16

Chapter 2
SURVEY OF LITERATURE
In order to assess the trend and level of research work done till date, in the area of
titled work, an exhaustive literature has been reviewed. A gist of some of the most relevant
research work is presented in this chapter under various classified headings.
2.1 Fatigue
Fatigue refers to the structural damage, which results from repeated or otherwise
varying stresses that are well below the static yield strength of the material. Fatigue
involves the initiation and growth of a crack, or growth from a pre-existing defect, which
progresses until a critical size is reached. As per ASTM E-1823 [57], the term fatigue is
defined as, The process of progressive localized permanent structural change occurring in
a material subjected to conditions that produce fluctuating stresses and strains at some point
or points and that may culminate in cracks or complete fracture after a sufficient number of
fluctuations.
2.1.1 Historical perspective
The work on fatigue goes back to 1837, when Wilhelm Albert established a
correlation between applied loads and durability in the context of chains used in mines [58].
Around 1839, Jean-Victor Poncelet, who designed cast iron axles for mill wheels, described
metals being tired in his lectures at the military school at Metz [58]. These lectures were
never published, but have been quoted in the works of many eminent authors [59]. Poncelet
also made the first official reference to the term fatigue [1] in his French book titled,
Introduction a la Mcanique Industrielle, (Introduction to Industrial Mechanics). The
phenomenon of fatigue was widely observed in 17
th
century during the failure of railway
structures that claimed many lives, as reported by Gray [60] and Smith [61]. Rankine [62]
17


investigated the fatigue failure of railway axles and suggested that the axles should be
forged with a hub of enlarged diameter and large radii, so as to reduce the cutting of grain-
flows during machining, which would improve the fatigue life of axles.
The first organized research on fatigue, concerning failure of railway axles, was
carried out by German engineer August Whler in 1860s. Besides developing the S-N
curve, Whler also fabricated apparatus for repeated loading of axles [63]. An extensively
cited piece of his work published in German, is titled, Versuche zur Ermittlung der auf die
Eisenbahnwagen Achsen einwirkenden Krfte und die Widerstandsfhigkeit der Wagen-
Achsen, (Tests to determine the forces acting on railway car axles and the resistance of
car-axles). Whler was also the first to arrive at the modern terms of fatigue life and
scatter in the context of design for fatigue life [1].
Subsequent to the initial work cited above, scientists and engineers in the
industrialized countries started working on morphological and material aspects of fatigue.
Batson and Bradley [64] undertook an organized research on fatigue of laminated springs,
which were subjected to different heat treatments as well as various surface finising
operations. Thum and coworkers did initial research on the role of stress concentration on
fatigue by investigating fatigue behaviour of shafts having rapidly varying cross-sections
[65-67]. Almen [68] did pioneerg work on the effect of surface modification on endurance
limit. Based on the data obtained by Whler, Basquin [69] represented the finite life region
of the fatigue curve in the form of stress vs number of load cycles on a double-log scale.
Later on, laboratory fatigue tests were performed by many researchers, notably Haigh
[70], Gough and Pollard [71] and Gough [72]. A well-known damage accumulation
hypothesis, commonly known as Palmgren-Miner rule, was developed by Palmgren [73]
and Miner [74]. Investigations by Tavernelli and Coffin [75], Coffin [76] and Manson [77]
led to the development of well-known Coffin-Mansion law of damage accumulation in low-
cycle fatigue, which was later extended by Manson himself [78], as well as subsequent
researchers, notably Brechet et al. [79]. The low cycle fatigue analysis has been
18


successfully applied to structures subjected to small number of fatigue cycles during their
lifetime, viz. electrical equipment subjected to thermal stresses. Around the same time,
Neumann [80-82] developed the slip-plane model of crack initiation, while Schijve and
Brock [83] investigated the factors affecting crack propagation in aircraft structures, which
were subjected to variable amplitude or gust-spectrum loading. Subsequently, Schijve
developed detailed model of fatigue crack growth and published a series of lectures on the
topic [84-87]. The developments during twentieth century are comprehensively covered in
a review article by Schijve [88].
Subsequent researchers further extended the concepts developed by pioneers, as
mentioned above. The prominent names among them include Brechet et al. [79] for
extension of Coffin-Manson law, Toth and Krasowsky [89] for damage process analysis on
the basis of Paris law and Coffin-Manson equation, Todinov [90] for work on Palmgren-
Miner rule, and Shodja and Kamalzare [91] for their work on Griffith-Inglis model of crack
growth.
The organized study of fatigue, beginning with the historical work of Whler on
railway axles, has come a long way to the safe life fatigue resistant design of modern
aircrafts. However, the problem of fatigue still continues to cause catastrophic failures and
claim lives wherever material properties or service loads deviate from the design values.
2.1.2 Fatigue of metallic materials
Microscopic investigations have revealed that the nucleation of fatigue cracks occurs
at a very early stage of fatigue life. Cheng and Laird [92] demonstrated that the microcracks
commence in the form of slip bands within a grain. The cyclic slip occurs as a result of
cyclic shear stress. On a micro-scale, this shear stress is not distributed uniformly, but
varies from grain to grain, depending on its size and shape, crystallographic orientation and
associated elastic anisotropy of the material. The slip occurring on surface grains leads to
formation of slip steps, as revealed in the study of Villechaise et al. [93] on 316L austenitic
stainless steel. In the presence of oxygen, the freshly exposed surface of the material in slip
19


steps gets oxidized, which prevents slip reversal. The slip reversal in this case occurs in
some adjacent slip plane, thereby leading to formation of extrusions or intrusions on the
surface of material, as observed by Gross [94] and Terentev [95] and depicted
schematically in Figure 2.1.
The fatigue life is generally divided into three stages: Stage-I or crack initiation stage,
Stage-II or crack growth stage and Stage-III, which involves rapid crack growth till final
fracture [Refer Figure 2.2]. Stage-I usually comprises maximum portion of fatigue life of
the component.

Figure 2.1: Formation of intrusion and extrusion marks on the material surface.

During crack initiation, fatigue is essentially a surface phenomenon. In this period,
the growth of crack is slow and erratic owing to its interaction with the grain boundaries.
However, a more regular growth of crack occurs afterwards. The periods of crack initiation
and growth are distinct from each other in many ways, viz. while the surface conditions do
affect the initiation period, they do not have much influence on the crack growth period.
Stress concentration factor is an important parameter during the crack initiation phase,
while the stress intensity factor is important for predictions of crack growth [96].
20


Figure 2.2: Phases of fatigue life

The difference between microcracks observed during the initiation period and
macrocracks developed during the propagation period is that while the former grow along
the plane of maximum shear, the growth of macrocracks occurs along the plane of
maximum tensile stress. However, although the crack propagates along the plane of
maximum tensile stress, the crack tip exhibits shear as well as tensile opening
displacements [97]. The cyclic opening of the crack tip leads to the formation of fatigue
striations [Refer Figure 2.3]. According to Davidson and Lankford [98], the cyclic crack
growth may equal the striation spacing at higher crack growth rates, while it may be much
less for slower growth. Grinberg [99] observed that regardless of the material, the minimum
striation spacing observed remains around 0.1m.
During Stage-III of fatigue crack growth, the striation-forming mode is gradually
replaced by the static fracture modes, viz. rupture or cleavage. Since stages I and II
comprise service life of a component subjected to fatigue, most of the research work has
been dedicated to the study of these modes. For a steadily propagating stage II fatigue
crack, the Paris relation [100,101] of crack growth rate can be applied:
m
K C
dN
da
) ( =

Equation 2.1

where a is the crack length, N the cycle number, K is the stress intensity factor, C and m
are constants. A value of da/dN =1 represents formation of striation in each loading cycle.
Berkovitz [102] extended this hypothesis in the opposite sense to develop a technique for
estimating the loads from the observations of fractured surfaces. The technique was further
developed by Ruckert et al. [103].
21



