Figure 8.8. Light Intesity Comparison

(a) Scratched
(b) Etched

Figure8.8 give an indicationof the light intesity difference

between a scratch and an etched grain boundary.
Brightfield showsvery little differencebetweenthe scratch
- the etchedboundaryhoweveris dramatic. Dark ground
on the other band shows an excellent contrast difference
between background and scratched surface.
To
understandthe principlesof dark ground your attention ~
drawnto figure 8.9.

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METAlJ..06RAPH"l EUROPE

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Figure 8.9 Dark Ground illumination

Ught illuminated from the lamp filament is projected
towards the incident semi-reflecting mirror. The central
portion of this light is blanked off by the means of the
darkground illumination stop, thus allowing an annular ring
of light to pass and be reflected into the optic axis. This
annular ring of light has an inside diameter greater than the
objective field of view. The light then passesthrough what
is called a 'catoptric' condenser system which focuses the
illwnination onto the object plane as shown.

It follows therefore that only light that is 'deflected' by the

specimen will re-enter the optical path, light that has ~n
reflected will be reflected out of the optical path. A
polished surface with for example a scratch would manifest
a black background, the scratch being the only illuminated
item.
Dark ground fin~ many applications, the following just a
few oftbe examples:. Improved contrast
Featuremorphology highlighted
Material translucencyidentifIed
Sub-surfacedamageidentified
Sub-surfaceporosity

.
.
.
.

(Examples of d1is and all other optical technique

applicationsis coveredby the series'Exploiting the Optical
Microscope'by the author.)
COPYRIGHf 1994BUEIn.ER Ltd

8.6

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1IT:AIJ..o6
RAPH'iEUROPE

POLARlSIN6

The bright field microscopeshown in figure 8.7 can be

usedfor simplepolarisingtechniques.The polarisercould
be in positionfor most applicationsjust to reduceglare in
the optical system. Once the analyseris introduced a
conditioncalledcross-polarscanbe achieved.This is when
the vibration ~tion
of the polariser is at 90 to the
analyser.The result beingall light is extinguishedi.e. light
reflectingfrom the specimenis totally extinguished. If the
analyseror polariserbe slightly rotated (1 - 3) then the
low intensitysubjectimagewill re-appear. This condition
is refenedto asun-crossedpolars.
To put this techniqueto use we needto understandwhat
happenswhen light is ilK:ident to a subject material.
Materialsnmmallyreflect light, incidentupon the prepared
surface,in a vibration direction identical to the incident
entry vibrationdirection.Materialsthat do not re-orientate
the incident ray vibration direction are said to be
'isotropic'. Metalsfor exampleareisotropic. Considerthe
bright field microscopeas shownin figure 8.7 with the
polariser in position and a steel specimenplaced in the
optic axis. Light when passingthrough the polariserwill
extinguishall but one vibration ~tion
(North/South).
This specificvibration (NS) will be reflectedoff the steel
samplewithout any noticeabledifference. If the analyser
be now placed in the optic axis and set to East/West
(crossed-polars)
thenall light will be extinguished
Somematerialssuchas mineralsreact differentlyto metals
in that when light is incident to the preparedsurfacethe
reflected image emerges in tWo specific vibration
directions,thesematerialsaresaidto be 'anistropic'.
Consider now an anistropic material being used as the
specimen. Polarisedlight vibrating in one direction will
upon reflectionbe now vibratingin two directionsat 90.
to eachother. When thesetwo directionsfail to coincide
with the analyservibration direction. an imageis created.
This can best be illustrated by using a cast nodular iron
sampleas the specimen. Betweencross-polarsthe iron
will be extinguishedbut the graphite (anistropic) will be
excited and imaged against this black extinguished
background. To convert d1is grey level image into the
most beautiful coloured structure it will be necessaryto
placeafterthe polariseran accessorycalleda 'sensitivetint

plate' (sometimes
calleda first order red plate). This
ac~-~corywhenplacedas suggestedchangesthe black
COPYRIGHr 1994BUEIR..ERLtd

8.7

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METAlJ..O6RAPH"l
EUROPE

extinguishedbackgroundto that of the 1st order red. (540

DIn).die anistropicgraphitenow a multitude of colours.
The preparationof thin sectionsbas been covered in this
manual, the microscope required to observe these thin
sectionsrequires to be illuminatedwith traDSmittedlight
A schematiclayout of a 1st order polarising transmitted
light microscopeis shownin figure 8.10

Figure 8.10 - Po1arisingMicroscope - Transmitted Light

Consider the light emanatingfrom the illuminator at the

bottom (as shown). This light incident to the optic axis ~
vibrating in all directions until it passes through the
polarlser. A single vibration direction when passing
through the anistropic material emergesin two vibration
directions,ultimately to passthrough the analyser. These
two rayswill, whenrecombinedin the primary imageplane,
interfere to create the image. (Constructively or
destructively).

COPYRIGHr 1994 B~R

Ltd

8.8

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METAUO6RAPH"i EUROPE

(
OIFFERNTlA L
INTERFERENCE
CONTRAST (OIC)

Differential interferen~ contrast can with a correctly

preparedspecimenprove to be the most revealingof any of
the optical techniques.Providing the abrasivedifferential
betweendifferentmaterialphasesbasbeenrestricted to the
equivalentdepth(or less)as the objectiveresolution then a
threedimensionalimagecanbe ~ved.
This subjecthas
receivedextensivecoveragein the 'Exploiting the Optical
Mi~ope'
series.also in the book 'Surface Preparation
and Microscopy of Materials'. The schematiclayout in
figure 8.11illustratesthe opticalcomponentsnecessary.

