Académique Documents
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Residual Stress
Measurement by Diffraction
and Interpretation
Springer-Verlag
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Series Editors
Preface
As industries find that the market for their goods and services is often as closely
connected to their quality as to their price, they become more interested in
inspection and quality control. Non-destructive testing is one aspect of this topic;
the subject of this book is a sub-field of this domain. The techniques for measuring
residual stresses have a long history for a technological subject. Yet, in the last
decade or so there has been renewed and vigorous interest, and, as a result of this,
there has been considerable progress in our understanding and in our methods. It
seemed a proper time to bring the new material together in an organized form
suitable for a course or for self-teaching, hence this book.
After an initial introduction to the qualitative ideas concerning the origin,
role, and measurement of residual stresses, we follow with chapters on classical
elasticity and the relatively new subject of microplasticity. These are primarily
introductory or review in nature, and the reader will find it important to consider
further the quoted references if he is to be involved in a continuing basis in this
area. There follows a chapter on diffraction theory, and then we fuse these subjects
with a chapter on diffraction techniques for measuring stresses and strains which
at present is our most general tool for non-destructive evaluation in this area.
In Chap. 6 we explore how to evaluate errors in such a measurement, a topic
almost as important as the stress itself and certainly vital in automating the
measurement. Practical examples are described in Chap. 7 and means for
measuring the strain distribution, in Chap. 8, in contrast to the measurement of
average values described in the earlier chapters.
The Appendices include solutions to the problems given at the end of some of
the chapters, Fourier analysis, and sources of useful data.
We emphasize diffraction because in our opinion it is the most well understood and reliable tool available for the measurement of stresses. Of course our
own background in niffraction colors our opinion, but we hope this book will
reveal to the reader why we feel this way.
Dr. M. James provided Appendices E and F, and Mr. W. P. Evans supplied
many practical examples for Chap. 7. Both gave us helpful comments on the
manuscript.
Both authors thank our many co-workers in this field, Drs. R. Marion,
M. James, H. Dolle,W. Schlosberg, Prof. Jai Wen Ho, Mrs. Rui Mai Zhong,
Messrs. T. Devine, W. Evans, and P. Rudnik. The two of us have enjoyed (most
of the time) working together over the past five years on research in this field and
on this book. One of us (I. C. N.) especially acknowledges the support of his
family.
I. C. Noyan
Evanston, IL, April 1987
J. B. Cohen
Dedication
We dedicate this book to the U.S. Office of Naval Research and particularly to
Dr. Bruce MacDonald of this office. His foresight led us into this field and his
helpful encouragement and support led us along many interesting avenues of
research on residual stresses.
Contents
1 Introduction . . . . . . . . . . . . . .
1
4
7
12
13
2.1 Introduction . .
2.2 Definitions . . . .
2.3 Stress and Strain. .
2.4 Forces and Stresses
2.5 Displacements and Strains
2.6 Transformation of Axes and Tensor Notation
2.7 Elastic Stress-Strain Relations for Isotropic Materials.
2.8 Structure of Single Crystals . . . . . . . . .
2.9 Elastic Stress-Strain Relations in Single Crystals
2.10 Equations of Equilibrium. . . . . . .
2.11 Conditions of Compatibility. . . . . .
2.12 Basic Definitions in Plastic Deformation
2.13 Plastic Deformation of Single Crystals .
2.14 Deformation and Yielding in Inhomogeneous Materials.
Problems . .
Bibliography. . . . . . . . . . . . . . . . . . . . . .
13
13
14
15
17
20
25
28
32
37
38
39
41
44
45
46
47
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8
3.9
3.10
3.11
3.12
47
47
51
52
54
56
61
62
63
65
66
69
Introduction . . . . . . . . . . . . .
Macroresidual Stresses . . . . . . . . .
Equations of Equilibrium for Macrostresses
Microstresses . . . . . . . . . . . . .
Equations of Equilibrium for Micro- and Pseudo-Macrostresses
Calculation of Micro- and PM Stresses . . . . . . . . . . .
The Total Stress State in Surface Deformed Multiphase Materials
Macroscopic Averages of Single Crystal Elastic Constants .
The Voigt Average. . . . . . . . . . . . . . . .
The Reuss Average . . . . . . . . . . . . . . .
Other Approaches to Elastic Constant Determination.
Average Diffraction Elastic Constants . . . . . . .
VIII
Contents
Summary
References.
73
73
75
4.1 Introduction . . . . . . . . . . . .
4.2 Fundamentals of X-rays . . . . . . .
4.3 Short-wavelength Limit and the Continuous Spectrum
4.4 Characteristic Radiation Lines .
4.5 X-ray Sources. . . .
4.6 Absorption of X-rays.
4.7 Filtering of X-rays. .
4.8 Scattering of X-rays .
4.9 Scattering from Planes of Atoms.
4.10 The Structure Factor of a Unit Cell
4.11 Experimental Utilization of Bragg's Law
4.12 Monochromators . . . . . . . . . .
4.13 Collimators and Slits. . . . . . . . .
4.14 Diffraction Patterns from Single Crystals
4.15 Diffraction Patterns from Polycrystalline Specimens
4.16 Basic Diffractometer Geometry . . . . . .
4.17 Intensity of Diffracted Lines for Polycrystals
4.18 Multiplicity. . . .
4.19 Lorentz Factor . .
4.20 Absorption Factor .
4.21 Temperature Factor
4.22 X-ray Detectors . .
4.23 Deadtime Correction for Detection Systems
4.24 Total Diffracted Intensity at a Given Angle 28 .
4.25 Depth of Penetration of X-rays . . . . . . .
4.26 Fundamental Concepts in Neutron Diffraction.
4.27 Scattering 'and Absorption of Neutrons
Problems . . . . . . . . .
Bibliography and References. . . . . . .
75
75
76
77
80
82
84
84
86
87
89
90
91
93
94
95
97
98
98
100
103
103
108
109
110
111
114
116
116
117
5.1 Introduction . . . . . . . . . . . . . . . . . .
5.2 Fundamental Equations of X-ray Strain Determination
5.3 Analysis of Regular "d" vs. sin 2 \jJ Data. . . . .
5.4 Determination of Stresses from Diffraction Data.
5.5 Biaxial Stress Analysis . . . . . . . . . . . .
5.6 Triaxial Stress Analysis. . . . . . . . . . . .
5.7 Determination of the Unstressed Lattice Spacing.
5.8 Effect of Homogeneity of the Strain Distribution and Specimen
Anisotropy . . . . . . . . . . . . . . . . . .
5.9 Average Strain Data from Single Crystal Specimens . . . . . .
117
117
119
120
122
125
126
130
131
IX
Contents
140
145
153
154
157
159
160
162
162
164
6.1
6.2
6.3
Introduction . . . . . . . . . . . . . . . . . . . .
Selection of the Diffraction Peak for Stress Measurements .
Peak Location. . . . . . . . . . . . . . . .
6.3.1 Half-Value Breadth and Centroid Methods.
6.3.2 Functional Representations of X-ray Peaks.
6.3.3 Peak Determination by Fitting a Parabola .
6.3.4 Determination of Peak Shift . . . . . . .
6.4 Determination of Peak Position for Asymmetric Peaks
6.5 Statistical Errors Associated with the X-ray Measurement 'of
Line Profiles . . . . . .
6.6 Statistical Errors in Stress.
6.6.1 The sin 2 tp Technique
6.6.2 Two-Tilt Technique.
6.6.3 Triaxial Stress Analysis
6.6.4 Statistical Errors in X-ray Elastic Constants
6.7 Instrumental Errors in Residual Stress Analysis .
6.7.1 Variatiol). of the Focal Point with 9 and tp .
6.7.2 Effect of Horizontal Divergence on Focusing.
6.7.3 Effect of Vertical Beam Divergence . . . . .
6.7.4 Effect of Specimen Displacement . . . . . .
6.7.5 Effect oftp-axis not Corresponding to the 29-axis .
6.7.6 Error Equations for the tp-Goniometer . . . . .
6.7.7 Effect of Errors in the True Zero Position of the tp-axis
6.7.8 Alignment Procedures. . . . .
6.8 Corrections for Macrostress Gradients
6.9 Corrections for Layer Removal
6.10 Summary.
Problems .
References. . .
136
137
164
164
166
167
168
171
175
178
181
186
186
187
187
189
190
191
192
195
196
199
200
202
. 203
. 205
206
208
209
209
Contents
211
7.1
7.2
7.3
7.4
7.5
Introduction . . . . . . . . . .
The Use of Ordinary Diffractometers .
Software and Hardware Requirements
Available Instruments . . . . . . .
Selected Applications of a Portable X-ray Residual Stress Unit
(By W. P. Evans) .
Reference . . . . . . . . . . . . . . . . . . . . . .
211
211
212
213
230
8.1 Introduction .
8.2 Slit Corrections
8.3 Fourier Analysis
Problem. .
References. . . . .
. . . . . . .
230
233
238
245
247
248
Appendix B . . . . . . . . . .
B.l Introduction . . . . . . . .
B.2 The Marion-Cohen Method. .
B.3 Dolle-Hauk Method (Oscillation-free Reflections)
B.4 Methods of Peiter and Lode. .
B.5 Use of High Multiplicity Peaks
References. . . . . . . . .
252
252
252
254
256
257
257
259
266
267
270
271
Subject Index
273
. . . . . . . . . .
. . . . . . . . . .
of Peak Broadening.
214
229
1 Introduction
In 200 B.C., Chinese artisans manufactured thick bronze discs that were flat and
polished on one side and had a relief cast on the other face. These were heated and
quenched. When such a "magic mirror" was illuminated on the flat face, the
reflection showed the pattern of the relief on the other side of the disc! Due to the
different cooling rates of the sections with various thicknesses, distortions occurred
on the flat side, which mimicked the pattern of the relief. To our knowledge, this is
the first deliberate use of residual stresses and strains. Today we know these playa
key role in the behavior of welded structures (and hence in ship construction,
pipelines and oil rigs) , in the response of heat treated or finished parts (ground
gears, shot-peened or sand blasted pieces, or material subjected to laser heat
treatments, or quenched after a heat treatment). These stresses are also a key
factor in the fatigue response of solids, and in the phenomenon known as stress
corrosion.
1 Introduction
Cooling curves
.:
.:
c;,
c:
OJ
-I
Q,
c
local
yielding
OJ
-I
Phase
transition
I
I
Time
Time
b
Strain
Fig. 1.1 a,b. Schematic cooling curves during heat treatment showing the difference in contraction
of the surface and interior. In a there is no phase transition, whereas one occurs in b. c Surface
deformation by peening elongates surface regions. 1, Surface element elongated by peening put
into compression by interior. d The harder surface regions contract more (on release on the load
at A) than the softer interior. 1, Hard region; 2, soft region. e Friction at the rolls in a rolling mill
tends to extend surface regions more than the interior. f Stresses due to welding. 1, Longitudinal
shrinkage; 2 weld metal; 3 lateral shrinkage; 4 stresses
1 Introduction
can be a significant portion (half or more) of the ultimate tensile strength of the
annealed material. Furthermore, in addition to residual stresses, it is sometimes of
interest to measure applied stresses.
(1.1 )
(1.2 )
Therefore, taking the first two terms of (1.2), a better approximation is:
cr~
(M+CE)E=M'E.
(1.3 )
(1.4 )
The wave velocity depends on the state of strain, E, in the material, and hence on
the residual stresses. Unfortunately, the distribution of phases present can
produce effects that so far have prevented general use of this technique. Some
progress is being made however (see Ref. [14]) but, so far, only for uniaxial
loading.
Still another stress measuring method is associated with the Barkhausen
"noise" in magnetic materials, produced when magnetic domains are moved by a
field close to the material [15]. This noise is sensitive to the stress fields in the
material since the fields affect the ease of rotation of the domains. The measuring
equipment is simple, but unfortunately the technique is limited to ferrous alloys.
Furthermore, the noise signal saturates at about 500 MPa (70,000 psi) in either
28
,...
I \
I \
I
____ J
28
Specimen
Fig. 1.2. a Schematic of diffractometer. The incident beam diffracts X-rays .ofwavelength A. from
planes that satisfy Bragg's law in crystals with these planes parallel to the sample's surface.
If the surface is in compression, because of Poisson's ratio these planes are further apart than in
the stress-free state. The d spacing is obtained from the peak in intensity versus scattering angle 20
and Bragg's law A. = 2d sin O. b After the specimen is tilted, diffraction occurs from other grains,
but from the same planes, and these are more nearly perpendicular to the stress. These planes are
less separated than in a. The peak occurs at higher angles of20. c After the specimen is tilted, the
stress is measured in a direction which is the intersection of the circle of tilt and the surface of the
specimen
tension or compres~ion so that the method is most useful (after calibration) for
determining the sign of the stress, but not its magnitude. More details on magnetic
and acoustic technique are reviewed in Ref. [16].
Plastic models can be employed to simulate a part, or a production method,
and the stress obtained from the birefringence oflight passed through the plastic
[17]. Progress is also being made in calculating the stress pattern, see papers in
Ref. [11] by Ericsson and Hildenwall, and Yu and Macherauch.
1 Introduction
Slit
Fig. 1.3. Neutron scattering. The beam penetrates the entire volume, but slits define a
local volume. By moving the slits as shown,
or the sample vertically, the stress in different volumes may be measured
various depths, using a slit as shown in Fig. 1.3. The resolution in this case is the
order of 1 - 2 mm, depending on the neutron intensity (that is the reactor
power).
Finally, it is worth mentioning that it is possible to monitor the development or
change in stresses in use, by first measuring the value with diffraction, and then
attaching strain gages or grids. Reference [22] describes some of these procedures.
measurements and the useful information such results provide. References to the
recent literature will be given, so that the reader can obtain more details. (We rely
largely on our own work, because we know it best.)
In preparing samples for mechanical testing, surfaces are often ground, or
sometimes even polished metallographically. ,(S Fig. 1.4 shows, for an HSLA steel
such methods can produce quite large stresses, even at significant depths [23].
Because these techniques of surface preparation are not usually carefully
monitored, different stresses may develop in each sample, and could be the source
of scatter in the data. Although it is not generally done, measurement of such
stresses prior to testing could be quite revealing!