Figure 2.3: Mechanism of fatigue crack propagation

Elber [104,105] introduced the concept of crack closure, according to which, when
the fatigue crack is loaded in tension, there will be Poisson contraction in the transverse
(through-thickness) direction. During unloading of the crack tip, this sucked-in material will
lead to establishment of contact between the two crack surfaces before complete unloading,
thereby resulting in compressive stress in the vicinity of crack tip, over the region of
premature contact. These compressive stresses have to be first overcome for the crack to
propagate further in the next loading cycle. The effective range of the tensile cycle is thus
the range between the opening load and the maximum load of the cycle. Different
researchers have further developed the concept of crack closure. Notable among them are
the experimental and numerical studies carried out by Blom and Holm [106] and the finite
element study by Chermahini et al. [107].
22


2.2 Design of fatigue test experiments
Different investigators have proposed different designs of fatigue tests in order to
meet the intended engineering and research objectives. While the engineering objectives
involve determination of fatigue properties of materials or structural elements, the research
objectives are usually concerned with determination of influence of one or more variable
factors, viz. composition, processing parameters, environment, load spectra etc., on the
resulting fatigue properties.
2.2.1 Fatigue tests
The design of fatigue tests depends on the following parameters:
Type of test: Stress based or strain based.
Type of loading: Tensile, torsional or bending.
Type of fatigue test piece: Actual components or standard specimens.
Nature of load cycle: Constant amplitude (CA), variable amplitude (VA) or
service simulation spectrum.
Environmental conditions: Temperature, humidity, presence of corrosives etc.
The choice of various parameters for a given application is based on the underlying
objective behind the fatigue tests. The stress-based tests are useful for situations involving
high cycle fatigue, where loading is confined to elastic stresses and associated strains.
However, plastic strains may exist in the vicinity of stress raisers, such as notches or holes,
even when bulk of the component is subjected to elastic loading. As proposed by Lee et al.
[108], such situations are better analyzed through strain-based tests, which take into account
local strains as the governing fatigue parameters.
In their study on constant and variable amplitude fatigue loading of standard
aluminum alloy specimens, Schijve et al. [109] state that the CA stress tests are generally
used for obtaining material-specific information pertaining to fatigue performance, while
23


VA loading is helpful in providing information on crack closure. However, in case of
critical assemblies, viz. aircraft structures, testing of actual components subjected to actual
or simulated service load spectra is indispensable for ascertaining their fatigue performance.
The nominal stress (S) for a given fatigue loading (tensile or shear) is given by:
A
P
S = (For axial load P)
J
Tr
S = (For torsional load T)
I
Mc
S = (For bending moment M)




Equation 2.2
where A is the area of cross section, J is the polar moment of inertia, r is the distance from
the centre of cross section to the point of interest, I is the moment of area about neutral axis,
and c is the distance of the fibre from the neutral axis.
Since the loading in case of rotating bending fatigue tests on round specimens closely
resembles actual components such as axles, these tests have been extensively applied since
the early phase of fatigue research [110].
2.2.2 Test specimens and loading conditions
Each one of the basic types of fatigue tests requires a test specimen having specific
geometry, as shown in Figure 2.4. The test specimens can either be notched or unnotched.
Notched specimens are supposed to be representative of the real life structures and contain
stress raisers in the form of holes or notches with well-defined geometry. On the other
hand, as opined by Schijve [96], the fatigue data for unnotched specimens is considered to
be representative of the materials fatigue properties, but does not provide information
regarding notch sensitivity of the material.
24


As the fatigue behaviour of unnotched specimens depends largely on the surface
conditions, the tests on these specimens in various states can be used for making a
comparative study of the effect of different surface treatments, viz. nitriding, carburizing
etc., on the resulting fatigue performance.

Figure 2.4: Various types of fatigue test specimens

As stated earlier in section 2.2.1, the rotating bending fatigue tests are most
commonly employed for assessing fatigue properties of the materials. These tests can be
further classified on the basis of the type of load applied, viz. single point, two-point or
four-point. The first one employs a cylindrical, toroidal or tapered cantilever specimen,
while the remaining two tests employ cylindrical or toroidal beam type specimens of the
form prescribed in IS:5075 [111], as shown in Figure 2.5.
In case of materials exhibiting high hysteresis losses during straining, excessive
heating may result in considerable rise in temperature of the test piece, thereby leading to
inconsistent fatigue life data. Accordingly, toroidal shaped specimens are used for fatigue
testing, so that relatively smaller volume of the specimen material is subjected to maximum
stresses. ISO1143 standard [112] recommends that wherever possible, the shape which
subjects the largest volume of material to maximum stress should be preferred, while a
liberal allowance is kept on the portion of specimen meant for holding purpose.
25



Figure 2.5: (a), (b) and (c): Cylindrical fatigue test specimens under single, 2-point and 4-
point bending respectively; (d), (e) and (f): Toroidal fatigue test specimens in single, 2-
point and 4-point bending respectively.

In case of single point loading, as shown in Figure 2.5 (a) and (d), the cantilever beam
specimen is also subjected to shear stress, while in case of two or four point loading, the
neck portion of the specimen does not have any shear stress and is subjected to pure and
uniform bending moment. When four point bending is applied to cylindrical specimens,
Figure 2.5 (c), it subjects the largest volume of material to maximum stress, which is
desirable according to ISO1143 standard [112].
2.3 Collection, analysis and presentation of fatigue data
The stress cycle during fatigue tests is characterized by stress amplitude (S
a
), mean
stress component (S
m
) and wave shape of the stress cycle. The stress ratio (R=S
min
/S
max
) is
1 for completely reversed rotating bending fatigue test.
The wave-shapes resembling actual loading conditions will provide more realistic
estimates of the fatigue performance of components during a real-life fatigue loading, but
the laboratory fatigue tests, aimed at determining materials fatigue properties, are generally
performed under simple load cycles, viz. the wave-shape of stress cycle for a rotating
bending test is a sine wave.
26


In order to generate realistic data for fatigue analysis, the fatigue tests are carried out
on several specimens at different levels of maximum alternating stresses. The fatigue data is
plotted on a semi-log or log-log scale in the form of S-N curve (i.e. stress vs. number of
cycles to failure curve), also known as Whler curve. The portion of curve with negative
slope constitutes the finite life region and represents fatigue strength of the material for a
given number of stress cycles, while the horizontal portion represents infinite life region.
The stress level corresponding to horizontal portion (i.e. infinite life) is known as fatigue
limit of the material. The changeover point, or the knee, signifies the phenomenon where
crack nucleation is essentially arrested by some microstructural features, as suggested by
McGreevy et al. [113] and Murakami and Nagata [114]. A typical log-log S-N curve is
mathematically expressed by the following relation proposed by Basquin [69]:
b
f f a
N S S ) 2 ( ' =
Equation 2.3
where S
a
is the stress amplitude, N
f
is the number of cycles to failure, b is the fatigue
strength exponent and
f
S' is the fatigue strength coefficient.
2.3.1 Analysis and determination of finite life
Owing to inherent microstructural inhomogeneity in the material properties,
differences in surface finish and test conditions, the fatigue data exhibits scatter, as
mentioned by Troschenko [115] and Rodopoulos and Chilveros [116]. The variance of log
life generally increases with decreasing stress levels, particularly for unnotched specimens.
This makes it necessary to take into account the statistical nature of the fatigue data, as
suggested originally by Weibull [117,118].
The objective of this section is to provide statistical background for constructing a
median S-N curve and associated lower and upper bound curves, that characterize the
minimum and the maximum fatigue lives (i.e. stress cycles) at a given level of fatigue
strength (i.e. stress amplitude), so that the majority of fatigue data falls within these lower
and upper bound curves. In this regard, various techniques have been prescribed in the
27


literature [119-122]. Out of these, the techniques provided in JSME [119] and ASTM [121]
standards are widely used by researchers for obtaining S-N curves and making fatigue life
predictions. These techniques are briefly described in the following sub-sections.
2.3.1.1 JSME S 002 standard
The median S-N test method, as described in JSME standard, involves testing of 2
fatigue specimens at 4 stress levels for finite life region, while 6 specimens are used for
determining the fatigue limit through staircase method. The recommended test sequence is
shown in Figure 2.6, where the numbers next to the data points represent the order for
conducting the fatigue tests. The fatigue limit is determined by taking the average of the
stress levels employed during the staircase test. The details of staircase method are
described in section 2.3.2.4.