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Figure 8.11 DifferentialInterferenceConstrast- Refelcted

Light
Basicallywhatwe haveis the standardbright field reflected
light microscopewith the addition of a polariser/analyser
and a beamsplitter often called a Normaski prism (named
after the inventor). From figure 8.11 the polars are
crossed,the prism slowly introduced Wltil the 1st order
grey extinctionpositionis achieved
DIC dependsupon the interferenceof the ordinary and
extra-ordinaryray whenre-combined.To havea perfectly
planar or steppedcomponentthe optical path difference

COPYRIGHT1994BUEIn.ERLtd

J.\
(

METALLO6RAPH"iEUROPE
(OPD) betweenthe two rays would be identical,resulting
in a backgroundcolour remaining unchangedinespective
of the planar or stepped surface. 1bankfu1ly all
mec}\~~-11yworked surfacesresult in slopes,rather than
steps,as one phaseis abradeddifferently to another. It ~
this slope that creates an OPD between the two rays
resultingin a colour change. ie. planarsurfaceswould all.
inespective of height be one colour - all sloped surfaces
would be anothercolour relatedto the angleof slope. This
is illustratedin figure 8.12

0 .~Ray
EX=~Ray

Figure 8.12 - Identification by Slope

CAMERA PLANE
PHOTOMlCR06RAPHY Camerascan be placedanywhereafter the secondaryimage
plane.they do tend howeverto be placedat what appears
to be an wmecessarilylong distanceawayfrom the camera
eyepiece(C.F.PL lens)asshownin figure 8.13

COPYRIGHT 1994BUEln..ER Ltd

8.10

J~

METALL06R.APH"l UROPE

F-]

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Figure 8.13 - Photomicrographic System

This long distanceis in fact a repeatof the original object

to imageconjugatedistance. This is done to give a unity
position where the quality of the secondary image ~
reproduced. Any other position could re-image optical
abeIrations designed out of the conjugate plane. If
therefore a single lens reflex camera was to be used it
would haveto be fitted with a 'long robe' adaptor.

QuALm' OFMICR06RAPHS
The quality of picttJreSdepends.in the main. on the care
taken in the surface preparation, the chosen optical
technique and observanceof some well defined rules.
Very rarely if ever should the microscopebe blamedfor
indifferentresults.
FILM
The choice of fiJm in generaltenus is to target for the
lowest ASA (speed)fiJm ming the largest format. This
siwation obviously dependsupon different circumstances
the authorwho alwaysusedKodak 5 x 4 cut film now uses
Fuji Velvia 50 ASA (ISO) transparencies.becauseof the
prioritiesof lectures.
COPYRIGHT 1994BUEIn..ER Ltd

8.11

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METALLO6.RAPH"/
EUROPE

~I
Fim~~
(UE

- underexposure;

OE overexposure)

Figure8.14FJlmOJaracteristics
Figure 8.14 showshow the low ASA (ISO) film with im
excellentrangeof densitymaximum/minimum
has inflicted
a high angleexposurecurvewith its narrow latitudeto
exposureerrors. The high ASA beingmuch lesssensitive.
very fast but could be lackingin contrast
Fn..TERS
Filters play an imponantrole in both balancingreciprocity
and contrasting both coloured and black and white
subjects.
Table 36.2 Guide to CC mien

~ure
1/8
1
5
10
30

time(s)

F1Itas

New film speed Setting

CC2OC +CC3OB

ISO 25/150

CC30B
CC20M+CCIOB
CC20M
CCIOM+CCIOR.

ISO 2S/lSO

ISO 20/140
ISO 16/1~
ISO 16/130

Figure 8.1SGuide to CC FDters

Figure 8.15 give an indication of the necessity to
supplement the illumination with different colour
correction filters as the exposuretime necessarybecomes
longer. Reciprocityfailme is when the intensity/exposme
curve proves no longer arithmetical.i.e. under or over
exposed. The materialograpberwill in the main be
underexposingand as can be seen from figure 8.15 the
addition of CC2OC + CC30B will be necessarywhen
8.12

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METAJ.J..06RAPH\'
UROPE
exposingat 1/8 secondin order to achievea faithful colour
reproduction. (Ibis assumesthe colour temperaturesof
the lamp andfilm arecompatible).
If the light intensity emanatingfrom the specimenwas so
low as to incur a 30 second exposure, then colour
correction filters of CCIOM + CCIOR would have to be
employed.
Fn..TERS CONTRAST
Yellow 8bsorbs blue CC20Y
Red absotbs

bkIe and green CC20R

Magenta absorbs green CC20M

Blue absorbs red and green CC20B

Cyan absOfbs red CC20C

Green absorbs bkle and red CC2OG

Figure8.16 ComplementaryColours
Filters can be introduced to complement a particular
coloured feature. Thesecomplementaryfilters are shown
in figure 8.16. It is important to reaIisethat filters are not
entirely confined to colour photography,they also have a
role to play in black andwhite.
One of the most enjoyable aspects of being a
materialographeris the ~hnicaIly revealing picblres that
canbe capturedwhencarefully using the microscope.

8.13

SECTION 1:

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Identify materialcharacteristics
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