Most parts in machines, engines, etc. are subject to rapidly varying alternating
stresses as they move. This alternating stress is described as fatigue. If the part fails
in only a small number of cycles, this is called low-cycle fatigue. (The stresses in
this case are relatively large, but may be below the static yield.) As Fig. 1.5 shows,
the residual stresses have a different sign, depending on whether the part is
released from the tensile or compressive portion of the alternating load [23].
In high-cycle fatigue, at much lower stresses the behavior of residual stresses is
not yet understood, although changes do occur. In a part without any initial
stresses, stresses may develop, as shown in Fig. 1.6 for an annealed 1040 steel [24]
in tension-tension fatigue (i.e. the applied load is tensile, then reduced, then tensile
etc.). Note that these stresses are compressive and therefore not harmful. In fact,
300.---------------------------~
MPa
200
III
III
100
C:i
::l
"tl
ID -100
n:
-200
-3000~--~~--~~--~~--~~~
0.05
Thickness removed
1 Introduction
III
III
300r----------------------------.
MPa
0 1 cycle. compo
200 I- " 100 cycles. compo
1 yccle. tension
100
... 100cycles . tension
Iii
O~"''''''
:J
Vi -100
&!
'f.
,....... --.,
...
.~~.~.~_r--~----~--
':I.
-&
-240
MPo
-200 l-
-160 r--
III
III
Cl>
';;-120
1III
a:J
u
Vi
-80
I-
-40
I-
Cl>
a:
01-40
1
~'
/1
I
10
10 2
10 3 101. 10 5 10 6 10 7 108
Number of cycles
they impede crack propagation and undoubtedly add to the life of the part.
However, if stresses are induced by processing, they "fade" at a rate which
increases with the cycling stress. An example is shown in Fig. 1.7. In this case
(peened 1040 steel, tension-tension fatigue), the initially beneficial compressive
stresses not only decrease, but reverse in sign early in the stress cycling, and
decrease the life. (This reversal occurs only in tension-tension fatigue but not in
bending, in which case only fading occurs.)
A two-dimensional map of the stresses ahead of a fatigue crack are shown in
Fig. 1.8 [25J; the component shown is normal to the crack face. Such stresses exist
well beyond the plastic (shaded) region, caused by the stress concentration ahead
of the crack, due to plastic upset in the region. Note the stresses behind the crack
front, and that the stress is compressive at the tip, impeding crack propagation.
During machining (milling, turning, or grinding), the near-surface region of
the workpiece is deformed plastically. As volume elements in this region are
extended when the tool passes by, the constraints of the bulk should introduce
compressive stresses near the surface. Indeed, this does occur for shallow, slow,
-600 r-------------------------~
-500 1"'.
-1.00 f- \
1Il - 300fIII
'"
~
-200 f-
-100
1:)
'iIi
0-
'"
cr:
80
~
100 -
200 -
102 10 3 10'
10
105 106
Number of cycles
2 .40
2.00
1.60
. 1.20
0.80
0 .40
If>
48
-~9
.,3
~2
16
- 05
0">
,"
~3
16
o.
- 0 .95 -0.55 -0 .1 5
0 .2 5
0 . 65
105.BI
\.05 1.45
1.9
1.0
1.85
(mm)
Fig. 1.8. Residual stresses around a fatigue crack produced by tension-tension fatigue of an HSLA
steel (in MPa). From Ref. [25]
well-lubricated cuts with a sharp tool. But, extensive studies of the stress pattern
have shown that the actual situation is usually much more complex. If strong work
hardening occurs only near the surface, this produces tensile residual stresses due
to the greater elastic relaxation of this region compared to the bulk. Local
compressive plastic deformation due to the pressure by the tool will cause tensile
residual stresses, and, if the sum of extermil stresses and residual stresses exceed
the local yield strength, plastic recovery will take place in this region. Even when
there is no cross-feed of the tool, a biaxial stress state has been observed. Heating,
due to the lack of lubrication or a dull tool or high downfeed, produces tensile
stresses because locally-heated regions are upset by the cooler surroundings. Thus,
1 Introduction
10
Table 1.1. Residual stress tensors (in MPa) for different samples
Specimen
Armco-iron
A1
151
A2
A6
n.c.
C1
567
-65
508
-4
-7
11
-7
28
-4
267
-12
-12
367
611
55
-8
507
4
74
39
80
90
10
n.c.
12
6
4
380
16
16
351
18
9
18
12
A5
Steel
-7
-8
A4
Specimen
-7
-4
A3
Parameters
of grinding'
645
39
C2
-65
-1
137
199
-10
-63
86
5
84
541
-20
-38
-20
-38
565
1
86
-17
59
6
-10
-63
C3
C4
408
-17
59
416
+-
390
14
14
306
-28
63
557
8
8
82
+-
5
C5
+-
534
-2
10
69
C6
108
63
-1
-1
92
-2
69
-3
-3
95
468
the stress patteni is altered by many parameters, such as the depth of cut, cooling
and cutting direction. For example, after a deeper cut, the stress pattern extends to
a depth greater than after a light cut, although the value of the stress near the
surface can be lower. The level of residual stress is also strongly affected in steel by
the carbon content, which influences the microplastic behavior of the material
significantly. Also, these residual stresses can affect dimensional stability.
We show some results in Table 1.1 for grinding Annco iron and medium
carbon steel [26], with a table motion of 0.33 ms - 1. The entire stress tensor is
shown in the fonn:
(Directions 1 and 2 are in the surface of the specimen, 3 is nonnal to the surface.
The stress cr 13 is in the direction 3 and acts on the face perpendicular to axis 1.)
11
1 Introduction
12
the peak position to stress and strain. Various sources of error are evaluated in
Chap. 6. Portable stress analyzers and several examples of actual measurements
and their use in understanding a material's behavior are .described in
Chap. 7. In Chap. 8, we consider what additional information can be obtained
from the shape of a diffraction peak, which often changes due to stresses in
addition to shifting of the peak.
References
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
2.1 Introduction
In this chapter the basic theorems of linear elasticity are reviewed, and some
fundamental definitions in plasticity theory are discussed. These concepts form the
basis of all types of stress analysis, and will be utilized in subsequent chapters for
the analysis of the deformation distributions that cause residual stress fields.
2.2 Definitions
All solid materials deform when subjected to external loads. The deformation is
manifested in displacements of the points in the body under load from their initial
(unloaded) positions. As long as the forces set up in the body due to external
loading are below a certain limit, the deformation is recoverable; that is, when the
load is removed the displacements vanish and the body returns to its unloaded
configuration. Such behaviour is termed elastic deformation. If, however, this load
limit is exceeded, the material undergoes plastic deformation. In this case some
permanent deformation remains after the load is removed. If the deformation
suffered by the material is uniformly distributed in the material volume, such that
all the points in the material volume have the same amount of deformation, the
deformation distribution is termed "homogeneous". It is also possible to have a
deformation distribution where the deformation varies from point to point along
any direction in the material volume. This type of distribution is called
"inhomogeneous" .'
It is well established that, in most of the elastic range, the deformation is
directly proportional to the load. This is known as Hooke's law. The proportionality constant, similar to thermal or electrical conductivity, etc., is a physical
property of the substance under load. If such properties do not change with
direction, i.e., the same displacement is observed for the same load for all testing
directions, the body is said to be isotropic with respect to that particular property.
However this is not always the case. If a property varies with orientation in a given
coordinate system (but is constant at all points in the material volume along a
given orientation), the body is termed to be anisotropic with respect to that
particular property. If, on the other hand, a given property varies along a given
direction in the material volume, the distribution of the particular property is
inhomogeneous.
14
F
A'
(2.1 )
where F is the applied load and A is the cross sectional area of the bar. For the
example showI\.in Fig. 2.1, the stress distribution is homogeneous since the stress
at any point on un is given by Eq. (2.2). However this may not always be the case.
For example, if the load distribution on the external boundary of the bar is not
homogeneous, the stress distribution on nn will be inhomogeneous. Equation
(2.1 ) will yield an average stress value in this case. The actual stress acting on any
infinitesimal element oN on nn must be calculated by defining the actual force of
acting on such an element. It should be noted that the actual stress acting on oN
may be quite different than the average stress given by Eq. (2.1 ).
The second normalized quantity used in load-displacement analysis, strain, is
defined as the deformation per unit length:
~u
L-Lo
e=Y=-L-
(2.2)
Here ~u is the total deformation suffered by the bar and Lo is the initial length of
the bar, as shown in Fig.2.1. If the bar is an isotropic, homogeneous body,
subjected to a homogeneous load distribution at its boundary, the strain at a point
will be given by Eq. (2.2). For other cases, the strain for an infinitesimal element
oL will be different than the average strain given by Eq. (2.2), resulting in an
inhomogeneous strain distribution.
F
n
L
' - - - - - - - ' ..-
6U
15
In all notations the stresses with mixed indices are the shear stresses. By
convention, the second index defines the normal of the plane in which the stress
acts, and the first index indicates its direction. Thus 0"13 is in the plane defined by
the line Ox 3, and acts in the Xl direction. 0"23 is also in the same plane, but acts
along the X 2 direction.
Normal stresses act along the direction of the axis indicated by the repeated
index. Positive values of stress indicate tensile stresses, while negative values
indicate a compressive stress state.
Thus, stress is a tensor of the second rank and stress components along any
axis require the specification of two indices. It is also seen from Eq. (2.4) that
16
F3 ___ _____
F1
Xl
--- ------
',
(2.5 )
17
(2.6)
(2.7)
N
r--I---i
T
~x
-'
Nt --I-----.
- I - N'
6U+6X
N't--I---'-'
18
x,
x,
0'
:h:_,
17
X,
x,
x',
x,
b
Fig. 2.5. a Displacement, deformation and rotation in two dimensions. b Displacement and
rotation without deformation
which describe the variation of the displacement .::lu l along x~, x~ respectively. The
total displacement at B' along X'l is:
OUl
.::lu l = ~ Lix l
uX l
OUl
+~
.::lx 2
uX
2
(2.10 )
Similarly:
(2.11 )
where
(2.12 )
19
'
o -<I
(2.15 )
(2.16 )
From (2.16) Eij = eji. Thus strain is also a symmetric second rank tensor.
The strain in three dimensions is also obtained by a similar procedure:
ell
- (e 12 +e 2d
- (e13 +e 3d
e22
-(e23+ e32)
= -(e 12 +e 2d
2
-(e13+ e3d - (e 23 +e 32 )
(2.17 )
e 33
The strain tensors described by Eq. (2.17) contain both the dilatation and
distortion terms. The normal strains Ejj contribute to the dilatation part,1, which is
defined as
(2.18 )
.113 is called the mean or hydrostatic strain component along each axis.
20
The distortion terms in the strain tensor are obtained by subtracting 11/3 from
each Eii :
(2.19 )
where
E;j
Xl
X3
(2.20a)
or:
Xl
X2
X3
Xl a 11 a 12 a 13
X1 a 21 a 22 a 23
X3 a 31 a 32 a 33
(2.20b)
21
X;\
\
\
\
L71
)Lp"2
x,
(0'.
x,
It
- ---x;
'/
x,
/
/
,
x,
Here the first subscript refers to the "new" axis (in L) and the second to the "old"
axis (in S), following Nye.
Let F be a force vector with components F I,F 2,F 3 in the S coordinate system.
The components of F along L,F'I ,F~,F~ may be obtained by resolving each Fj
along X'I ,x~,x~ and then summing up the components for each x;. For example the
new force component along x~ will be:
F~=F 1cos (Xl X'd +F 2COS (x2x'd +F3 cos (x3x'd.
(2.21 a)
The force F; has components from all F j Equation (2.21 a) may be written more
compactly by utilizing Eq. (2.20b):
(2.21b)
F~ =a 31 F 1 a32F 2 + a 33 F3 .
x~
and
x~:
(2.21c)
In Eqs. (2.21a,b,c) the leading subscript for each of the direction cosines a jj is the
same as the subscript for the new direction along which the new force component
is being determined. Thus Eqs. (2.21) can be written more compactly as
F; =
L Fj"a jj .
j= 1
(2.22 )
22
This equation can be simplified further through the use of the Einstein suffix
notation:
(2.23 )
Here i occurs singly on the left hand side of the equation and denotes the new
direction along which the force component is required. It is termed a free suffix
and is defined by the user of the equation. The index "j", on the other hand, is
repeated on the right hand side of the equation. Such repetition implies summation
of the terms in the equation over all possible values ofj. An index such as "j" in this
example is called a dummy suffix.
The transformation of stresses, caused by the loading forces, from S to L
utilizes the transformation rule for second rank tensors:
(2.24 )
where ij are the free sufflXes and define the stress O";j in S. Since both k and I are
repeated on the right hand side of the equation they are both dummy suffixes and
summation of 3.;k a jl ( over all possible combinations of k and I) is required. For
example, expanding Eq. (2.24) for arbitrary ij:
O"ij= 3.;1aj10" 11 + 3.;1 aj20"12 +ail aj3O"13
+ 3.;2aj1 0" 12 + 3.;2 a j20"22 + ai2a j30"23
+ a i3 aj1 0"13 + a i3 aj20"23 + ai3aj30"33 .
(2.24b)
For each ij pair, one such equation exists. Since stress is a symmetric second rank
tensor, six such equations, each with nine components on the right hand side, are
required for the complete transformation of O"ij in L to O";j in S.
The transformations given by Eqs. (2.23), (2.24) are valid for all first and
second rank tensors, respectively, and are not restricted to the transformations of
forces and stresses. They can be applied, for example, to the electric field vector (a
tensor of the first rank) , or to electrical conductivity (a tensor of second rank) .
For symmetric second rank tensors it is possible to define a unique coordinate
system in which the tensor has no off-diagonal components. That is, a tensor of the
form
dermed in S, becomes
when transformed into the new set of coordinate axes P. The set of axes P, thus
defined, are the principal axes, and the tensor components referred to them are
called the principal tensor components.