Figure 2.6: S-N testing according to JSME standard
2.3.1.2 ASTM E739 standard
The guidelines for generation of statistical S-N curve are provided in ASTM E 739
standard [121]. In order to assess the variability and statistical distribution of fatigue life,
28


the standard recommends replication of fatigue tests, i.e. testing more than one specimen at
each stress level. The percentage replication (PR) depends on the size of test batch (k) and
number of stress levels (L) used during fatigue testing, and can be determined from the
following relationship:
PR = 100(1-L/k) Equation 2.4

The guidelines recommend employing 6-12 specimens for preliminary, research and
development tests and 12-24 specimens for design allowable and reliability tests. The
recommendations regarding percentage replication for various tests are as follows:
17 33% for preliminary and exploratory work
33 50% for research and development tests
50 75% for design allowable data tests
75 88% for reliability data tests
Once the requisite fatigue data has been collected, statistical analysis prescribed in
ASTM E739 standard can be applied. The analysis assumes that the fatigue life at a given
amplitude of stress follows log-normal distribution and the variance of log-life is constant
within the test range. The resulting regression model of fatigue is expressed as:
Y = A + BX + ,
where, Y = log N
f
, X is the maximum alternating stress and is a random variable
representing error.
The linear regression model of fatigue is given by:
X B A Y

+ =
Equation 2.5
where the over-bar () symbol signifies average values and the caret (^) symbol represents
estimated values, obtained by minimizing the sum of squares of deviations of the observed
values of Y from its predicted values, i.e.,
29


2
1 1
2 2
)

( )

(
i
k
i
i
k
i
i i
X B A Y Y Y = =

= =

Equating the partial derivatives of
2
with respect to the estimators A

and B

to zero,
we get:
0 ) 1 )(

( 2

1
2
= =

=
k
i
i i
X B A Y
A
and
0 ) )(

( 2

1
2
= =

=
k
i
i i i
X X B A Y
B

Therefore, the least squares method gives the estimators A

and B

as:

=
=

=
k
i
i
k
i
i i
X X
Y Y X X
B
1
2
1
) (
) )( (

X B Y A

=
Equation 2.6
The variance, which is assumed to be constant within the range of X
i
, can be
estimated as follows:

=
k
i
i
Y Y
k
1
2 2
)

(
) 2 (
1


Equation 2.7
Taking logarithm of both sides of the Whler relation (Equation 2.3), we get:
) log(
1
) ' log(
1
) 2 log(
a f f
S
b
S
b
N + =

Equation 2.8

Comparing this equation with the regression Equation 2.5, we get:
X=log(S
a
), Y=log(2N
f
), ) ' log(
1

f
S
b
A = and
b
B
1

=

Equation 2.9
In other words, the fatigue strength exponent (b) is inverse of the linear regression
constant B

, while the fatigue strength coefficient

)

(
'
A b
f
e S

= . The coefficient of variation
of
f
S' , defined as the ratio of standard deviation to mean, is calculated as:
30


1
) (
'
2 2
=
b
S
e C
f

The double-sided confidence band for the entire median S-N curve can be computed
from the following equation:
2 / 1
1
2
2
) (
) ( 1
2

(
(
(
(

+ +

=
k
i
i
i
p
X X
X X
k
F X B A



Equation 2.10

where F
p
is taken from statistical tables abstracted in ASTM E 739 [121]. The plots of these
confidence bands take hyperbolic form, as shown in Figure 2.7. The confidence band will
become narrowest when

=

k
i
i
X X
1
2
) ( is maximum. This is possible if the fatigue tests are
conducted at the farthest possible points, i.e., at the extreme stress levels of S-N curve,
provided the linearity of S-N curve is already ascertained.

Figure 2.7: S-N data along with ASTM regression fit and confidence bands.
2.3.2 Analysis and determination of infinite life
Just as observed for the finite life regime, the endurance limit too exhibits scatter. The
objective of this section is to provide statistical analysis for estimating the endurance limit
at a specific high cycle fatigue life. Depending upon the availability of time, number of test
31


specimens and the accuracy required, any one of the methods, as described in the following
sub-sections can be employed for estimating the endurance limit.
2.3.2.1 Estimation of endurance limit from material properties
This method provides a technique, developed by various researchers, notably
Bannantine et al. [123], Dowling [124] and Stephens et al. [125], for estimating the
endurance limit on the basis of limited information, viz. ultimate strength, hardness and
available S-N data for various materials. The strength value thus obtained is modified to
account for other factors, such as loading, surface finish, size and desired reliability on S-N
curve.
2.3.2.2 Step test
As discussed in the preceding sections, due to statistical nature of fatigue, it usually
becomes necessary to test many specimens at stress levels in the vicinity of fatigue limit.
However, it is possible to make an approximate determination of fatigue limit by
employing very small number of specimens, if one adopts the step-test method. The method
is also useful for estimating the fatigue limit in situations where only one specimen of its
kind is available, as suggested by Bellows et al. [126]. In this method, a specimen is tested
for a large number of cycles (~10
7
) at a stress amplitude S
a0
, slightly lower than the
expected value of endurance limit. If the specimen does not undergo fatigue failure after
completion of stipulated number of cycles, S
a0
may be considered to be slightly below the
endurance limit. The test is then repeated for the stipulated number of cycles, by
successively increasing the stress amplitude by small amount S
a
each time, till failure
occurs. The endurance limit (S
f
) is then considered to be between (S
a
- S
a
) and S
a
; where
S
a
is the final stress amplitude at which fatigue failure occurred. The method is graphically
represented in Figure 2.8.
32


Figure 2.8: Step test for approximating the fatigue limit using a single specimen.

2.3.2.3 Probit method
The Probit method is described in ASTM Special Technical Publication 91-A [127].
In this method, a number of specimens are tested at various stress levels in the vicinity of
endurance limit. For the specimens, which do not fail, the test is stopped at some high value
of N (say, 10
7
cycles), which is to be associated with the endurance limit. In this way, the
percentage of failed specimens is recorded at various stress amplitudes and thus, provides
the estimated probability of failure at that particular stress amplitude. These probabilities
are then plotted on a probability graph, as shown in Figure 2.9, so as to obtain the
distribution function of the endurance limit associated with N = 10
7
cycles. The mean value
of endurance limit is taken against a 50% probability of failure, while the standard deviation
is calculated from the slope of the probability graph.


33



Figure 2.9: Probit method for determining the endurance limit.

2.3.2.4 Staircase method
The staircase method provides an estimate of the endurance limit by taking into
account its statistical nature. Also known as the up-and-down method, it has been adopted
and prescribed by many standards, viz. JSME [119] and British Standard [128], for
assessing the statistical properties of endurance limit.
In this test method, first of all, the mean endurance limit is estimated. Following this,
a specimen is tested at stress amplitude S
a
slightly (~5%) higher than the expected
endurance limit. If the specimen fails before completion of stipulated number of cycles, say
210
6
, then the next specimen is tested at lower stress amplitude. However, in the event of
survival of a specimen, the test is suspended after completion of stipulated number of
cycles and the next specimen is tested at higher amplitude of maximum alternating stress.
Thus, the stress amplitude of each successive test is based on the outcome of its previous
test. The graphical representation of the method is given in Figure 2.10.

34


Figure 2.10: Staircase method for determining endurance limit.