23
B
Fig. 2.8. The principal unit cube and an
arbitrary unit cube in a homogeneously
stressed solid
F
Since both stress and strain are symmetric second rank tensors, it is possible to
determine the principal axes associated with them (sometimes called eigenvectors
in the literature). Physically, this means that it is possible to define a unit cube in a
generally stressed material on whose faces only normal stresses (Fig. 2.8), or
normal strains, act. These stresses and strains are also termed principal stresses
and strains.
Principal stresses and the direction of the principal axes can be easily
determined in terms of the stresses existing in an arbitrary cartesian coordinate
system. Consider the homogeneously stressed, tetrahedron-shaped, free body in
Fig. 2.9, which is at static equilibrium. Assume that the normal N to the plane ABC
is a principal direction, along which the principal stress crii acts, and which makes
the direction cosines a, b,c with the coordinate system Xi' ( a 2 + b 2 + c 2 = 1 ), in
which a general stress tensor cr;j is defined. Writing the force balances of the free
body for the X 1,X 2,X3 directions:
( crii - cr ~ l)'a - cr'12b- cr'l3'C
=0
-cr'12a + (crii-cr~2)b-cr~3c=O
- cr ~3'a- cr~3b+. (cr ii - cr~3) 'c=O,
(2.25 )
24
(2.28 )
(2.29)
The roots of Eq. (2.28),0"11,0"22,0"33' are the principal stresses. The direction
cosines a,b,c, can then be obtained from Eq. (2.25).
It must be noted that, since the coefficients 11,12,1 3 of the cubic Eq. (2.28)
define the principal stresses, they are independent of the stresses O";j, defined in the
arbitrary coordinate system Xi' These quantities are called the stress invariants.
From the first stress invariant 11 , which is the sum of the leading diagonal of the
25
stress tensor, it is seen that the sum of the normal components in any coordinate
system is invariant and equal to the sum of the principal stresses.
An equivalent discussion can be also given for the strain tensor. In this case
Eq. (2.28) becomes
( Eii ) 3- I~ ( Eii ) 2 + I~ ( Eii )
I~ =
(2.30)
0,
where
I~ =E~l +E~2 +E~3
(2.31 )
The terms I;, defined by Eq. (2.31) are the strain invariants.
(2.32a)
(2.32b)
-+
A
26
1
Ejj = "O"jj,
v
Ejj = - E O"jj,
i=l=j.
(2.34)
Thus for a unit cube subjected to three normal stresses 0"11 ,0" 22,0" 33' the strain
along any direction Xi is the sum of the strain caused by the stress in that direction,
and the strains caused by the stresses acting in the transverse directions:
1
v
E11 =EO"l1-E (0"22+0"33)
1 ..
V
E22= E 0"22-" (0"11 +0"33)
(2.35)
1
v
E33 ="0"33-E (0"11 +0"22).
From Eqs. (2.17) and (2.35) it is seen that for isotropic materials, normal stresses
O"jj cause only dilatation. Pure distortion (shape change) occurs when a shear
stress O"ij' i =1= j, is applied to the material. The shear strain in this case is given by
1
2Eij =Y= ~O"ij,
i=l=j.
(2.36)
Here the quantity y = 2Eij is called the "engineering shear strain" and the
proportionality constant "11" is called the shear modulus. For isotropic materials 11
is related to E and v by 211 = Ej ( 1 + v ) .
Equations >( 2.35) and (2.36) can be expressed compactly in the suffix
notation as
(2.37 )
where k is the dummy suffix and implies summation for all k, and ()ij is
Kronecker's delta, which is defined as:
1, i=j
()ij = { 0 . =1=
,
1 J.
(2.38)
v
1 +v
Ell = 0"11-" (0"11 +0"22+0"33)
which is identical to Eq. (2.35).
(2.39a)
27
Table 2.1. Young's modulus and Poisson's ratio for some materials (at room temperature)
Material
E(GPa)
Aluminum
Copper
Gold
Iron
Molybdenum
Tungsten
Titanium Carbide
Lead
70.3
129.8
78.0
211.4
320.0
411.0
436.9
24.5
0.345
0.343
0.44
0.293
0.293
0.280
0.199
0.410
Data adapted from R.W. Hertzberg, Deformation and Fracture Mechanics of Engineering
Materials, Wiley, New York, 1976, p.8, and G. Simmons and Herbert Wang, Single Crystal
Elastic Constants and Calculated Aggregate Properties, MIT Press, Massachusetts, 1971
(2.39b)
and substituting for any two stresses O"jj'O"Il in (2.39b) (i.e. the stresses 0"22,0"33'
expressed in terms of strains I':ij from equations similar to (2.39a), would be
substituted in (2.32b) if we wanted to determine 0"11 ) :
E
vE
O"ij = (1 + v) I':ij + (1 + v) ( 1 _ 2v) oihk
(2.40)
The term vE/[ (1 +v) (1- 2v)] is usually represented by the symbol A and is
called Lame's constant.
From Eq. (2.18) and Eqs. (2.35), (2.39) it can be seen thatthe dilatation A is
linearly related to the hydrostatic component of stress that causes it:
A=
(1-2v)
1
E
.30"Hyd. = K O"Hyd.
(2.41 )
where O"Hyd. = ( 1/3) O"kk and K is called bulk modulus. It can be seen by inspection
that for isotropic materials, K = E/3 ( 1 - 2v ) .
From an examination of the above equations, it can be seen that the stressstrain relations for an isotropic solid in the elastic range require the specification of
only two constants E and v. Typical values of these constants for some important
materials are given in Table 2.1.
Up to this point elastic behaviour in homogeneous isotropic solids has been
discussed. Single crystals, or the grains in a polycrystalline material, are
homogeneous (in a macroscopic sense) but anisotropic solids. Thus, the simple
equations between stress and strain given in this section are no longer applicable
and a more general treatment that takes into account the particular structure of
single crystals is required.
28
!11J
1
acto
1
10
II
-.-
o '.
12
13
14
Fig. 2.11. Unit cells of the 14 Bravais lattices: 1, Simple triclinic; 2, simple monoclinic; 3, basecentered monoclinic; 4, simple orthorhombic; 5, base-centered orthorhombic; 6, body-centered
orthorhombic; 7, face-centered orthorhombic; 8, hexagonal; 9, trigonal (rhombohedral);
10, simple tetragonal; 11, body-centered tetragonal; 12, simple cubic; 13, body-centered cubic
( BCC); 14, face-centered cubic (FCC)
29
Triclinic
Monoclinic
Three axes, one pair not at right angles, all of unequal lengths.
a 1 *a2 *a3 , cx* ~*y=900
Orthorhombic
Tetragonal
Hexagonal
Trigonal
Three axes of equal length, all equally inclined but not mutually
perpendicular.
a 1 =a2 =a 3 . cx= ~=y*900.
Cubic
ment at any point in the crystal is uniquely defined by the symmetry associated
with this particular lattice. There are only fourteen different ways of arranging
points in space such that each has identical surroundings. These point lattice
arrangements are called the Bravais lattices. They are described simply by a unit
cell which reflects their symmetry. This unit cell can be repeated periodically (like
stacking bricks in a wall) to form the complete lattice. In Fig. 2.11 and Table 2.2
. the fourteen point lattices and the seven crystal unit cells that describe them are
shown. Each of these cells has several possible arrangements of atoms around the
points consistent with periodicity, (but because of periodicity the number of such
arrangements is limited), resulting in 230 "space groups", or possible patterns for
atomic structures: We say patterns because the dimensions and actual distances
between the atoms vary for the same pattern, depending on the material. (For a
complete discussion of symmetry and point groups, the reader is referred to the
standard texts on the subject. See, for example, "Diffraction from Materials" by
Schwartz and Cohen. )
The position of an atom within the unit cell is given by its fractional coordinates
u,v,w, where u,v,w are defined by the vector r=ua 1 +va 2 wa 3 , that connects the
atom to the origin ofthe unit cell. For example an atom at the body center of a unit
cell, referred to an orthogonal set of axes has the coordinates ~,~, ~, while the one
at the origin is located at 000.
The direction of any line in a unit cell is described by drawing a line through the
origin parallel to the given line and then expressing the coordinates of this line as
the smallest set of integers that is a multiple of these coordinates. Directions are
30
[001]
,A
[101]
[021]
[010]
[100]
[100]
Fig. 2.13. a Various crystallographic planes in a cubic unit cell. b Various crystallographic planes
and directions in a hexagonal unit cell
31
cube axes at l/h,1/k,1/1 are (hkl). Alternately, the intercepts of the plane (211) is
0.5 along Xl and 1 along X 2 and x3 . If a plane is parallel to one of the axes, its intercept is at infinity and the Miller index for that axis is o. In Fig. 2.13a various planes in
a cubic lattice are illustrated. Using a reasoning similar to the one given for the
equivalent directions, it can be seen tha the planes (100), (010), (001), (TOO),
(010), (001) are equivalent planes related by symmetry. Such planes are called
planes of a form and are denoted by {hkl}. In the case discussed above the planes
belong to the {100} form.
For hexagonal systems a slightly different system of plane indexing is used
instead of the one discussed above. In this scheme a third axis a 3 , which makes
angles of 1200 with the basal vectors a 1 ,a 2 , is defineq in the basal plane of the
hexagonal unit cell. The Miller indices of any plane are then determined by
obtaining the inverse of the fractional intercepts of the plane on the three basal
axes a1>a 2,a 3 and the vertical axis c. Thus four numbers [hkil] are specified as the
plane indices. Since the intercepts on a 1,a2 uniquely determine the intercept on a 3,
the index i is a function of the indices hand k, where i is given by
(2.42 )
h+k= -i.
In Fig. 2.13b, various planes and directions in a hexagonal unit cell are shown. It
must be noted that, even though the plane indices are referred to four indices as
described above, the lattice directions are referred to the three crystallographic
axes a 1 ,a 2 ,c, in keeping with the convention for all crystal systems.
A single crystal of finite dimensions contains a very large number of unit cells,
each with its own set of {hkl} planes. For an unstressed single crystal, the family of
(hkl) planes throughout the volume are parallel (due to symmetry) , and the plane
spacing between them is constant. This spacing oflattice planes is a function of the
indices (hkl) of the plane and the unit cell constants a 1,a2,a 3,Cl,(3;y. A summary of
these relationships for some unit cells is given in Table 2.3. In general, all planes of
a family have the same lattice spacing.
Table 2.3. Formulas relating the plane spacing, dhkb to the indices h, k, I, and unit cell parameters
for various unit cells '
Cubic
Tetragonal
Hexagonal
Rhombohedral
Orthorhombic
d2
1 h 2 k 2 J2
-=-+-+d2 a~ a~ a~
32
Vro
(dV)
dr
ro'
1(ddrv)
u +2
ro'
u 2 + ... ,
(2.43a)
Noting that
The applied force is the derivative of the potential energy with respect to
displacemen t:
F=
ov (u) = (02V )
OU
or2
.U
ro
'
( 2.44a)
or
F=K-u
where K,
(2.44b)
Equation (2.44b) is the original form of Hooke's law. If, instead of forces and
displacements, it is expressed in terms of stresses and strains, the proportionality
constant is direc;tly proportional to the elastic modulus of the material.
From the above discussion, the elastic modulus will be the same for both
tension and compression since K is independent of the sign ofu. As it is dependent
only on the variation of the interatomic forces with interatomic distance about the
equilibrium position, the modulus is a basic material property and is not
significantly affected by processes such as heat treatment or plastic deformation
for most common engineering materials. Furthermore, since along various
directions in the point lattices the spacing between the atoms is different, the
variation of potential energy with distance, and hence the elastic modulus, will
change with direction, causing anisotropy. However it must be noted that, because
a crystal is built up by repeating the unit cell periodically, the elastic modulus
along a given direction will be constant through the crystal volume.
>
33
r-
(2.45 )
Eij = SjjklO"kl
or, inverting the equation and expressing stresses in terms of strains:
(2.46)
Here Sjjkl,C jjkl are the compliance and stiffness moduli of the crystal under
consideration, and are both tensors of the fourth rank.
Equation (2.45) means that if a general homogeneous stress is applied to a
single crystal, the resulting homogeneous strain is linearly related to each
component of the stress tensor through the appropriate component of the
compliance tensor. For example the strain in the Xl direction, Ell' is given by:
Ell = Sl1l1 0" 11 + Sl112 O" 12 + Sl113O" 13 +S1121 0" 12 + Sl1220"22
(2.47)
tensor notation
matrix notation
11
22
33
23,32
31,13
12,21
34
(2.48 )
The matrices Sjj and Cjj are 6 x 6 matrices and contain 36 terms each. However not
all of these terms are finite and independent. It can be shown, from consideration
of the strain eJlergy of a crystal, that for any crystal Sij = Sji" Similarly C jj = Cjj.
Thus the number of independent constants is reduced to 21 (for i = j, there are six
terms, and for the remaining 30, only one half is independent, for a total of 21 )
for a general anisotropic crystal. A particular crystal symmetry or atomic
arrangement can further reduce the number of independent constants (see Nye
for a complete discussion). For example, for cubic materials there are only three
independent constants. The compliance matrix in this case becomes
Sjj=
Sl1
S12
S12
0
0
0
S12
Sl1
S12
0
0
0
S12
S12
Sl1
0
0
0
0
0
0
S44 0
0
S44
0
0
0
0
0
0
0
0
0
0
S44
(2.49)
It should be noted that, even though there are three independent constants for
cubic crystals, the compliance matrix contains nine non-zero components. In
Table 2.4 the number of independent constants and total number of non-zero
components for each of the seven crystal unit cells is given. It can be seen that as
the symmetry o(the crystal increases, the number of independent constants in the
stiffness and compliance matrices decrease. Typical values of stiffnesses and
compliances for various crystals are shown in Table 2.5.