The statistical parameters of the test results can be obtained either by Dixon-Mood
[129] or Zhang-Kececioglu [130] techniques. The Dixon-Mood method is based on the
maximum likelihood estimation and assumes that the normal distribution curve best fit the
data pertaining to endurance limit. The Zhang-Kececioglu [130] analysis is based on either
the maximum likelihood estimation or the suspended-items analysis method. The method
can also be applied to staircase tests with variable stress-steps.
The Dixon-Mood method on the other hand, requires uniform stress-steps in the
staircase. This method is widely used as it is easy to apply and provides good estimate of
the endurance limit [131], with slight bias towards conservative side. It assumes that the
data pertaining to endurance limit has normal distribution. This method provides formulae
for estimating the mean (
s
) and standard deviation (
s
) of the endurance limit (S
e
). The
mean and standard deviation are estimated by using the data of less frequent event out of
the two possible events, i.e. survivals or failures. The individual stress amplitudes (S
i
),
which are spaced uniformly at an interval of d, are numbered as i, where i=0 is used to
35


denote the lowest stress amplitude, (S
o
). The stress increment (d) should be in the range of
S
S
d

2
2
. The estimate of mean endurance limit is given by:
|
|
.
|

\
|
+ + =

2
1
,i DM
DM
O S
n
A
d S , if survival is the less frequent event


Equation 2.11

|
|
.
|

\
|
+ =

2
1
,i DM
DM
O S
n
A
d S , if failure is the less frequent event


Equation 2.12


Here, ( )( )

=
i DM DM
n i A
,
, while
i DM
n
,
is the count of less frequent event
corresponding to the i
th
stress amplitude.
The standard deviation is estimated from either of the following two expressions:
( )
|
|
.
|

\
|
+

029 . 0 62 . 1
2
,
2
,
i DM
DM i DM DM
S
n
A n B
d

Equation 2.13
if
( )
3 . 0
2
,
2
,

i DM
DM i DM DM
n
A n B

or
d
S
53 . 0 = Equation 2.14
if
( )
3 . 0
2
,
2
,
<

i DM
DM i DM DM
n
A n B

where ( )( )

=
i DM DM
n i B
,
2

Once the values of mean and standard deviation are known, the one-sided confidence
levels (lower bounds) for the endurance limit can be determined by the expression:
S s C R e
K S =
, ,
Equation 2.15
where K is the factor for one-side tolerance limit for normal distribution, which can be
obtained from the works of Lieberman [132] or Link [133]. The lower bound endurance
36


limit (
C R e
S
, ,
) signifies that with a confidence level of C%, R% of the tested fatigue limit
would be expected to exceed the stress amplitude
C R e
S
, ,
.
2.4 Effect of surface modification on fatigue
A number of researchers have investigated the influence of various types of surface
modification processes on the fatigue behaviour of substrate material. Bruzzone et al. [134],
in their paper concerning state-of-the-art in surface engineering, have discussed in detail the
properties of functional surfaces, their applications and the technologies available to
engineer these surfaces. They have observed an expansion in the importance as well as
application of engineered surfaces to new domains. These developments are attributed to
the greater knowledge of the phenomena occurring on the engineered surfaces as well as the
availability of affordable technologies for mass production of engineered surfaces.
As described earlier in section 1.2, the surface modification processes can be broadly
classified into two categories. The first category involves modification of the material
properties upto a certain depth, as in case of heat treatment processes such as case
carburizing or nitriding etc. The second category involves application of various types of
coatings on the substrate surface. Following sub-sections present the literature pertaining to
the effect of both types of surface modification processes on the resulting properties,
particularly fatigue.
2.4.1 Effect of heat treatment
A variety of heat treatment processes have been developed for various grades of
steels. Since the response of steels to heat treatment is governed largely by the percentage
of carbon present in it, therefore the selection of process, viz. physical or chemical heat
treatment, depends primarily on content of carbon in steel. For most of the low carbon alloy
steels that find widespread application in machine tool and automotive industries, the heat
37


treatment processes like nitriding, carburizing or a combination thereof are widely
employed for achieving the desired properties of hardness and strength.
Although nitriding is possible on many grades of steels, but very high hardness is
obtained in certain special grades of steels that contain nitride forming elements, viz.
aluminium, chromium, molybdenum or vanadium, which help in maintaining a high
concentration of nitrides near the surface and prevent their diffusion further deep into the
core. Thus, while nitriding of case achieves higher hardness in comparison to case
carburization, the depth of nitrided case is less. Nitriding is also known to cause substantial
improvement in fatigue performance, as reported by many researchers, viz. Czerwiec and
coworkers [135,136], Suh et al. [137] and Ashrafizadeh [138]. However, owing to the
associated shape distortions, the use of nitriding is generally restricted to tribological
applications [139].
Case carburization is the most common surface modification technique and finds
widespread application as it leads to tremendous improvement in mechanical properties of
hardness, strength and endurance [140,141].
While high hardness of martensitic case is important from wear resistance standpoint,
the enhancement in fatigue properties is attributed mainly to the presence of residual
compressive stresses within the carburized case. In his historical work on case carburized
steels, Ebert [142] correlated these residual stresses, induced during carburization process,
to the time lag in the occurrence of martensitic transformations in the layers at various
depths, which have different carbon concentration. The work by Krauss [143] shows that
the factors responsible for this favourable shift in properties root from the martensitic
transformations taking place during the course of heat treatment process. Bag et al. [144], in
their study on dual phase steels, found that the maximum fracture toughness is obtained for
steels having martensitic volume fraction in the range of 0.7 to 0.8.
Yang et al. [145] in their study involving case carburized 20CrMnTi specimens, have
reported the shift in residual stress field resulting from case carburization process. The
38


study revealed that in the non-carburized quenched specimen, the residual stress is tensile at
the surface and compressive in the center, however, in carburized specimen, it is observed
to be compressive in the surface zone. The authors also proposed a simulation model, which
accounts for percentage of carbon and calculates the residual stress resulting from
martensitic transformation.
Since the magnitude of residual stresses in steel components is dependent on the
substrate microstructure, viz. percentage of retained austenite, the same can be modified
through some suitable processing, viz. cold treatment, as employed by Surberg et al. [146]
and Stratton and Graf [147], so as to reduce the amount of retained austenite. The resulting
change in the stress field has been worked out by Bensely and coworkers in different
studies [148,149]. They investigated the distribution of residual stress in case carburized
EN353 steel subjected to cryogenic treatment prior to tempering and observed an increase
in the compressive residual stress for the specimens subjected to cryogenic treatment.
In his work on bending fatigue strength of carburizing SS2506 steel, Preston [150]
reported that the fatigue performance is largely dependent on the presence of residual
compressive stresses in the surface layer. It was reported that as the case depth is increased,
the magnitude of compressive stresses in the outermost layers gets reduced, thereby
increasing the chances of surface crack initiation. Genel and Demirkol [151] further
extended the work to investigate the effect of case depth on fatigue behaviour of case
carburized SAE8620 steel specimens. They reported an optimal relative case depth, which
results in best performance under fatigue loading.
In their study on fatigue of carburized steels, Farfan et al. [152] reported a general
trend of improvement in endurance limit with increasing depth of case. In another similar
work, Asi et al. [153] divided their standard fatigue test specimens into three batches and
subjected them to a different type of heat treatment by varying the parameters such as
carburizing temperature, carburizing time and holding time at 850C. The study reveals that
the higher depth of case leads to greater depth of surface oxidation, which in-turn enhances
39


the non-martensitic transformations, thereby adversely affecting the distribution of residual
stresses and leading to a lower fatigue life. In another study [154], they reported
degradation in fatigue performance with increasing carburization temperature, owing to
unfavorable distribution of residual stresses within the carburized case. Woods et al. [155]
suggest that a favourable modification in stress field can be utilized for enhancing the
performance of machine elements, such as gears, which are subjected to bending fatigue
during their normal operation.
For certain grades of alloy steels, which contain higher percentages of oxide forming
elements, such as manganese and chromium, internal oxidation can occur, which is often
accompanied by the formation of high temperature transformation products (HTTP) viz.
pearlite, upper and lower bainite up to a certain depth below the surface [156]. For steels
containing silicon, manganese and chromium as major alloying elements, oxides of
chromium are generally formed in the outermost layers in the form of precipitates within
the grains. This is followed by oxides of manganese, which form at some depth below the
surface and may appear either in the form of precipitates or as grain boundary oxides. The
oxides of silicon penetrate to maximum depths, generally in the form of grain boundary
oxides [157,158]. The oxidation potentials of major alloying elements, as presented by
Kozlovskii et al. [159], are shown in Figure 2.11.
As a consequence of internal oxidation, non-martensitic microstructures are likely to
form within the alloy-depleted regions in the vicinity of oxides, thereby resulting in loss of
hardness, even though the microhardness tests performed on the outer surface may not
reveal such phenomenon. Further, the high temperature transformation products are usually
the first to undergo transformation and their coefficient of thermal expansion is also less
than that of the surrounding material. As a result, these products are likely to come under
compression when the component cools down to room temperature. Owing to differential
contraction during cooling, the residual compressive stresses in the carburized layer get
compromised. This reduction in residual compressive stress in turn can lead to deterioration
of fatigue performance, as reported by Arkhipov et al. [160] in their work involving fatigue
40


testing of case carburized gears. In his comparative study on fatigue performance of
20MnCr5 and 15CrNi5 steels, Brugger [161] observed that the fatigue limits of these steels
were substantially different at 680 and 780 MPa respectively in the absence of HTTPs, but
dropped in the range of 520 to 540 MPa for both the steels when similar amounts of HTTPs
were present in the surface layer. Naito et al. [162] in their work on SCM415 steel, also
reported a negative influence of internal oxidation and HTTP on the resulting fatigue
performance. Besides, they also observed the phenomenon of double-knee formation in the
fatigue curve in the presence of HTTP.


Figure 2.11: Oxidation potentials of alloying elements and iron in steel, heated in
endothermic gaseous environment.
2.4.2 Effect of surface coating
Coating materials of various types and deposited by different means onto various
substrates have been extensively used in the cutting-tool, aerospace and automotive
applications for enhancing specific properties of a given component, such as resistance to
corrosion, heat and wear. Corrosion resistance has traditionally been achieved by means of
41


nickel or chrome plating. However, owing to the environmental concerns associated with
this process, application of physical vapour deposition is on the rise.
The resistance to heat is usually achieved through the application of thermal barrier
coatings (TBCs) [163]. These coatings are usually applied by means of EB-PVD process,
as explained in section 1.4.4.4. The state-of-the-art in thermal barrier coatings is described
in the review by Schulz et al. [164].
Over the course of last couple of decades, the application of hard coatings for
enhancing tribological properties has become very popular in the cutting tool industry. In
this context, TiN is one of the most well-established coating, which gained widespread
popularity for its excellent tribological properties [165].
Besides TiN, coatings based on amorphous carbon [166] or diamond-like carbon
(DLC) [167] have also been developed and successfully applied. A number of researchers
have evaluated the properties as well as performance of these coatings. Gupta and Bhushan
[168] and Bouzakis et al. [169] evaluated mechanical properties, Wellman et al. [170]
investigated hardness and Sundararajan and Bhushan [171], Precht et al. [172] and Shum et
al. [173] evaluated tribological behaviour of these coatings.
Since fatigue is an important performance parameter and is closely linked to the
prevalent state of material at the surface of a component, a number of researchers have
studied the effect of coatings on the resulting fatigue properties. The influence of some
conventionally applied as well as recently developed coatings on the substrate properties,
with particular reference to fatigue, is being discussed in the following sub-sections.
2.4.2.1 Electroplating
Chrome plating is the most commonly eletrodeposited coating, known for its
corrosion and wear resistance, along with low coefficient of friction. However,
environmental and mechanical problems concerning chrome plating are resulting in
research aiming to identify alternative baths [16,17], remedial treatments [174,175] as well
42


as economically viable alternatives [176]. An important characteristic of chrome plating is
the presence of high tensile residual stresses, which are detrimental for fatigue performance
of the chromium plated components [177-179].
2.4.2.2 Thermal spray coatings
With a view to offset the detrimental effects of chromium plating on the environment
as well as components fatigue properties, Nascimento and coworkers [180,181] have
proposed the application of thermal spray coatings as a viable alternative [182]. Thermal
spray coatings are deposited by processes such as detonation gun, High Velocity Oxy-Fuel
(HVOF) arc etc. Coatings applied by means of HVOF technique possess high mass density,
good adhesion, good mechanical strength and improved fatigue properties of the coated
components.
An early study correlating the residual stress with fatigue life of thermal sprayed steel
and aluminium substrates was conducted by McGrann et al. [183]. In their extensively cited
study, the authors have established a positive correlation between the observed fatigue life
and the magnitude of residual compressive stresses present within the coating. The authors
have observed a ten-fold improvement in fatigue life as a result of WC-Co thermal spray
coating as compared to conventional or accelerated chrome plating. The authors have
attributed this enhancement to the presence of residual compressive stresses induced during
thermal spray process.
In another study involving WC-Co thermal spray coating, Ahmed and Hadfield [184]
conducted rolling contact fatigue tests and identified four modes of failure, viz. abrasive,
delamination, bulk deformation and spalling. The delamination failure is stated to be the
most catastrophic mode of failure. The study also confirmed the presence of protective
residual compressive stresses within the coating.
43


2.4.2.3 Chemical vapour deposition
The CVD process overcomes many of the shortcomings of thermal spray process, as a
result of which, the CVD coated components exhibit enhanced tribological performance
[185,186]. However, CVD process can also cause surface embrittlement, thereby leading to
detrimental effect on mechanical properties [187].
The effect of CVD coatings on fatigue performance is also detrimental. During
rotating bending tests of PE-CVD coated specimens, Baragetti and Tordini [188] have
reported a small decrease in fatigue limit. Schlund et al. [189] have also observed a decline
in fatigue properties of CVD coated specimens, which could be overcome by applying a
combination of PVD and CVD coatings [190].
2.4.2.4 Physical vapour deposition
The physical vapour deposition (PVD) process offers numerous advantages over the
older processes such as electroplating or thermal spray coating. It has led to the
development of a number of commercially and technologically successful tribological
coatings, such as TiN, TiCN, TiAlN, TiZrN, DLC, TiC etc., which have found widespread
application in the cutting tool industry [191].
The influence of PVD coatings on fatigue behaviour of the substrate is also governed
by factors similar to those discussed for thermal spray coatings. In their investigation on the
high temperature fatigue performance of TiAlN coatings applied to 1Cr-1Mo-0.25V steels,
Suh et al. [192] conclude that the fatigue performance is associated mainly to the presence
of residual compressive stresses in the coating. Ferreira et al. [193], in their study involving
fatigue behaviour of 42CrMo4 steel coated with W, WN, WTi and WTiN deposits,
observed a general trend showing improvement in fatigue performance at lower levels of
maximum alternating stresses. The gain in fatigue performance is attributed to the presence
of residual compressive stresses within the coating. At higher stresses, cracks get initiated at
places where flaws exist within the coating and then find their way into the bulk substrate.
Similar observations have been reported by Su and co-workers [10,11] for TiN PVD
44