The stiffnesses and compliances given in Table 2.5 are defined in the unit cube
axes, (100), which are also termed crystal axes. The compliance (or stiffness)
tensor in any otqer coordinate system can be calculated from the transformation
law for fouith rank tensors:
(2.50)
where Sjjkl is the elastic compliance in the new coordinate system, ajj are the
direction cosines between this system and the crystal axes, and Smnop are the
35
Table 2.4. Number of independent constants and number of non-zero elements in the stiffness and
compliance matrices of the seven unit cells
Crystal system
Independent constants
Triclinic
Monoclinic
Orthorhombic
Tetragonal
Trigonal
Hexagonal
Cubic
Isotropic
21
13
9
7'
21
13
9
11'
7-
1499
3
2
, For certain symmetries this lattice has 6 independent constants and 12 finite elements
- For certain symmetries this lattice has 6 independent constants and 9 finite elements. See Nye
for details
Table 2.5. Elastic stiffness and compliance values for selected materials
Material
(cubic)
C ll
C 12
C 44
10.82
16.84
18.60
23.70
46.00
50.1
27.9
51.3
Material
( hexagonal)
C ll
Titanium
Zinc
16.0
16.1
C I2
6.13
12.14
15.70
14.10
17.6
19.8
15.3
10.6
C 13
C 33
2.85
7.54
4.20
11.60
11.0
15.14
15.3
17.8
1.57
1.50
2.33
0.80
0.28
0.26
0.585
0.21
C 44
Sll
(x10 Io Pa)
9.0
3.42
S44
(x 10- 11 Pa -I)
(x10 10 Pa)
Aluminum
Copper
Gold
Iron
Molybdenum
Tungsten
Spinel
Titanium carbide
SI2
SII
-0.57
-0.63
-1.07
-0.28
-0.08
-0.07
-0.208
-0.036
SI2
SI3
3.51
1.33
2.38
0.86
0.91
0.66
0.654
0.561
S33
S44
(x 10- 11 Pa -1)
6.6
5.01
18.1
6.1
4.65
3.83
.97 -.47
.84
.05
-.18 .69
-.73 2.84
2.15
2.61
compliances defined, in the crystal axes. Equation (2.50) can also be used to
determine Young's modulus for any arbitrary direction: Assume that a uniaxial
stress 0' is applied to a cubic single crystal along the direction [hkIJ. The strain
along [hklJ is linearly related to the stress through Hooke's law:
E=
1
-(E) .0'.
hkl
( 2.51)
36
1.22
3.20
2.86
2.51
0.79
1.00
0.877
2.43
E(100)
E(lIl)
(GPa)
(GPa)
63.7
66.7
42.9
125.0
357.1
384.6
476.2
170.0
76.1
191.1
116.7
272.7
291.6
384.6
429.2
364.5
However, since the material is anisotropic, Eq. (2.51) can also be written through
the general form of Hooke's law. Arbitrarily defining [hkl] as the x~ of a
coordinate system,
(2.52 )
where S' 1111 are referred to the x; coordinate system. From Eq. (2.50), (2,51) and
( 2.52 ), Young's modulus along [hkl] can be written in terms of elastic
compliances S;jkl defined in the crystal axes:
1
.
-(E) =Slill =almalnalOalpSmnop'
hkl
(2.53)
Here alj are the direction cosines between the crystal axes and the direction [hkl].
Expanding Eq. (2.53), and noting that the terms almalnalOalpsmnop indicate
summation over all mnop, with m,n,o,p = 1,3 (i.e., all nine components of the
compliance tensor (2.49) will contribute to the summation), one obtains:
1S44 ](alla12+aI2a13+alla13)
22
(E1).
hkl =Sllll=Sll-2 [(Sll-S12)-2
22
22
(2.54 )
Equation (2.54) shows that Young's modulus in cubic crystals is anisotropic,
and is a function of the direction cosine term (aIlaI2+aI2aI3+aIlaI3)' This
term varies between 0 for the (100) family of directions, and
family. Thus the direction with the maximum Young's modulus depends on the
term Sll - 2 [( Sll - S12) -
~ S44
J.
exhibits a maximum along (111) and a minimum along (100). Ifit is negative, as
it is for Mo, the maximum is along (100), and the minimum along (111). If this
term is zero, Young's modulus is isotropic. That is, it is independent of direction.
Thus, for isotropic materials Sl1 -S12 =
(Sl1-S12)- ~ S44' the greater the anisotropy in Young's modulus. This quantity
37
(CT 12 hJ OX I OX 3
(2.55)
+ OCT12 + OCT 13
oX 2
OX3
=0.
(2.56a)
OCT12
oX I
+ OCT 22 + OCT 23
=0
OCT l3
oX I
+ OCT 23 + OCT 33
=0
oX 2
OX2
oX 3
oX 3
(2.56b)
(2.56c)
38
j=!
(2.57 )
OO'ij =0,
oXj
O'ij,j=O.
Here j is the dummy suffix implying summation, and the comma before j indicates
the derivative of each term with respect to xj .
It must be noted that Eq. (2.58) describes the variation of stresses within the
body volume and must be satisfied at every point within the body if the body is at
static equilibrium. If the stress distribution is homogeneous, Eq. (2.58) is
automatically satisfied since each derivative with respect to distance is identically
equal to zero.
If the volume element has a surface boundary, any surface forces will also
contribute to the force balance. A similar treatment for this case yields
(2.59 )
Here OJ is the unit vector in the Xj direction on the boundary and Fi is the applied
force in the Xi direction. If the surface has no applied tractions, i.e., it is a free
surface, Eq. (2.59) becomes
(2.60)
Equations (2.59) , (2.60) describe the boundary conditions for the stress
distribution existing within the material required for equilibrium.
(2.61 )
t ij ="2 (Ui,j+Uj,i) ,
03 U1
ox~ = oX 1ox~ ,
02t 22
03 U2
oxi
ox 20xi '
02t 12
03 U!
03 U2
+ ox 2 0xi
thus:
(2.62 )
39
OX Zox 3 =
1 0 {
2 oX I
Oe23
- oX I
Oe13
oX z
Oe12 }
oX 3
(2.63 )
Four other equations similar to Eqs. (2.62) and (2.63) may be obtained through
the cyclic permutation of the suffixes in these equations. Written in the suffix
notation the compatibility conditions are expressed as
epkjeqljeij,kl = 0 ,
(2.64 )
40
The actual flow curves for ductile materials shown above are hard to model
mathematically and can not be incorporated easily in plasticity theories. Instead,
idealized flow curves which simplify the mathematics without deviating too much
from physicaf'reality, are usually used. The flow curve for rigid, perfectly plastic
material, which does not deform elastically but starts to flow plastically at a
constant stress, is shown in Fig.2.17a. Another variation of this model is the
perfectly plastic material with an initial elastic region (Fig. 2.17b ). Strain
hardening (increase in stress with increasing plastic deformation) materials are
often modeled by the piecewise linear flow curve shown in Fig.2.17c.
The stress and strain plotted in all of the flow curves shown above are the "true
stress" and "true strain". Due to the large deformations usually encountered in
plasticity these values are defined with respect to the instantaneous specimen
dimensions rather than the original specimen dimensions, as shown in
Eq. (2.1 ), (2.2) for the elastic loading regime.
True strain is defined as the sum of incremental strains over the total
deformation length:
E=
l:
j=l
Lj-L(i-l) = S dL =ln~.
Lj
Lo L
Lo
~ 1,
(2.65 )
true strain is equal to the strain given
c
Fig. 2.17 a-c. Various idealized flow curves. a Perfectly plastic material; b elasto-plastic material;
c elastic and linearly work-hardening plastic material
41
True stress at any time t is defined as the instantaneous load intensity which is
cr=F/A.
(2.66 )
Here F is the load and A is the actual load bearing area at time t.
It must be noted that the true strain at any time t contains plastic and elastic
components. For example, upon unloading from a point A (Fig. 2.18 ) on the flow
curve, with true strl;lin E 3 , the material unloads along a line (AA'), parallel to the
elastic region of the flow curve, to residual plastic strain E 2 The elastic strain
component at A is thus Ee = E3 - E2
-. .
42
.
....
A-
.. .
The slip plane and the slip direction together define the slip system. Depending
on the symmetry of the particular crystal under consideration, there may be a
number of equivalent slip systems. For example in FCC crystals the {111} planes
are the most densely populated planes, with the (110) directions the closest
packed directions in these planes. Since there are four sets of {Ill} planes in a unit
cell, each containing three (110) directions, there are 12 equivalent slip systems in
the FCC lattice. In the HCP lattice, On the other hand, the only high density plane
is the basal plane {0001} and the close packed directions within the basal plane are
the three (110) directions. Thus there are only three equivalent slip systems for
this lattice, unless slip occurs on other planes (as it sometimes does).
The slip system that will be activated during extemalloading depends on the
resolved shear stress on the equivalent slip systems. Slip begins when the shearing
stress on a particular slip system exceeds a critical value (Schmid's law) which is
called the critical resolved shear stress. For example, consider Fig. 2.21, where a
normal tensile load F is applied to a single crystal of cross sectional area Ao normal
to the load. The cross-sectional area A of a slip plane which is inclined at angle <I> to
the tensile axis is
(2.67)
A=Ao/cos <1>.
(J --
-.l..L
Slip Plane
------------ - - - - - -
---
(J--
IJ
Fig. 2.20. Schematic depiction of slip by movement of an edge dislocation, denoted by 1-, to the
material boundary
43
Slip Plane
Normal
Fig. 2.21. Relative orientations of the loading direction, slip plane and slip direction in a sample loaded in
uniaxial tension
If the slip direction in this plane makes an angle A with the load, the resolved load
for this direction is
P=POCOSA.
(2.68 )
(2.69 )
The geometric term cos <I>'cos Ais called the Schmid factor and is a maximum when
<I>=A=45. When <I> or A=900, there is no resolved shear stress on the slip plane
and thus no slip will take place on this particular plane.
Once plastic deformation by slip starts, it can proceed in two ways. The crystal
sections bounded by the slip planes may simply slide over each other without
changing their orientation with respect to the load axis (Fig. 2.22a ) . In a normal
tensile test however, such lateral movement is constrained by the grips applying
the load, and the slip planes rotate to accomodate these constraints, (a similar
process occurs also in a macroscopically homogeneous body subjected to complex
loading when its movement is restrained) . The planes near the grips also undergo
bending in addition to rotation (Fig. 2.22b). In both cases however, the
~
Twin plane
44
deformation distribution is inhomogeneous, with plastic deformation concentrated in certain regions in the crysta1.
Another process by which crystal deformation can take place is twinning. In
twinning, one section of the crystal deforms in a manner that brings it into mirror
or rotational symmetry with the rest of the crystal lattice (Fig. 2.23 ). Twinning
involves more types of atomic planes, compared to slip, and usually causes small
deformations. However, after twinning, a set of slip planes may be oriented
favorably with respect to the applied load, thus twinning may facilitate slip. The
plastic deformation distribution caused by twinning is also inhomogeneous.
45
Vi
~
ClI
.c
lfl
r.
and reflect the movement of a very small number of dislocations. The true elastic
limit is associated with the movement of a few hundred dislocations. Above this
value, a load-unload cycle produces a completely closed, parallelogram shaped
mechanical hysteresis loop (OABC in Fig. 2.24 where AB is arbitrarily small) at
the strain levels involved. The loop closes on itself (OADE) until the applied
stress reaches the anelastic limit ('tA)' Any further increase in stress results in an
open hysteresis loop, with some micro plastic deformation distributed in the
material. These values are especially important in applications like the manufacture of inertial navigation systems, etc., where no plastic deformation can be
tolerated.
A parameter more commonly used in engineering is the "yield strength" which
is the stress required to produce a specified amount of plastic deformation. The
amount of plastic deformation ( or offset) is usually specified at 0.002 inch/inch or
0.2 % strain) and the yield stress is taken as the stress at which a parallel drawn to
the elastic portion of the stress-strain curve from 0.2 % strain intersects the curve.
This value is also n;:ferred to as the "offset yield stress".
It must be emphasized that whenever the applied stress exceeds the "anelastic
limit" some plastic deformation occurs in the material, and such deformation is
usually inhomogeneously distributed for polycrystalline solids. Analysis of such
behaviour is possible by the extension of the theories treated so far into the micro
scale, where the interaction between regions of different properties is also taken
into account. These procedures will be treated in detail in Chap. 3.
Problems
2.1. The stress tensor in the
0" . .
1J
= (-500 -400
30
Sj
30) MPa.
200
46
a) Calculate the stress tensor in the L coordinate system if: cos - 1 a 33 = 45, and x~
is in the plane defined by X l ,X 2 and is rotated 60 counterclockwise from x2 .
b) Calculate the strain tensor for both coordinate systems, assuming an isotropic
Fe sample.
c) Calculate the principal stress tensor for this system.
2.2. Assume that the stress
crij= (
-400 0)
0 0 0 MPa
is applied in the [100] direction ofa Fe single crystal. Calculate the strain tensor in
the crystal axes.
Bibliography
L.H. Schwartz and J.B. Cohen, "Diffraction from Materials', Academic Press, New York, N.Y.,
1977
G.E. Dieter, "Mechanical Metallurgy", 2nd. ed., McGraw-Hill, New York, N.Y., 1976
T. Mura, "Micromechanics of Defects in Solids", Martinus Nijhoff Publishers, Hague, The
Netherlands, 1982
J.F. Nye, "Physical Properties of Crystals", Oxford University Press, Oxford, Great Britain,
1976
S.P. Timoshenko and N.J. Goodier, "Theory of Elasticity", 3rd. ed., McGraw-Hill, New York,
1970
3.1 Introduction
In one of the most comprehensive books on micro plasticity, Mura[1] defines
48
X2
Workpiece
Fig. 3.1. Schematic description of the normal shot-peening process
directions and of initial thickness to), and plastically deforming these layers
(Fig. 3.1 ). FOlt a homogeneous, isotropic material, peened with a large number of
shot impinging randomly on the surface, the plastic strain tensor e~ in the surface
layers will be
(3.1 )
The plastic strain component e~3 is produced due to the force exerted by the shot
at the time of impact in the X3 direction. Since the material is, in effect, compressed
in the X3 direction, plastic flow also occurs in the X I ,X 2 directions, and from
conservation of volume e~2 = ell = - e~3/2. Thus, the plastic deformation distribution in the plane of the surface is homogeneous, as expected from the symmetry
of the process causing the deformation.
The plastic strain terms ell,e~2 imply a length change in the surface layers, i.e.
if the surface layer, of initial length Lo and thickness t? (t? ~ to), could be
separated from the rest of the sample and shot peened, the final dimensions would
be
L'=Lo+Jel'ldx1 =Lo+oL
tl
= tl0 + JeP33 d x3 ,
(3.2 )
where it is assumed in this example that the plastic deformation at all depths in the
surface layer is constant.
This layer is now placed on the rest of the sample (the bulk), which has
suffered no plastic strains and is still oflength Lo. In order to match the dimensions
of the surface layer and the bulk, surface tractions F must be applied at the
boundaries (Fig. 3.2) which will elastically deform both the bulk and the surface
layer to a final length L, where L' > L > Lo (Fig. 3.2b ) . The tractions, F, will cause
macro residual stress fields of opposite signs in the surface and in the bulk volume.
49
Lo ... b L -
--I~
lt=
1 ====~I~
F ;-==~
t -11
- - L o-
,I
f--
-F
- - L - - - -.,
a
b
Fig. 3.2. Free-body deformation of the surface and bulk layers without mutual constraint (a),
and with mutual constraint (b) of a hypothetical shot-peened specimen
0'1
O~~----------------~
O~--~--------+-~
Fig. 3.3. Variation of the in-plane stress (cr 11) with depth (x 3 ) in a hypothetical specimen shotpeened on one side (a), and on both sides (b)
The magnitude of the macrostresses in the bulk and the surface can be calculated
from Hooke's law:
L
( all) s = Eln L'
L
(all h=E-ln Lo .
(3.3 )
The stress (all) s will be equal to (a 22) s due to the symmetry of deformation in
the plane of the surface. The stress distribution in the work piece after reattachment is shown in Fig. 3.3a. This stress distribution will produce a couple
which will cause bending of the specimen to a curvature co. This curvature is
proportional to the stresses in the volume and can be used to calculate the residual
stress value at the surface when the stress distribution is known. This concept
forms the basis of mechanical residual stress determination methods. If the plate is
shot peened with the same intensity on both faces, the stress distribution is
symmetric with respect to the central plane of the specimen (Fig. 3.3b ) . In this
case the stress distribution can be represented by two equal but opposite couples,
and the specimen remains flat.
50
E
o~----~-------------
I t,
I
I
0'11
I
I
I
I
I
O~--~I C=========~
Fig. 3.4. Variation of the in-plane plastic strain
( E) (a) and in-plane residual stress (b) with
depth in an actual specimen
b
51
~z
Us
cro) Tu
(a-o)2(crr )Sh ..
b2 -a 2
(1 + r
b2)
2
(3.5b)
in the tube. (The detailed solution for this case may be obtained from any book on
elasticity theory, for example see Timoshenko [2J, pp 65 - 75.) It may be noted
that, in contrast to the shot-peening case, in which no stress component in the
direction of the surface normal occurs, the shrink-fitting has such a component
( crr ) , which decays to zero at the surface where r = b, and thus exists as a gradient
with depth.
52
In addition to Eq. (3.5) the macrostresses at a point must obey the differential
equations of equilibrium given in Sect. 2.10:
O"ijnj=Fi
(3.7a)
O"ij,j=O.
(3.7b)
ox!
+ 00"23 + 00"33
oX 2
oX 3
=0
(3.9 )
since the terms 00"13/0Xl' 00"23/0X2 are zero, the term 00"33/0X3' which describes
the variation of 0"33 with depth is zero. Thus the value of 0"33 at any depth is equal
to its value at the surface, which, as shown before, is zero.
In the case of shrink-fitting a tube on a solid shaft there is a stress gradient
along the radial direction, even though the stress at the surface is zero. The
tangential and radial stresses caused by the shrink-fitting operation also obey the
equations of equilibrium (3.7a,b). This can be easily seen by writing the force
balance in cylindrical coordinates [2] and is left to the reader as an exercise,
3.4
~crostresses
It can be seen from the discussion given above that macrostresses are homog-
eneous on a macroscopic scale along at least one direction. For example, the radial
stress for the shrink fitted tube at any depth is independent of e. For the case of
shot-peening discussed before, the stress 0" 1 1 is independent of Xl ,x 2 and depends
only on x3 . Microstresses are, however, usually inhomogeneous on a macroscopic
scale and may also be inhomogeneous on a microscopic scale as well, such that the
components of the microstress tensor are different at all points in the material
volume. These stresses may arise from a number of causes. The inhomogeneous
distribution of plastic deformation on a micro scale, such as the partitioning of
plastic deformation between the matrix and precipitates of a two phase alloy,
causes a microstress field in and around each precipitate. This case may be
visualized as follows. Assume that initially there are no stresses of any kind in the
uu o o
3.4 Microstresses
01
Ie>
~
ol
a
53
Fig.3.6a-c. Formation of microstresses due to inhomogeneous partitioning of plastic strains in a twophase body
material volume. ' If a precipitate could be removed from the material without
disturbing its surroundings, the dimensions ofthe precipitate and the void which it
leaves behind in the matrix would be identical. However, since the yield points of
the matrix and the precipitate are different, a given applied stress will cause
different plastic deformation in the precipitate and the matrix. This means that
after plastic deformation, the dimensions of the precipitate and the void are no
longer identical. In order to insert the precipitate into the void, tractions must be
applied to the boundary of the void and the precipitate such that they match each
other at all points (Fig. 3.6). These tractions will cause a microstress field in and
around each precipitate. Such microstresses will be referred to here as "microstresses due to differential plastic deformation". An inhomogeneous distribution
of elastic constants in the material volume may also cause formation of
microstress fields when a homogeneous stress is applied at the boundary of the
material. Consider, for example, a sample consisting of two contiguous grains
with different cryst~llographic directions (and hence elastic constants Sijkl ) along
a vector V across the grain boundary. This bi-crystal is subjected to the
homogeneous stress CJ 11 at the surface (Fig. 3.7). If these grains were subjected
separately to CJ l l on their boundaries, each would have a different strain
[Eq. (2.39) J, and ~ence different displacements [Eq. (2.2) ] along V. However,
in a solid body, the grains are in rigid contact and displacements across the grain
boundary must be constant in order to avoid having voids at the boundary.
Therefore, a microstress field arises which modifies the applied stress and thus
constrains the displacements in the material surrounding the grain boundary.
Such microstresses are called "microstresses due to elastic incompatibility".
0'1
~~o,
V
1
<J
_8
I)
54
(3.7b)
55
where D is the total volume of the body. It must be emphasized that this equation
is valid if and only if Eqs. (3.7a,b) are satisfied, as is shown below. Rewriting
Eq. (3.11a):
(3.11b)
( Ojk = Xj,k, since oxiox = 1 for i = j and = 0 otherwise)
Integrating (3.11 b) by parts 1, with "xt the coordinate in the j direction:
J O"ijdD = J O"ikxjnkds - J O"ik,kxjdD = 0 .
D
I~
(3.12 )
The first integral on the right-hand side is over the boundary of the body ID I, where
O"iknk=O [Eq. (3.10)], and the second integral on the right-hand side, evaluated
in the volume, is zero as O"ik,k=O [Eq. (3.7b)].
For a two-phase material Eq. (3.11) can be written as
J O"ijdD =
D
D-Q
O"ijdD + J O"ijdD = 0,
n
(3.13a)
(3.13b)
or,
(3.13c)
where the carats "( )" imply averages over the appropriate volume. Multiplying
both sides of Eq. (3.13c) by liD:
(3.14a)
Here f is the volume fraction of the second phase, and (O"ij)m, (O"i)ppt. are the
average stresses (PM stresses) in the matrix and precipitates (second phase)
respectively.
.
For a multi-phase material a similar derivation yields:
N
L f;"( O"ij)i = 0
i= 1
(3.14b)
where N is the number of phases, fi is the volume fraction of the ith phase which
has the average stress (O"i)i' It can be seen from the above discussion that when
the PM stresses obey Eqs. (3.14a) or (3.14b), the actual stress distribution at all
points in the body volume obeys the differential equations of equilibrium
(3.7a,b). Thus, even though 0"33 can not exist as a macrostress gradient in the near
surface regions of a shot-peened homogeneous material [Sect. 3.2, Eq. (3.9)],
0"33' as well as 0" 13,0"23 can exist as pseudo-macro stress gradients in a shot-peened
two-phase material. In this case, the gradient for each PM stress component
(0"33),(0"13),(0"23) is balanced in the grains of the respective phases In
1 Integration by parts utilizes the formula Judv=uv-Jvdu, where u,v are functions in x.
56
accordance with Eq. (3.14). (The shear components will be especially important
if peening is not normal to the part. An example of this is given in Chap. 7,
Example 7.7.)
57
7-5v
Sl1l1 =S2222 =S3333 ~ 15( 1-v)
5v-1
S1122 =S2233 =S3311 =S1133 =S2211 =S3322 = 15( 1-v)
4-5v
S1212=S2323=S3131 = 15( 1-v)
all other Sijkl =0.
b Penny Shape (a l = a 2 ~ a3 )
1-2v 1t a 3
13-Sv a3
Sl111 =S2222= 32(1-v) 1t ai' S3333=1----1-v 4 a l
Sv-1
a3
2v-1
a3
Sl122=S2211 = 32(1-v)1t al , S1133=S2233=S(1_v)1t al ,
7-Sva3
1(
V-21ta3 )
S1212= 32(1-v) 1t ai', S1313=S2323= 2 1 + 1-v"4 a l '
1 - 2v 1t a3
Skkl1 = Skk22 = -1-- -4 -val
+1 ()'
-v
1 - 2v 1t a 3
Skk33 = 1 - -1-- -2 -val
inclusion-matrix interface will cause a stress disturbance at all points within the
material volume such that the stress at any point in the matrix will be
(3.16)
where (Jij is the stress caused by the elastic incompatibility, egl is the homogeneous
strain that would occur in the matrix with elastic constants Cijkl if no
58
incompatibility was present and Ekl is the elastic strain due to O'ij.1t can be seen that
Eq. (3.16) is simply Hooke's law written for the matrix. Similarly Hooke's law for
the precipitate is
(3.17 )
where the terms are similar to the ones for the matrix but are defined for the
inclusion with elastic constants C;jkl'
The stress/strain values for this problem may be solved through the equivalent
inclusion method of Eshelby [5]. In this method the goal is to transform the
problem into the eigenstrain problem for a homogeneous material where both the
matrix and the inclusion have the same elastic constants C jjkb and then solve it
using the procedure discussed above. Eshelby showed that this is possible by
proving that a fictitious homogeneous inclusion having the same elastic constants
C jjk1 as the matrix will be equivalent to the actual (inhomogeneous) inclusion
when the equation
(3.18 )
is satisfied in the inclusion volume. In this equation the right-hand side is the stress
for the fictitious equivalent inclusion and E;j are the inelastic strains (eigenstrains)
that must be introduced in a homogeneous inclusion of the same shape and size as
the actual inclusion such that the equivalency is satisfied. It must be noted that
such equivalency cannot be achieved if elastic strains are introduced instead of E;j
since this would change the overall stress state through Hooke's law.
Substituting (3.15) into (3.18):
(3.19)
which may be solved for the unknowns E;j' Then Ejj is determined from (3.15) and
the stress state for the interior points obtained from Hooke's law (3.17). For
explicit solutions for a number of inclusion shapes and for solutions for exterior
points the reader is referred to the original papers by Eshelby [3,4,5] or to Mura
[1,pp 151-158].
59
(3.24 )
E~k}
(3.25 )
Here Jl,A,Jl' and A' are the shear modulus and Lame' constants of the matrix and
the precipitate respectively.
Equation (3.25) can be expressed in a more useful form by defining the
deviatoric components of the strains contributing to it:
'0
s: 0
eij
= ei. - uije
kk /3
( 3.26)
60
' - eij
'p} = 211 {'O
' - eij
,..}
2 11*{'O
eij + eij
eij + eij
(3.27 a)
K* {e~k+ekk-e~k} =K{e~k+ekk-e;k}'
(3.27b)
where K" and K are the bulk moduli of the precipitate and matrix respectively
[K = (211 + 31..) /3].
For shear strains (i =F j), Eqs. (3.27) become
(3.28 )
since all oij = 0 for this case.
The unknowns eij,e~ can be expressed in terms of each other by the property
(3.29)
where Sijkl is the Eshelby tensor components associated with the precipitate shape.
From Eqs. (3.28) and (3.29) (expressing e;; in terms of eij' where i =F j, and
noting that the terms Siiik,Siikl are zero):
.. _ {2(1l-1l*)e?j+21l*e~}!, .4-.
eij- {4( *_)
2} 10rl,J.
11 11 Sijij + 11
(3.30 )
=0.
(3.31 )
IJ
IJ
e=e
21l*f( 1- 2Sijij )
*
4(1l-Il)sijij+21l-f(1-2sijij)(21l-1l*)
lor I=FJ.
(3.33 )
<(J'ij)m = 2Ile~,
i =F j .
(3.34 )
Here e~ is given by Eq. (3.33). The PM shear stresses in the precipitate are then
obtained from Eq. (3.14).
Unfortunately, the solution for the normal stresses (i=j) is much harder:
Equations (3.26) and (3.29) yield three equations in the six unknowns e~ and e;;
(for i = j ). Another three equations between e~ and e;; are obtained from the
equilibrium equation (3.14). Then e~,e~ can be obtained from the simultaneous
solution of these six equations. Since the terms in the equations are too long and
cumbersome to express in closed form, explicit solutions for e~ are not given here.
61
However, it can be seen by inspection of Eqs. (3.33) - (3.37) that these strains
will be functions of the plastic strain E~ in the direction xj, the total plastic strain
E~k and the Eshelby tensors Sijkl associated with the shape of the second phase
particles. Once the eS are determined, the PM stresses O"ij) in the matrix can be
evaluated from Hooke's law. The stresses in the precipitate can then be obtained
from Eq. (3.14).
In this procedure the interaction between the stress fields around individual
inclusions was not taken into account. This approximation is valid for f ~ 1. For
large f, the solution will follow along the same lines. However, an average
interaction term will also contribute to the PM stresses. If the surface is near the
region of the calculation, a surface effect term (similar to the "image stress"
associated with dislocations) is also needed. These effects are complicated and will
not be treated here. However, the PM stress contributions from both of these
effects will obey the equation of equilibrium (3.14).