coatings, where fatigue properties were found to be adversely affected below 510
5
cycles,
but observed to improve beyond this point.
Puchi-Cabrera et al. [194] conducted rotating bending fatigue tests on the substrate
coated with a PVD film of TiCN and observed 140 180% gain in fatigue life, which is
attributed to compressive residual stresses and good adhesion of the deposit to the substrate.
Similar findings have been reported by Berros-Ortiz et al. [195,196] and Puchi-Cabrera et
al. [197] in their works on fatigue behaviour of AISI 316L stainless steel coated with: (i)
different TiN
x
[195,197] and (ii) ZrN
y
[196] understoichiometric films deposited by
unbalanced close field magnetron sputtering (UCFMS) process and (iii) TiN films
deposited by plasma assisted PVD (PAPVD) tehnique. The studies reported an
improvement in fatigue life of the coated specimens in comparison to their uncoated
counterparts.
Baragetti et al. [198] investigated the influence of CrN PVD coating on fatigue
behaviour of 2205 duplex stainless steel substrate, subjected to four-point bending. The
study also investigated the effect of substrate preparation processes (rolling, polishing and
shot peening) on surface residual stress as well as fatigue properties. The investigation
revealed an enhancement in the fatigue life of the coated specimens, which is attributed to
the presence of compressive surface residual stress field induced by PVD coatings. In
another work [199] regarding the influence of CrN PVD coatings on fatigue behaviour of
steel substrate, a 15% improvement in endurance limit was reported by the same authors.
They were also successful in developing FEM model for the problem. However, in their
study on Plasma Enhanced Chemical Vapour Deposition (PECVD) coatings, Baragetti and
Tordini [188] reported a slight reduction in endurance limit.
Multilayer coatings of various compositions have also been developed by various
researchers. The chief advantage of multilayer coatings over single layer coatings lies in
that they can be better customized to accomplish the desired properties. In their work
involving multilayer metallic coatings on copper substrates, Stoudt et al. [200] observed
45


improvement in fatigue properties due to retardation of fatigue crack initiation. They
hypothesized that the fatigue properties can be enhanced by depositing an ideal surface
layer, which possesses the desired properties of hardness, toughness, cyclic work
hardenability, residual compressive stresses and good adherence. However, higher cost
associated with multilayer coatings is a major prohibitive factor in their application.
A recent addition to the class of PVD coatings is the WC/C coating [50], described
earlier in section 1.4.4.4. The microstructural and mechanical properties of these coatings
have been reported by Carvalho and DeHosson [201] and Park et al. [202]. It is reported
that the amorphous phase dominates in the layers of carbon as well as WC. By varying the
concentration of WC particles and correlating the resulting electrical conductivity with
mechanical properties, Park et al. [202] showed that the physical contact between the
carbide particles is an important structural factor that governs the physical properties of the
nanocomposite films. The hardness as well as residual compressive stresses within the film
were found to increase only at higher concentrations of WC phase, which was attributed to
physical contact between the WC particles present within the matrix of amorphous carbon.
The applicability of WC/C coating on machine elements appears to be justified for a
number of supporting reasons. First, the range of processing temperatures for this coating
renders it suitable for heat-sensitive machine elements, viz. heat treated steels. Secondly,
the coating possesses compressive stresses as well as good tribological properties that are
often required in tandem for the machine elements such as gears, which are subjected to
wear as well as fatigue during their service life. The favourable effect of WC/C coating on
the performance of gear-pairs working under loss of lubrication condition has been
demonstrated by Murakawa et al. [203]. The tribological performance of WC/C coatings
depends on the hardness of WC particles and the lubricating properties of amorphous
carbon matrix. The effect of this coating on the fatigue properties has been reported in a
study by Baragetti et al. [204] concerning 2011-T6 aluminium alloy coated with PVD
WC/C, PA-CVD DLC and PE-CVD SiO
x
. The authors conducted rotating bending fatigue
tests and reported an improvement in fatigue limit of WC/C coated specimens. The
46


observed improvement was attributed to the presence of residual compressive stresses in the
coating, apart from its excellent adhesion to the substrate surface.
In a recent study concerning application of WC/C coating on gears made of case
carburized steel, Fujii et al. [205] made comparative tests on three types of pinions, labeled
as: NT (case carburized, uncoated), WT (case carburized and WC/C coated) and ST (case
carburized and WC/C coated, with an interlayer of CrN). The authors reported better
fatigue performance for WT pinion than the NT pinion, under a maximum hertzian
pressure, p
max
= 1700 MPa. The WT pinion exhibited poor performance in comparison to
NT pinion at p
max
> 1900 MPa, which was attributed to peeling of the coated layer. The
peeling was found to occur at relatively lower loads for the ST pinion. The authors
concluded that the occurrence of peeling in the coated layer is the dominant factor affecting
surface durability of WC/C coated gears.
2.5 Residual stress and its estimation
It is revealed from the literature that hardness and adhesion of the coated deposit
alone play a dominant role in determining tribological properties of the coated components,
such as cutting tools and gears, but the influence of coating on fatigue properties of the
coated substrate is a more complex function of various factors, viz. (a) properties of
coating, (b) surface and bulk properties of the substrate, (c) influence of coating process on
the substrates properties, (d) distribution of residual stresses in the coating and substrate
and (e) adhesion of coating to the substrate. The last two parameters are actually inter-
related in the sense that the adhesion of deposit is affected by the presence of residual
stresses in the coating/substrate system.
In their article concerning interactions between residual stress and crack growth,
Fitzpatrick and Edwards [206] point that though residual stress plays a major role in
determining the fatigue behaviour of a component, but the growing crack can in-turn affect
the residual stress field at the crack tip. They observed that in order to know the influence
of stress field on crack propagation, the exact effect at the crack tip should be estimated
47


through some suitable model. However, the approach has limited validity due to the
changes imminent in the residual stress field once the crack begins to grow.
The inter-relation between residual stress and integrity of PVD coatings has been
described in two different studies by Teixeira [207,208]. The author has analyzed the stress-
induced cracking in thin PVD coatings, originating from the presence of residual stresses
and has also presented a numerical model to estimate the distribution of residual stress
within a layered metal-ceramic composite coating.
Thus, it is evident that for a given composition and properties of material in the
surface layer, magnitude of residual stresses plays an important role in determining the
mechanical properties, especially fatigue of a heat treated or coated material. In view of
this, it is extremely important to measure residual stresses within the component for
predicting its fatigue behaviour.
As stress is an extrinsic property of the material, it cannot be measured directly, but is
rather estimated indirectly by measuring some other physical quantity, viz. velocity of
sound in the material, which in turn is affected by the presence of stress. The residual
stresses can be divided into two categories micro-stresses and macro-stresses. Micro-
stresses are those stresses, whose range is on the order of the microstructure, viz. crystallites
or grains. Macro-stresses, on the other hand, cast their influence over ranges, which extend
far beyond the dimensions of grains.
2.5.1 Methods for residual stress measurement
A number of destructive and non-destructive methods have been developed for
estimation of residual stresses [209]. While mechanical test methods, such as hole drilling
[210] or curvature measurements on thin strips [211] can estimate the magnitude of macro-
stresses, the diffraction techniques, viz. X-ray and neutron diffraction, can provide an
estimate of both the micro as well as macro-stresses. Besides, diffraction methods being
non-destructive in nature, can be applied to any number of components, whether freshly
48


manufactured, in service, or failed. In case of large components that cannot be
accommodated in X-ray diffraction equipment, or where stresses are to be determined in
layers that are well below the surface where X-rays cannot penetrate, it becomes necessary
to either cut a section of material from an appropriately selected location, or remove surface
layers either mechanically or chemically. In such situations, the method obviously
becomes destructive. However, owing to the importance of non-destructive testing, portable
X-ray diffraction equipment for residual stress measurement has also been developed and
successfully employed in industry to address the problems associated with accommodation
of large components inside the equipment [212]. Besides XRD, some other non-destructive
methods for residual stress measurement have also been developed, viz. ultrasonic
techniques [213-215], micro-magnetic measurements [216,217]) etc.
2.5.2 X-ray diffraction residual stress measurement
Among the various non-destructive methods of residual stress estimation, X-ray
diffraction is a well-developed and widely applied technique [218-223]. X-ray diffraction
method for estimation of residual stress involves the measurement of strain within the
crystal lattice, which is used to estimate the residual stress causing the observed strain. The
presence of micro-strains, such as those resulting from plastic deformation processes like
cold-working etc., affects the lattice spacing within individual grains in a random manner,
thereby leading to broadening of diffraction lines.
On the other hand, presence of macro-strains systematically alters the spacing
between a particular set of lattice planes as a function of their orientation with respect to the
direction of macro-stress [Refer Figure 2.12]. This in-turn causes a shift in the
corresponding diffraction peak. The strain along the normal to reflecting planes varies with
the angle between the normals to lattice planes and the surface normal. As a result, there
are two slightly different diffraction angles, 2
1
and 2
2
corresponding to the lattice planes
having normals N
1
and N
2
on the lower and higher sides of the detector respectively. The
resulting Debye ring from the specimen no longer remains perfectly circular, but becomes
49


slightly distorted, so that the radii S
1
and S
2
are no longer equal. The measurement of radii
S
1
and S
2
at various values of tilt angle () provides an estimate of the strain and hence
corresponding stress.