When an external load is applied to an inhomogeneous two-phase material
(i.e. the elastic constants of the second phase are different than those of the
matrix) which already has nonelastic strains (eigenstrains) in the second phase
grains, the PM stress tensor will have components from both types of microstresses. A procedure similar to the ones discussed above can be used to determine
the PM stresses in the matrix and precipitates (second phase particles) for this
problem. Writing. Hooke's law for the matrix and the precipitates:
<
(3.35 )
Here O"ij is the residual stress created due to the differential plastic deformation
plus the elastic incompatibility. The other terms are equivalent to those discussed
in Eq. (3.16).
To solve Eq. (3.35) one can use the equivalent inclusion method discussed
above. For the actual derivation and discussion on a number of precipitate shapes
the reader is referred to Mura [l,pp 151-168,334-342].
(3.36)
62
where (O'ij) DPD are the microstresses due to differential plastic deformation
between the matrix and the precipitates, (O'~) is the macrostress which will form
due to the constraining effect of the bulk material which has suffered no plastic
deformation [the effect of the bulk can be represented by the appropriate
tractions F acting on the boundary of the surface layer (Fig. 3.2)], and ( O'ij )EI are
the microstresses due to elastic incompatibility which are caused by the tractions,
F i, imposed by the bulk on the surface layers. The terms (O'ij )INT> (O'ij )SE describe
the microstresses due to the interaction of the elastic fields of the precipitates, (this
term is zero for f ~ 1. ) , and the microstresses due to the presence of a free surface
respectively.
The stresses measured in the surface layers from a given phase will then be
<O'ij)t=O'~+ O'ij)
(3.37)
where the terms are volume averages of the stresses contributing to Eq. (3.36).
It must be noted that the equations of equilibrium applicable to the terms
contributing to the total average stress are different. For the PM components
<(O'ij), Eqs. (3.14) apply individually or in total, whereas for the macro-stress
component, the~equations of equilibrium are
Here F are the tractions imposed by the bulk on the surface layers as discussed
before.
The stress state in the bulk is simpler. There will be no microstresses due to
differential plastic deformation between the phases (since the bulk suffers no
plastic deformation at all) , and the surface effect term (O'ij) SE may be neglected.
However, the other two components contributing to the total stress tensor at a
point will be finite.
63
a
b
Fig. 3.10. Distribution of elastic constants in the volume of a piecewise homogeneous body (a),
and an inhomogeneous body (b)
(3.38)
Here y is the engineering shear strain [Eq. (2.36)] and D-v is the average shear
modulus in the Voigt limit.
For a piecewise isotropic multi-phase material, the average shear modulus is
defined as
D
D-v=
L filli
i=O
(3.39)
1 The methods of Z. Hashin and S. Shtrikman (J. Mech. Phys. Solids 10, 343 (1962); 11,
127 ( 1963) ) which are based on a variational principle, generally yield better upper and lower
bounds for the elastic moduli than the Voigt and Reuss limits. These calculations are
complicated however, and are beyond the scope of this book. The reader is referred to M ura [1]
for a review of these methods and their extensions.
64
Here Il; is the shear modulus of the ith phase which has a volume fraction f; in the
material.
For a material composed of anisotropic single crystals with elastic moduli
Cijkl' the average elastic moduli C;jkl can be calculated in a similar manner. In this
case the average stress is related to the uniform strain through the generalized
Hooke's law. For example, the average stress for the shear strain S~2 is
( 3.40)
Here D is the volume of the material and the average elastic constant
the Voigt limit is given by
n
(C 1212 )y=
;=0
fdC 1212 );
J C 12dD in
D
(3.41 )
Here (C 1212 );, the elastic modulus of the ith crystal, is referred to the same set of
axes in which S~2 is measured.
Calculation of the bulk modulus is similar: Consider the case where a
hydrostatic stress O'H is applied to the boundary of a material consisting of i
discrete phases and the matrix. In this case the Voigt limit assumes that all
elements of the solid have the same dilatation sa. The average hydrostatic stress
within the body is then evaluated from
n
crH = ;=0
L r;K;"sa
(3.42 )
Kv= L
;=0
f;"K;.
(3.43 )
0'
s~; JCjjjjdD.
= 3"1 JD O'jjdD = 9"
(3.45 )
Cjjjj is an invariant tensor quantity within the volume (Nye [15] ,p 146). Thus
Eq. (3.45) becomes
_
0' =
9" CjjjjSjj
(3.46 )
65
from which the average bulk modulus of the polycrystal in the Voigt limit is found
as
(3.47 )
Expanding Eq. (3.47):
9Kv= {Cllll +C 2222 +C 3333 } +2{C 1212 +C 2233 +C 3311 }
(3.48 )
1
C44 =-s
44
(3.53 )
Poisson's ratio v and Young's modulus E can be evaluated from Eq. (3.50) and
(3.51) using the formulae
K=
3 (1-2v)
(3.54 )
66
the average shear strain is related to this uniform shear stress through an equation
of the form
(3.55 )
Thus, the average shear modulus in the Reuss limit is
ilR =
.L
,=0
fJlli
)-1
(3.56 )
IlR
(3.58b)
ilR
~ {(8
11
:28 12 ) } =
~ (C
ll
+2C12 ) =Kv
( 3.59a)
(3.59b)
It must be noted that the fundamental assumption in the Reuss model, that
stress is constant over the total volume of the polycrystalline body, does not satisfy
compatibility at the grain boundaries, in that two points on either side of a grain
boundary between grains of different orientation would suffer different displacements due to the different respective strains given by Hooke's law.
stress on their surfaces, both the stress and strain vary from point to point in the
material volume due to the inhomogeneous distribution of elastic constants along
any given direction, as discussed in Sect. 3.8. The actual stress at a point in such
materials will be affected by the shape of the precipitates (through the
components of Eshelby's tensor Sijkl), and the actual distribution of elastic
67
constants in the composite elements around the point. Thus, the average elastic
moduli linking stress to strain at a point for such a material contain components
from these effects in addition to the elastic moduli Cjjkl,Sjjkl. The effect of such
parameters was determined by Eshelby [3,4,5] through the use of the equivalent
inclusion method (Sect. 3.6) . For the case of a piecewise homogeneous composite
material, with n elliptical inclusions, each with elastic constants (C jjkl ) and
volume fraction fj, where fj is very small compared to the volume fraction of the
matrix fo, the average shear modulus linking the shear stress a jj to shear strain Ejj is
( 3.60)
where Sjjjj is the appropriate Eshelby tensor component and Jlo is the shear
modulus of the matrix. Similarly, the average bulk modulus is given by
KE = Ko
(3.61 )
When the total volume fraction of inclusions becomes comparable to the volume
fraction of the matrix, or when a polycrystalline material is under analysis (in
which case the terms matrix and inclusions become vague) the interaction effects
among particles become more important and formulae (3.60), ( 3.61) can no
longer be used. For such cases the "self-consistent analysis", proposed first by
Kroner [13] may be utilized. Consider a given grain embedded in a random
polycrystalline aggregate subjected to a load on the material surface. The average
stress and strain in the material are crij and Eij respectively. The self-consistent
method assumes that the elastic response of the material surrounding the
crystallite can be represented by a homogeneous material with average elastic
constants (Cjjkl ) B, ( Sjjkl) B, equal to the average constants of the polycrystal. The
stress in the embedded crystal is directly proportional to the average strain
through an equation of the form
aij ( n) = (Cjjkl+ rjjkl ( n) ) Ekl .
(3.62 )
Similarly:
Eij (n) = (Sjjkl + tijkl (n) ) crkl
(3.63 )
Here CjjkbSjjkl are the elastic constants of the single crystal of volume n. The terms
rjjkl,tjjkl are tensors of the fourth rank which describe the interaction of the crystal
having a particular shape and orientation with the matrix. They are related to the
Eshelby tensor Sjjkb and have the same symmetry as C jjkl. If Eqs. (3.62), (3.63)
are integrated ove"r all possible orientations, the average values for the bulk should
be obtained:
crij = (Cjjkl ) BEkb Ejj = (Sjjkl) Bcrkl .
(3.64 )
Therefore:
JD rjjk1dD = JD tjjk1dD = 0 .
(3.65 )
68
For an anisotropic spherical crystal with cubic symmetry and elastic constants
C jjkl (0) in an isotropic medium, the following relations are given between
rjjkbtjjkl (Kroner [13]):
rjjkl (0) = (Cjjkl)B +Cjjmn (0) +umnkl (0)
tjjkl (0) =ujjmn (0) (Smnkl)B
(3.66)
5 K+3~K
4 K+6~K'
(3.67)
where K and ~K are the bulk and shear moduli of the matrix. Since for cubic
crystals K is equal to the single crystal bulk modulus [see the derivation for Kv
given in the V<Jigt assumption, Eq. (3.50)], it is known exactly. The average shear
modulus ~K can be obtained from the integration of Eq. (3.62) or (3.63).
In later work Kroner [14] derived the average elastic moduli of a perfectly
random composite material from the local elastic moduli using correlation
functions. For an aggregate of cubic crystals the K value is equal to that for the
single crystal, as discussed above. The shear and bulk moduli are given by
( 3.68a)
a
x
3K+6~v
3K+4~v
- 1(
KK=3
(3.68b)
1 )- -
=KR=Kv
This approach also yields values very close to the self-consistent method [for
example for Cu, the elastic constants calculated from formula (3.68a,b) are
within 1.1 % of the values calculated from the self-consistent method].
In Table 3.2 the bulk averages in the Voigt, Reuss approximations and mean of
Voigt and Reuss values, as well as experimentally determined elastic moduli of
various materia~s, are shown.
Based on these and other similar results, (the fact that the measured values of
elastic moduli usually fall between the values calculated by the Voigt and Reuss
assumptions was first pointed out by Neerfeld [16] in 1942), the arithmetic mean
of the Reuss and Voigt values are frequently used as bulk elastic constants in
practical stress analysis when experimentally determined values, or means of
69
Table 3.2. Average bulk elastic constants in the Voigt and Reuss limits calculated from
experimentally determined single crystal stiffness coefficients. Experimentally determined bulk
elastic constants and Hill averages
Material
AI
Cu
Au
Fe
Material
Al
Cu
Au
Fe
C l2
C44
'J.lR
fJ.v
10.8
10.7
18.6
23.7
6.22
12.3
15.7
14.1
2.84
7.5
42
11.6
26
26
54
31
89
40
24
74
Experimental values
'K
.&t
.liy
'va
Vv
78
139
167
173
71
109
69
193
71
144
87
229
0.349
0.369
0.431
0.313
0.348
0.328
0.413
0.280
GPa
Hill Averages
il
ilH
KH
vH
26.5
74
133
166
159
71
118
79
207
0.34
0.35
0.42
0.285
26
47
27.5
81.5
78
139
167
173
71
127
78
211
0.349
0.349
0.422
0.297
43.6~
27.8
80.8
complicated modeling, are not available. (Measured x-ray values are given in
Appendix F.)
All of the analyses treated above have assumed a random distribution of
elements in the composite and polycrystalline bodies. This assumption is not
always justified in practice, in textured materials for example. Further extensions
of these procedures as well as other methods have been proposed for such cases.
However, a general theory applicable to all cases is still lacking.
70
extension of the self-consistent method was given by Bollenrath et al. [19J. In the
following these results are reviewed.
Since the Voigt method assumes constant strain in all grains, regardless of
orientation, the directional restraint imposed by the diffraction condition does not
affect this model. Thus, the average values obtained from the treatment in
Sect. 3.9, [Eqs. (3.50), (3.51 ) J are used without modification. Expressed in terms
of (1 +v) IE, -viE, which are termed "x-ray elastic constants", since they appear
in the fundamental x-ray stress equation (given in Chap. 4) , the Voigt values are
( 1 +v) = 10S 1212 (Sl1l1 -S1212)
v
3S 1111 -3S 1122 +4S 1212
E
So' (Sl1l1 + 2S 1122 ) + 10S1122,S1212
3S 1111 - 3S 1122 + 4S 1212
(3.69a)
(3.69b)
where
(3.69c)
The Reuss model, on the other hand, assumes constant stress. This means that
grains with different crystallographic directions along the stress axis suffer
different strains, since the elastic modulus along the stress direction is not the same
due to elastic anisotropy. Similarly, the average elastic constants obtained from
grains of a particular orientation will not be equal to those obtained from grains
with a different orientation. This effect necessitates modification of the Reuss
treatment given by Eqs. (3.58a,b) such that the averages are taken over only
certain directions.
For a flat specimen in the normal position on a diffractometer only those
grains which have (hkl) planes with normals in the direction of the surface
normal S3 can satisfy the diffraction condition (Fig. 3.11 ). Thus the average
strain is obtained from
( 3.70)
where do is the unstressed lattice spacing, and d, the lattice spacing of planes
parallel to the surface, is along the S3 direction. This strain is related to the stress
O'jj in Sj by HObke's law:
(3.71 )
where compliances S~3kl are referred to Sj'
The relationship between the true elastic compliances, which are referred to the
axes Cj of the unit cube of the crystal, and the elastic compliances S~3kl is given by
the fourth rank tensor transformation equation
(3.72 )
where aij are the direction cosines between the two sets of axes. The relative
orientations of the two sets are defined by the one direction which is given in both
71
[hkt]
Fig. 3.11. Definition of the measurement axis for a nat specimen in the
normal focus ing position on a
diffractometer
5,
1 ---
[hk ll
531
I
I
I
I
c,
Fig. 3.12. Relative orientations of the measurement and crystal axes in an x-ray
experiment
sets. This is the surface normal Sj, which is also the normal to the diffracting planes
(hkl) , and is thus a crystallographic direction (Fig. 3.12). It must be noted that
the orientation of C j with respect to Sj is not uniquely determined by the
coincidence of S3 with a lattice direction. The entire set of axes C j can be rotated
around S3 to any arbitrary orientation without violating this condition. Thus, in
order to obtain the average value of S;jkl along Sj, the average of all possible
rotations must be considered.
F or cubic crystals, where the normal to the plane (hkl) is the direction [hkl] ,
the direction cosines between Sj and C j can be written in terms of the indices h,k,l,
since h,k,l are the coordinates of a point on the vector rhkl> connecting this point to
the origin. Thus, writing all components of aij in terms ofh,k,l and then taking the
average of Eq. (3.72) for all possible rotations of C j around <hkl), the Reuss
averages for the elastic constants can be shown to be
( - ; ) R =Sl122 =sor
(3.73a)
(El+V)
(3.73b)
R =SIIII
72
(3.74a)
to=t3333-t3311-2t3131
Here (SjjkdB':are the average bulk values and are given by
1)
1 (1
(S331dB= 3 3KK - 2JlK
1
(3.74b)
(3.74c)
The average shear modulus ilK and average bulk modulus KK in the Kroner limit
are given by Eqs. (3.68a,b) respectively. For single-phase polycrystalline
materials with random grain orientations, the interaction tensor components
t 3333 , t 3311 , t 3131 are given by
(3.75)
1
where t3311 =t 3131 = - 2t3333' and Sjjkl(Q) are the single-crystal elastic
constants.
Of the three approaches discussed above, the average diffraction constants
calculated in the Kroner limit are closest to experimentally determined values. The
median of the Voigt and Reuss values (the Neerfeld-Hilllimit) is also close to the
Kroner limit, and can also be used in practice. For example, for the 211,310
reflections usually employed in residual stress determination in iron or steels, the
mean values are within 5 % of the Kroner values. All of the approaches discussed
above break down however, when non-random orientation distributions
(texture) exist within a material. X-ray elastic constants also exhibit variations
with plastic deformation in certain cases; thus it is usually safer to use
experimentally determined elastic constants. The experimental determination of
elastic constants with diffraction methods will be discussed in detail in Chap. 5.
Some typical values are given in Appendix F.
References
73
Summary
Inhomogeneous partitioning of inelastic strains (such as plastic or transformation strains) over macroscopic volumes of a given specimen causes the formation
of residual macrostresses. These stresses arise due to the mutual constraint of such
regions. Macrostresses are homogeneous over macroscopic dimensions that are
larger than the grain size of a common engineering material.
Residual microstresses may be caused by inhomogeneous partitioning of
plastic deformation on a micro scale (microstresses due to differential plastic
deformation) or, in the presence of an applied load, by inhomogeneous
partitioning of elastic constants on a micro scale (microstresses due to elastic
incompatibility). These stresses are distributed inhomogeneously on a macro
scale.
Pseudo-macro residual stresses are the average microstresses where the
average is taken over a statistically representative volume. As long as external
parameters (such as the deformation distribution and/or the applied load) are
constant in the ~aterial volume, the PM stress is independent of the position of
the averaging volume.
Macro- and micro residual stresses must obey the equations of equilibrium at a
point (3.7). PM stresses on the other hand obey the average equation of
equilibrium (3.14) when the stress values are determined from mutually-exclusive
subsets of the same volume such as matrix and precipitates.
Calculation of micro- and PM residual stresses are possible for elliptical
precipitates through the equivalent inclusion method of Eshelby. Such formulae
are generally too restrictive for real specimens with random precipitate shapes.
However, analysis of the solutions yields valuable information on the possible
contributions to the total residual stress tensor.
The macroscopic average elastic constants of a polycrystalline solid may be
calculated from the elastic constants of the constitutive single crystals using
various assumptions such as the Voigt limit (constant strain in all grains) , or the
Reuss limit (constant stress in all grains) . Hill and Neerfeld have shown that the
measured values ate very close to the mean of the Voigt and Reuss limits. The
Kroner calculations for anisotropic precipitates coupled to an isotropic matrix
also yield values close to this mean. The same approximation is also valid for the
average constants applicable to diffraction, which take into account the added
constraint imposed by the diffraction conditions. If there is preferred orientation,
none of these approaches may be valid.
References
2
3
74
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
4.1 Introduction
Diffraction methods of residual stress determination basically measure the angles
at which the maximum diffracted intensity occur when a crystalline sample is
irradiated with x-rays or neutrons. From these angles one then obtains the spacing
of the diffracting lattice planes by using Bragg's law. If the material is under load,
these values will be different than the unstressed plane spacing, and the difference
will be proportional to the stress acting on the planes. At this point one can use
elasticity theory, lis discussed in Chap. 2 and 3, to determine the stress (residual or
applied) acting on these planes. Thus, no matter how sophisticated the elasticity
analysis, the final stress results are only as good as the data supplied by the
diffraction methods.
In this chapter the theory and instrumentation for x-ray diffraction required in
residual stress determination will be discussed in detail. These concepts, along with
those discussed in Chaps. 2 and 3 will then be used in Chap. 5 to derive the
equations of residual stress analysis. In addition, the pertinent concepts for
neutron diffraction, which is also used in residual stress analysis, will be discussed
briefly. It must be noted, however, that even though the pertinent topics are
reviewed as completely as possible, the treatments given are by no means
exhaustive, and the reader is urged to consult the standard textbooks on the
subject, such as Cullity[l], Schwartz and Cohen [2] , Azaroff[3], Barrett and
Massalski [4], Klug and Alexander [5] and Bacon [6], when necessary.
76
on the fIlm due to the contrast produced by these features in the transmitted x-ray
intensity. Generally, features larger than a millimeter can be resolved, and the
technique is mainly used in (relatively) macroscopic defect studies, as well as in
medicine.
In 1912 von Laue established the electromagnetic wave nature of x-rays by
showing that they are diffracted by crystalline materials. These experiments
proved that the diffracting medium is, in fact, the periodic atomic structure of the
material, and that the wavelength of x-rays is of the same order as the lattice
spacing of materials. Further study by W. L. Bragg, who derived a simple, elegant
set of laws relating diffracting phenomena to crystal structure, facilitated the use
of x-ray diffraction in the study of the structure and behaviour of materials on a
very fine scale, on the order of the dimensions of the unit cell (10 - 7 mm).
lmv =eY,
(4.1 )
where m is the mass of the electron and v is its speed just before impact. For a given
voltage, Eq. (4.1) yields the maximum kinetic energy of the x-ray photons
produced during an impact in which the incoming electron loses all its kinetic
energy in a single collision. Using wave-particle duality, the energy of the x-ray
photon may be expressed as
(4.2)
eY =hc/A,
where A is the wavelength, h is Planck's constant and c is the velocity oflight. It can
be seen that a given acceleration voltage cannot produce x-ray radiation with
wavelengths shorter than a limiting value, the short-wavelength limit, \WL' From
Eqs. (4.1) and (4.2):
Amin = ASWL =
12.400
-Y-
(4.3 )
77
Intensity
Intensify
28
a
or
28-or
--?-
A~
A---
Fig. 4.1. Variation of intensity vs. acceleration voltage (a), or vs. filament current (b)
Here Y, the applied potential difference, is in practical units (volts). ASWL is calIed
the short-wavelength limit and represents the most energetic photons possible at a
given acceleration voltage. On the other hand, an incoming electron may not give
up alI of its energy with a single impact. In such a case only a portion of the total
energy is available for x-ray photons. These impacts cause producton of lower
energy (longer wavelength) x-rays. For a given voltage this effect causes the
presence of a continuous spectrum of wavelengths in the x-ray beam produced by
deceleration. This type of x-ray radiation is calIed polychromatic, white or
bremstrahlung (slowing down) radiation. In Fig. 4.1 a,b the intensity vs. wavelength plots are shown for an x-ray tube operated at various accelerating voltages
( a) and filament currents (b). Increasing the filament current simply increases
the total intensity at alI energy levels since the number of impinging electrons
increases. However, the energy distribution itself is a function of acceleration
voltage only and does not change with filament current.
In addition to these parameters the total x-ray intensity (the area under a
given curve in Fig. 4.1) is also dependent on the atomic number Z of the target
material:
(Icont.spect.dA)
cdZy n .
(4.4 )
A.SWL
Here i is the filament current, Y is the accelerating voltage and n varies between 1.5
and 2 for different targets.
78
: 4 1---+-II---lo-od-+--+--+----1
Q)
...=.
III
c:
Q)
C 2 I---++--++---."..~~-'k---+---I
:>.
~ I l---tH'--I----b-T--<.po~~~-I
I
SWL
O~~~~~~~~~-~-~
Wavelength (angstroms)
(4.5 )
where C and 0' are constants for a given transition and material. It can be seen
from Eq. (4.5) that characteristic radiation lines occur at wavelengths independent of the acceleration voltage. For these lines the x-ray intensity is proportional to
the filamentcuqent, i, and acceleration voltage, V, through an equation of the form
ICh. Rad = B+ (V - VChar. ) n ,
( 4.6)
where B is a constant and VChar. is the excitation voltage of the characteristic line.
The characteristic lines are named according to the primary excited shell and
the shell that supplies the electron required for the decay to the lower energy state.
For example, a Kline is produced when an electron is ejected from the K shell and
the L shell supplies the electron to it. The L shell however has two electrons with
different spins and depending on which electron is supplied one can have a Kcx 1 or
Kcx2 line. If the electron is supplied by the M shell the line is termed a KII line. In
Fig. 4.4 the relative position and intensities of these lines are shown schematically.
79
..!.. Imll
n
4
Ionization
Level
4s
3d
K -excltahon
L -excitation
3p
Ll[
Lm
2
2
Lx
3s
I
0
2p }
2s
is
L Shell
K Shell
II AK
u
.c
'-
c:
.9
E
.,~
EllA
<lIlA
'"
L"
'0 IIX- ~
Lm
'"'
c
II
II
Kil
emiSSion
L state (Lelectronremoved)
La
-'
AM
II AN
Q)
""
"''''
1M IMa
~
Fig. 4.3 a, b.
Electronic
transitions causing emission of characteristic radiation. a Electron energy
levels of Cu metal with associated
quantum numbers n,l,m. the arrows
indicate the direction of the electron
transition that causes the excitation
to a K state, L state etc., indicated
in b
It must be noted that if the electron beam can excite K characteristic radiation
it will also excite all the other, less energetic, lines. However usually the K lines are
used in x-ray diffraction because of their high penetration through air. For targets
with moderate atomic numbers, like CU,Fe,Cr, lower energy lines are strongly
attenuated in air through scattering and are usually not observed. There are,
I
................ .
Ka ,
Intensity
0.5 ................ .
0.16-0.25
Kp
28-
80
however, important L lines from targets like Pt,Au,W, etc. In fact, for these
elements they are the only lines produced by the usual voltages (20 - 60 kV)
encountered in standard diffraction units.
target
current
for
filament
gloss
to metal
seal
W filament
81
Energy (keV)
1016 . - . -_ _-----.1o
___----,-1_ _ _ _,.1---.,
6 pole
supercon. wiggler
_ - - __
/I.e
---- ----
'}/
/'
Arc source
X-roy ring
I
i
0,1
10
100
Wavelength (A)
tubes the maximum power is limited by the amount of heat that can be dissipated,
and is usually of the order of 1.5 - 3 kW. The direct beam intensity at the sample
for such tubes is around 109 counts per second. In rotating anode generators the
target is cylindrical in shape and is hollow. The coolant is circulated through this
interior cavity. During operation the target is rotated at high speed, such that the
beam impinges on new material all the time, facilitating much greater heat
dissipation. With these generators, beam currents of up to 2000 rnA, (compared to
40 - 60 rnA for sealed tubes) can be used, resulting in beam intensities around
10 10 cps at the sample. The targets for rotating anodes are demountable, so that
different anodes can be used to produce characteristic radiation at desired
wavelengths.
In synchrotron., radiation sources a packet of high energy electrons is
accelerated to speeds close to the speed of light in a circular "ring". The
centripetal acceleration due to the curvature of the path causes the electrons to
emit electromagnetic radiation. Depending on the energy of the electrons, and the
local radius of curv~ture at any point in the ring, the emitted radiation will have a
range of wavelengths, and thus will be essentially white radiation. It is also
possible to insert electromagnetic devices (undulators or wigglers) locally into
the ring, and thus enhance the production of a certain range of wavelengths. In
Fig. 4.6 the wavelengths and the intensity distribution that make up the white
radiation spectrum at the Brookhaven Synchrotron X-ray ring is shown. This
particular ring is 170 meters in circumference and operates at 2.5 Ge V stored
energy and 200 rnA. It can be seen that the x-ray intensities are much larger than
conventional sources. Also, in contrast to the tubes which produce high intensities
only at the characteristic wavelengths, synchrotron radiation has much higher
intensities over a large wavelength range, facilitating the selection and use of a
number of wavelengths during a given experiment.
82
dl
T = -~dz.
( 4.7)
Here I is the transmitted beam intensity, and (~), the proportionality constant, is
called the linear absorption coefficient. It is proportional to the density (Q) of the
absorber and is ll;sually listed in the tables as (~/Q). This ratio is called the mass
absorption coefficient. The term (~/Q) is a material property and is independent
of the phase Of the material (solid, liquid or gas). Mass absorption coefficients of
some elements are given in Table 4.1. It can be seen from this table and Eq. (4.7)
that the incident beam is attenuated typically to 1/1001h of its value in the first 20
microns of a solid sample. Tabulated values of ~/Q for various elements and
radiations are listed in the International Tables for X-ray Crystallography
[7,vo1.3].
For a homogeneous slab of finite thickness z Eq. (4.7) can be integrated to yield
( 4.8)
(~/Q)I=
L Wd~/Q)i'
i= 1
( 4.9)
Density
(gmjcm 3 )
Mo Kex
(1..=0.711
Aluminum
Iron
Nickel
Copper
Titanium
Chromium
2.70
7.87
8.90
8.96
4.54
7.19
5.30
38.3
47.7
49.7
23.7
30.4
A)
Cu Kex
(1..= 1.542
48.7
324
49.3
52.7
204
259
A)
Co Kex
(1..= 1.790
73.4
59.5
75.1
79.8
304
392
A)
Cr Kex
(1..=2.290
149
115
145
154
603
89.9
A)
Kedge
t:. edges
83
A-
absorption. In this process the incoming x-ray photons are active enough to eject
electrons in the electron shells around the nucleus. This causes the atom to be
excited to an activated state, and it decays to the ground state by supplying an
electron from one of the higher energy electron shells, emitting characteristic xrays for the particular transition in the process. These characteristic x-rays are
identical to the x-rays produced by accelerated electrons as discussed in section
4-4. However, here they are caused by the incident x-ray beam and are called
fluorescent radiation. Similar to the accelerated electrons, the incoming x-ray
photons require ~ minimum energy before they can activate fluorescence.