Figure 2.12: Diffraction from a set of hkl planes for residual stress measurement.
The estimation of strains and corresponding stresses requires application of classical
continuum mechanics. The technique is based on the Reuss or Voigt linear elastic distortion
models for the crystal lattice [224,225]. The Reuss model assumes stress to be
homogeneous throughout the polycrystal, as a consequence of which, the strain distribution
becomes heterogeneous. Voigt model, on the other hand, is based on homogeneous strain
distribution and associated heterogeneous stress distribution.
2.5.2.1 Relationship between stress and strain
If a cylindrical bar of initial diameter D, is loaded axially to induce uniaxial stress
y

acting along the y-direction, the corresponding strain,
y
, in the y-direction is given by:
50


E
y
y

=

Equation 2.16
where E is the Youngs modulus. If the Poissons ratio of material of the bar is , the
corresponding strains in the x and z directions, for the material assumed to be isotropic,
would be given by:
y z x
= =
Equation 2.17

The measurement of
y
by X-ray diffraction is not practically feasible since it would
require recording the diffraction pattern of planes which are normal to the axis of the bar.
On the other hand, measurements of strain are made normal to the cylindrical surface, i.e. in
the x or z-direction, (or any combination thereof if the direction is not important and the
material is isotropic) and are given by:
0
0
d
d d
n
z x

= =

Equation 2.18
where d
n
is the spacing of hkl planes, whose normal is perpendicular to the surface of the
bar, and d
0
is the value of spacing for undeformed lattice.
The longitudinal strain
y
and hence the corresponding stress
y
can thus be deduced
from the treatment given in Appendix A.
For such a measurement, only a set of selected grains, whose hkl planes are parallel
(within the range of angle of divergence of the incident beam) to the specimen surface, will
contribute to the diffraction cone. For these hkl planes, which are oriented parallel to the
specimen surface, the inter-planar spacing is reduced as a result of Poissions ratio.
However, for the grains whose hkl planes are oriented normal to the specimen axis, this
spacing between the planes would be extended. In other words, the spacing d
hkl
is a function
of crystal orientation with respect to the direction of macro-strain [Refer Figure 2.12].
One basic problem with steels is that there does not exist any standard value of lattice
constant d
0
against which the lattice strain can be measured. One alternative for determining
51


the value of d
0
is to make measurements on a small, stress-free portion cut from the
specimen, but it will make the method destructive. Another method is to use calibration
against known values of stress (hence strain) on identical specimens, but this may not
always be practical. A practical workaround for this problem is that uniaxial internal strain
can be estimated by comparing the diffraction patterns obtained from the same location on
specimen at different tilt angles () [Refer Figure 2.12], typically =0 and at some higher
value, viz. =45. The relationship between stress and strain on a free surface is developed
in Appendix A.
In practice, it is usually desired to determine stress

[Refer Figure 2.13] in a given

direction of interest (on the specimen surface), where the Greek alphabet represents the
azimuth angle between

and the direction of principal stress

11
. This can be achieved by
recording two diffraction patterns: one for hkl planes whose normal is parallel to the surface
normal and the other for hkl planes whose normal is at an angle with the surface normal.
The corresponding measured strains are termed as
33
and

. The X-ray diffraction

technique thus involves working with three coordinate systems: crystallite coordinate
system (K
i
), equipment or laboratory coordinate system (L
i
) and specimen coordinate
system (S
i
).
The diffraction peaks are obtained according to the orientation of lattice planes hkl
within the volume of material contributing towards diffraction pattern. The coordinates K
i

for these planes of the crystallite should satisfy Braggs relation with the equipment or
laboratory coordinates L
i
in order to obtain a diffraction peak. Further, since the Braggs
relationship between these coordinate systems is only a function of hkl and wavelength of
X-rays, so it is completely independent of the specimen coordinate system, S
i
.
Thus, stress and strain referred to in the preceding discussion refer to the crystallite or
laboratory frame of reference. But in actual practice, it is required to determine their values
in relation to the specimens frame of reference, viz. with respect to direction of rolling etc.
52


This can be achieved through the application of suitable transformation matrices [Refer
Appendix B], which lead to the following result:
( ) { }
{ } { }

2 sin cos cos
1
1
sin 2 sin sin cos
1
'
23 13 33 22 11
33
2
12 33
2
22
2
11 33
+
+
+ + +
+
+ + +
+
=
E E
E E


Equation 2.19
where the prime superscript denotes strain in the specimen coordinate system.

Figure 2.13: Relationship between equipment coordinate system, principal stresses and
stress to be measured,

.
2.5.2.2 Determination of biaxial residual stresses from diffraction peaks
Following the treatment given in Appendix C, Equation 2.19 provides the relationship
between biaxial residual stress at the free surface, in terms of lattice-spacings corresponding
to various -tilts. The Equation C.5 derived in Appendix C is reproduced below:
( )

E
d
d
+
=

1
sin
1
2
0


Equation 2.20
53


If the values of d
0
, E and are known,

can be obtained by measuring d

at two
values of . However, as stated earlier, determination of d
0
is a problem in itself, especially
for materials containing alloying elements, such as alloy steel. So, for practical purposes, d
0

is taken as equal to d
0
which is nothing but d corresponding to = 0.
The factor E/(1+) in the above equation is known as effective elastic parameter or
E
eff
and it relates the macroscopic stress to the strain measured along a particular
crystallographic direction in a polycrystalline material. Where required, the value of this
parameter can be determined with the help of a calibrating specimen according to the
procedure outlined in ASTM E 1426 [226].
If multiple values of d

are recorded and plotted against sin

2
, a more accurate value
of

can be obtained. If an isotropic material is subjected to plane stress condition, the (d

vs sin
2
) graph would be in the form of a straight line, as shown in Figure 2.14a. A positive
slope of the graph indicates tensile stresses, while the negative slope implies compressive
nature of residual stresses.
It should, however, be noted that since X-rays can penetrate to a considerable depth
below the free surface, triaxial stress states might also be encountered in certain cases,
under the influence of which, different lattice spacings would be observed for positive and
negative values of , as explained by Skrzypek and Baczmanksi [227]. Such a case is
known as -splitting, as shown in Figure 2.14b. The plot shown in Figure 2.14c indicates
the presence of crystallographic texture in the material, as described by Cullity [220] and
Prevey [221].
Since the Reuss and Voigt models are based on the assumption of isotropic character
of material, the presence of texturing, which leads to anisotropy, would adversely affect the
accuracy with which residual stresses can be determined [225]. Presence of strong texturing
may also lead to low intensities of diffracted beams and thus, further increase the
uncertainties in estimated values of residual stress. Such problems can, however, be
overcome through some suitable treatments. For example, Kapoor et al. [228] have
54


developed an approach for determining the stress tensor in textured material, while Smith et
al. [229] have presented an analysis for obtaining complete multi-axial residual stress
distribution from limited measurements.

Figure 2.14: Various forms of d vs sin
2
plots; (a): Under uniaxial or biaxial stresses in
isotropic material, (b):Under triaxial stresses and (c): For textured material.
When residual stress measurements are to be made on thin films, specialized
techniques have to be employed, viz. grazing-incidence diffraction technique [227,230],
micro-area diffraction [231] or Debye ring analysis [232].
2.5.2.3 Diffraction peak location
According to Lonsdale [233], the reliability of residual stress estimation is closely
related to the precision and accuracy with which peak-positions of the X-ray diffraction
pattern are determined; along with the applicability of the linear model that relates peak
shift to the specimen orientation. A number of factors influence the accuracy of this
measurement, as discussed briefly in the following text.
The first consideration is related to the source of X-rays, as the transition metal targets
(viz. copper) used in the X-ray tubes produce white radiation, along with the characteristic
radiation of K
1
, K
2
and K. While the wavelength of K is sufficiently different to
facilitate its filtering-out (by using -filters), the separation between K
1
and K
2
is too
small and hence, the K doublet contributes towards formation of diffraction peaks, which
in case of broad peaks would remain unresolved. Further, peak broadening is a common
55


phenomenon among the most hardened and fine-grained steels, as reported by Pineault et
al. [234]. Thus, the estimation of residual stresses in heat treated steels would involve
locating the peak-positions for unresolved pairs of diffraction peaks.
The modern day, position-sensitive detectors make is possible to record diffracted
intensity at various locations spanning the diffraction peak. While sharp diffraction peaks
can be located rather easily using low precision data, broad peaks, on the other hand,
mandate the collection of large number of X-rays at each location, thereby increasing the
time required for stress measurement. Subsequent to recording, the data pertaining to
intensities at various locations is corrected for polarization, absorption and sloping variation
in background radiation by assuming a linear variation beneath the peak. Once the raw data
has been refined, the next step involves determination of peak position. An old method,
proposed by Koistinen [235] and recommended in SAE literature, involves calculating the
vertex of parabola defined by three points confined to the top 15% of the peak.
With the refinement in resolution of position detectors to the tune of 0.01, it is now
possible to record a reasonably large number of points within close proximity of the peak,
to which a parabola can be fitted by least squares regression. This method provides better
location of the peak position. The fitted parabola provides the best estimate of peak position
in case of symmetrical peaks. However, its accuracy gets compromised in certain situations,
viz. when beam is defocused as a result of tilting, or where the doublet is not fully
combined or in case of asymmetrical peaks [236]. Prevey [237] recommends that for such
situations, fitting Pearson VII functions separately to the K
1
and K
2
peaks provides the
best estimate of peak location. Such corrections can be conveniently applied with the help
of computer programs or spreadsheet software, such as Microsoft Excel [238].
For the intensity of data recorded at high angular resolution, the peak position can
also be calculated as the centroid of the area above the background. This area-integration
method is independent of the peak shape, but is extremely sensitive to the precision with
which the tails of the diffraction peak can be determined.
56


2.6 Fracture toughness and its estimation
Fracture toughness signifies the ability of a material to resist fracture when a crack is
present. It describes the intensification of applied stress at the tip of a crack of known size
and shape at the onset of rapid crack propagation. The fractured surfaces of carburized
steels failed under bending fatigue are known to consist of well-defined stages of (i) crack
initiation, (ii) stable crack propagation and (iii) unstable crack propagation. In the high
carbon case of carburized steels, crack initiation usually occurs through intergranular
cracking at prior austenitic grain boundaries [239]. This occurs as soon as the applied stress
at the surface exceeds the sum of surface compressive residual stresses and the cohesive
strength at the prior austenitic grain boundaries. The crack thus initiated usually progresses
as stable transgranular crack for a few hundred micrometers, till it reaches a critical size.
The size and shape of stable transgranular crack propagation region is a function of fracture
toughness (K
IC
) of the material. Beyond a critical size, the crack begins to progress in
unstable intergranular mode, which continues upto low carbon portion of the case,
whereupon cleavage-like ductile fracture becomes the dominant mode.
Though the sites of initiation and stable crack propagation are often too small and
difficult to find, but they do provide information regarding fracture toughness of the
material. The fracture toughness can be estimated from the relationship put forth by Hyde et
al. [240]:
Q
a
K
a
IC
2 . 1
=


Equation 2.21
65 . 1
2
2
2
464 . 1 1 and,
212 . 0 where,
|
.
|

\
|
+ =
|
|
.
|

\
|
=
c
a
Q
ys
a

Here, a and c are depth and width of the stable crack propagation region,
ys
is the
yield strength of material and
a
is the amplitude of stress at which the given specimen
failed under fatigue.
57


2.7 Problem formulation
The literature consulted so far reveals that the application of numerous thin hard
coatings to cutting tools is a reliable solution for improving efficiency and productivity in
high demand applications. However, except for cutting tools, as far as machine elements are
concerned, the application of coatings is limited to very few components, viz. components
of fuel injection system [241]. Though, many well-established surface engineering methods
have found widespread application in the automotive sector, owing to performance
improvement [242], but the full potential of thin hard coatings in improving performance is
far from being realized.
The literature concerning application of coatings on automotive components is rather
scant, but nevertheless provides an insight regarding their potential towards performance
enhancement [243,244]. The influence of coatings on many potential automotive
components such as piston rings, bearings and gears has still not been explored. The
foremost advantages of thin coatings are their excellent friction and wear behaviour, which
are of great importance for coated parts exposed to intense as well as varying normal and
tangential loads.
Besides friction and wear, the critical parameter to be taken into account during the
selection of an appropriate coating-substrate combination for a specific application is the
effect of coating on fatigue strength and endurance limit of the component. The research
available on fatigue behaviour of coatings is rather scarce in terms of their application to
machine elements (viz. gears, cams, shafts etc.), which are subjected to various standard
processes, such as heat-treatment, prior to their application involving fatigue loading.
Therefore, it is important to investigate the effect of coatings on fatigue behaviour of
materials, which are used for manufacturing such machine elements.
Further, the research in this area is also motivated by environmental concerns
associated with the manufacturing sector. These concerns are addressed in terms of
enhanced service life of the components as well as through replacement of environment-
58


damaging materials and processes such as chrome and cadmium plating with the eco-
friendly process such as PVD. Besides, the PVD process induces residual compressive
stresses within the surface layer, which can lead to better fatigue performance as compared
to electroplated components, which possess tensile residual stresses within the electroplated
layer. In their study concerning EB-PVD coatings, Reinhold et al. [245] point out that PVD
is the most promising coating process and its use is increasing gradually.
The case-carburizing alloy steels are extensively used in automobile industry for
manufacturing machine elements viz. cams, gears, shafts etc. [246-248]. In addition to
increasing surface hardness, the case-carburizing process also imparts residual compressive
stresses on the surface [249-251], which contribute towards enhanced fatigue performance
of the component [252]. However, these residual stresses as well as surface hardness are
compromised to some extent during the subsequent tempering process [246]. A surface
coating deposited through the PVD process, in addition to enhancing tribological
properties, also imparts compressive residual stresses [253] and therefore may be employed
to further enhance the fatigue life of heat-treated components. An important consideration is
that the temperature during the coating process should not be high, as it might impair the
substrate properties gained through the heat treatment process. Among the various PVD
coatings, the recently developed carbon based tungsten carbide doped coating (WC/C) is
accomplished at a relatively low substrate temperature [254], which renders it suitable for
heat-treated components. In addition to its high hardness and low coefficient of friction,
ranging from 0.1 to 0.2 [255,256], the small thickness (1-4m) achievable in this coating
makes it suitable for application over finished components without casting any sizeable
effect on their dimensions [257].
In the light of above-stated facts, the present study has been taken up to develop an
understanding of the effect of WC/C PVD coating on fatigue performance of substrates
made of various low-alloy steels. The study attempts to investigate the influence of WC/C
coating on the fatigue performance of case carburized low-alloy steels in finite life as well
as infinite life regimes. It aims at quantifying the influence of coating on the fatigue
59


strength corresponding to a given fatigue life for the case carburized low alloy steels. An
attempt is made to understand the mechanisms responsible for the observed fatigue
behaviour by correlating the fatigue properties with measurable parameters, viz. hardness,
residual compressive stress and fracture toughness. Efforts are also made to investigate the
crack propagation mechanisms in case carburized (uncoated) as well as case carburized
PVD coated specimens made of low alloy steels.