For lower energies (longer wavelengths) attenuation is due, in large part, to
absorption processes involving scattering. As the energy increases to the minimum
energy for the excitation of K electrons for example, there is a sudden increase in
the beam attenuation. At this point true absorption, in addition to scattering
processes, is taking place, with the irradiated material producing K fluorescent
radiation, and there is a large increase in the absorption coefficient. This point is
called the K absorption edge. As the incident beam energy further increases, the
absorption coefficient gradually decreases. This is so since, even though scattering
and true absorption mechanisms are still operating, high energy x-ray photons
have a higher probability of passing unaffected through the material. The
variation of mass absorption coefficient with wavelength ( or energy) of incoming
x-rays is shown schematically in Fig. 4.7. Between the absorption edges, absorption depends on the atomic number Z of the material:
( 4.10)
84
28...,,-
28-
(Atomic no.)
( 42)
(30)
(29 )
(28 )
(27 )
(26 )
(25 )
(24 )
Filter
Niobium
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
Vanadium
(Atomic no.)
(41 )
( 29)
(28 )
(27 )
(26 )
(25 )
(24 )
(23 )
In Table 4.2 ftlters for some commonly used materials are shown. It may be
noted that for all cases, the atomic number of the filter material is 1 or 2 less than
that of the target metal.
Another important parameter in x-ray filters is the thickness of the filter foil.
Too thick a filter foil will cause unnecessary intensity loss. Usually foil thicknesses
that decrease the K~ to 1/5001h of its original intensity (which will reduce Kcx
intensity by 50 % ) are used in practice.
85
( 4.11 )
Here m is the electron mass, c is the speed of light and e is the electron charge. The
term r is the length of the position vector to P, and 29 is the angle between r and the
incident beam direction (Fig. 4.9). The term (1 +cos 2 29), which describes the
variation of scattered intensity with scattering angle is called the polarization
factor. It can be seen that, due to this term, the scattered intensity in the forward
(29 = 0 0 ) and backward (29 = 1800 ) directions will be stronger than directions
90 to the incident beam 1 .
Equation (4.11) gives the scattered intensity from a single electron. When, on
the other hand, the x-ray beam impinges on an atom, with atomic number Z, the
total scattered intensity to a point P in space will be slightly different. In this case
there will be Z electrons, and, therefore Z (scattered) beam sources at different
positions around the atom. Therefore Z rays, all with wavelength A. will arrive at a
point P away from the atom. However, the total scattered intensity at P, It, will
depend on the relative phases of the individual rays arriving at the point. If all the
beams are in phase [i.e., 29 = 0 in Eq. (4.11 ) for all the electrons in question] , the
It must be noted that this polarization factor is applicable only when the incident beam is
unpolarized. If the incident beam is polarized, as in the case of synchrotron radiation, there is
no polarization correction term to the scattered intensity. The beam may also be partially
polarized, if a single wavelength is chosen by, say, diffraction from a "monochromator"
( crystal) prior to impinging on the sample.
86
E
X1
Fig. 4.9. Geometry for the coherent scattering by a single electron to a point P
total intensity is Z2 '(le), where the intensity Ie is given by Eq. (4.11). For any
other direction, the beams from individual electrons will be out of phase by
various amounts and a certain amount of destructive interference will take place,
causing a reduction in the intensity scattered into non-zero 29 angles. It can be seen
that only coherent scattering, where all the beams have the same wavelength and
definite phase relationships with each other, can take part in this process.
Compton modified scattering, due to its random wavelength distribution and
arbitrary phase relationships, cannot take part in constructive or destructive
interference and contributes only to the overall background.
The term used to describe the total coherent scattering from an atom to a point
P is "r', the atomic scattering factor, which is defined as
f = amplitude of wave scattered by an atom
amplitude of wave scattered by an electron
( 4.12)
As indicated above, fis equal to Z at 29=0, and decreases with increasing 29. If
the total diffracted intensity at a point P is calculated, it is seen that f is, in fact, a
function of sin 9/1.., where 29 is the angle of scattering and Ais the wavelength of
the incident radiation. Further information, as well as tabulated values on the
atomic scattering factors of common ions can be obtained from the International
Tables for X-ray Crystallography [7, volume IV, pp 71-146].
87
each other if the path difference GEH between them is an integral multiple (n) of
the radiation wavelength A.. Since
GE=EH=dsin9.
Constructive interference, that is, diffraction will occur when
nA.=2d sin 9.
(4.13 )
Equation (4.13) was first derived by British scientist W. L. Bragg in 1912, and is
called Bragg's laW:
In the case of an actual three-dimensional crystal of finite dimensions, there
are a very large number of atomic planes. Thus there are, in fact, a large number of
mutually reinforcing beams causing appreciable (diffracted) x-ray intensity at
the correct angles. Along directions that do not satisfy Bragg's law, however, the
scattered waves are out of phase, resulting in destructive interference and no
diffracted intensity. In addition there will, of course, be background radiation at
all points, caused by inelastic (Compton) scattering and, if the incident beam is
sufficiently energetic, fluorescent radiation.
88
3'
,,
a
b
Fig. 4.11. a The unit cell of a body-centered crystal. b diffraction from the (100) planes of a body
centered cell
law is satisfied. Of course, total destructive interference is not always the outcome.
However, in general, the diffracted intensities vary considerably, depending on the
particular unit cell under consideration.
The total intensity diffracted by a given unit cell can be determined from the
summation of the waves from the individual atoms. If the scattering amplitude
atom, with fractional dimensionless coordinates Uj,Vj,Wj' is fj' the
from the
relative intensity scattered by the unit cell for a given reflection hkl is proportional
to
(4.14 )
Here the summation is over all the atoms present in the unit cell. The term Fhkl is
called the structure factor and represents the sum of the amplitudes and phase
differences of the waves scattered by the individual atoms. In general F is a
complex number, containing real and imaginary parts, and the magnitude of the
total scattered intensity is proportional to the square of the absolute value of F,
1F12. In Table 4.3, the structure factors for some simple Bravais lattice types are
summarized. The reader can derive these from Eq. (4.14).
From the discussion given above, it can be seen that when a perfectly
monochromatic, parallel beam of x-rays impinges on an infinite single crystal that
is perfect throughout its volume, diffraction can occur if and only if:
a) Bragg law 'nA. = 2d sin e is satisfied for one or more sets of crystallographic
planes (hkl),
Table 4.3. Structure factors and allowable reflections for selected lattices
Bravais
lattice
Structure factor
Reflections
present
Reflections
absent
Simple
Body-centered
Face centered
F=f
F=f( 1 +e'i(h+k+l
F= f( 1 +e'i(h+k) +e'i(h+l) +e'i(k+I
all
(h+k+l) even
h,k,l unmixed
none
(h+k+l) odd
h,k,l mixed
89
69
29
28--
b) The structure factors F for these hkl reflections are non-zero for the unit cell
of the particular crystal.
Under these conditions Bragg's law predicts that the variation of diffracted
intensity I with incidence angle 29 can be described by a step function (Fig. 4.12a ) .
However, the ideal conditions assumed in the derivation do not exist in reality. The
beams produced by x-ray tubes are polychromatic and even if a flltered
characteristic line is used, there is still some white radiation left in the beam and the
characteristic line itself has a range of wavelengths (about 0.001 A). Furthermore,
the beam contains parallel, divergent and convergent rays. The crystal itself is
rarely "perfect", but contains mosaic structure, that is, small regions within the
volume which are slightly misoriented with respect to each other. In addition the
size of the crystal is finite, and in some cases, very small. In certain cases, there can
be elastic strains and stresses distributed throughout the volume of the crystal. All
these effects cause "broadening" of the diffracted beam. That is, the diffracted
intensity is observed over a range of 29 (Fig. 4.12b ), with the maximum intensity
occuring at the exact Bragg angle. The width of the peak at half the maximum
intensity is proportional to the deviation of the experimental set-up and specimen
from ideality. Such broadening can be analyzed to yield information about the
mosaic size and strain distribution within the irradiated volume, and will be
treated in detail in Chap. 8.
90
4.12 Monochromators
The beam exiting from the traditional x-ray sources contain white and characteristic spectra, and synchrotron sources produce white radiation. In many
experiments, however, monochromatic radiation is required. This may be
achieved by passing the incident beam through a fIlter with the appropriate
absorbing edge, as discussed in Sect. 4.7. After fIltration KII intensities usually drop
to 1/500 of their initial value, while K", drops by 50 %.
Another way of obtaining a monochromatic beam is by scattering the incident
polychromatic beam from a set of lattice planes within a single crystal. Only one
wavelength will diffract. Such devices are called crystal monochromators. Since in
I
./
Dr/~3\!
"-
"
"-
"\
Fig. 4.13. Focusing monochromators in
a diffractometer in (a) back -reflection
and (b) transmission modes. In both
cases S is the x-ray source, PD is the
powder specimen and D is the detector
91
11
the monochromator the x-ray beams are attenuated through absorption and
scattering, the exit beam is substantially weaker than the incident beam. In some
applications monochromators are bent to focus x-rays (Fig.4.13), as this
increases the incident x-ray intensity on the specimen. Such set-ups are termed
"focusing monochromators". The diffracted beam from a crystal monochromator contains not only the primary diffracted wavelength ')., but also its
harmonics at ').,/2;:').,/4, etc. Various strategies can be employed to get rid of the
harmonics, and to increase the intensity of the diffracted beam. The reader is
referred to the standard textbooks on the subject for a detailed treatment.
One other effec;t arising from the use of a monochromator to filter the incident
beam is the change in the polarization correction. If the diffraction angle from the
monochromator is 29m (Fig. 4.14) the polarization factor for the beam diffracted
from the sample at an angle 29 is given by
( P F) = 1 + K cos 2 29
m
1 +cos 2 29 '
where K is equal to cos 2 29m for a perfect monochromator crystal, and Icos 29m I for
an imperfect one.
...
2r
d'
(4.15 )
The beam exiting from the target of an x-ray tube will be composed of rays from a
very large number of point sources. This beam will thus contain divergent,
92
------il
~~lL---
- - d - - - ------t
S ~=d~====----~~-
!-
- -- d
~w
convergent and parallel rays. The effect of the collimator discussed above on the
beam from such a source is shown in Fig. 4.16. The maximum angle of divergence
in this case is
A=
,...
4r
d'
(4.16 )
The beam will also contain convergent rays, with a maximum convergence
2r
cx= d+w .
( 4.17)
Line source
Soller plates
Tube
Fig. 4.17. a Soller slit geometry and its divergence limiting effect. b Use
of slits and soller slits to limit divergence of x-rays in two mutually
perpendicular planes
93
The pinhole collimators discussed above utilize very small apertures, causing a
large loss of incident beam intensity. In certain applications soller slits are used to
form a parallel beam. These devices are simply a number of thin foils placed
parallel to each other. The exiting beam is in the form of a line and contains mainly
rays parallel to the metal foils (Fig. 4.17). Thus, the divergence perpendicular to
the plane of the plane of the foils is, in large part, eliminated. The divergence
parallel to the plane of the soller foils may be limited by the use of rectangular
apertures which have their narrow dimension in the plane of the foils (Fig. 4.17b).
These apertures are called slits.
d'
(4.18 )
where r is the distance between the transmitted beam spot and the diffracted spot.
The plane spacing can then be determined from Bragg's law. If the crystal is now
rotated an angle <I> around the incident beam, while keeping the Bragg angle
constant, the diffracted spot on the fIlm will move on the circumference of a circle
of radius r, to a new position on the fIlm.
If, however, a polychromatic beam ofx-rays impinges on the crystal, there are
a number of wavelengths (with the shortest at AsWL ) available for diffraction. In
this case diffraction will occur for all the sets of planes which can satisfy Bragg's
law with one of the available wavelengths, resulting in a number of diffracted spots
on the fIlm. The Bragg angle for any of these spots is also given by Eq. (4.18). In
this case the wavelength of the diffracted beam is not known. However the pattern
Film
94
d---l
Fig. 4.19. Back-reflection Laue camera geometry
of spots on the fllm is related to the point group symmetry, and can be used in
some point group symmetry determinations. These patterns"are also valuable in
determining the orientation of a given face of the crystal. X-ray patterns of this
type are called Laue patterns, after von Laue who obtained the first pattern of this
kind in the first diffraction experiment ever performed. The particular geometry in
Fig. 4.18 is a iransmission Laue pattern. Laue patterns can also be taken in the
back-reflection mode. The geometry for this case is shown in Fig. 4.19. In this case,
the Bragg angle associated with any spot is given by
.
D '
( 4.19)
~----a
95
case the diffraction pattern emerging from the material for each (hkl) plane is in
the shape of a cone, with the specimen at the apex (Fig. 4.20). The intersection of
this intensity cone with the film plane causes a ring for a given family of planes,
{hkl}. (This case is equivalent to rotating a single crystal, diffracting at an angle
29 to a point P which is at a distance r from the transmitted beam, 3600 around the
axis defined by the incident beam while keeping the 29 constant. As noted before,
the diffraction spot will describe a continuous circle of radius r on the film.) These
patterns may also be obtained in the back-reflection geometry. In this case the
diffraction angle is related to the ring radius through Eq. (4.18). In both cases the
circles in such "pinhole" patterns are called Debye rings. From the radius of
Debye rings one can obtain the spacing of the diffraction planes through
Eqs. (4.18) or (4.19) and (4.13). The appearance of the rings also yields
information about the grain size in the material.
96
Source
28
28 + 268
+
focuSing
Fig, 4.22. Schematic of an x-ray
diffractometer
circle
used for residual stress measurements, as well as powder work is shown. The
geometry of such a diffractometer is shown schematically in Fig. 4.22. X-rays from
a tube (or any other source) impinge on the specimen which is on a holder
that can rotate around an axis (X) perpendicular to the plane of the diffractometer. The diffracted beam is then detected by a suitable detector, which can be
rotated around X, along the circumference of the diffractometer. The rotation of
the specimen holder and detector are through stepping motors and gear drives and
can be determined very accurately (0.005 to 0.00052e). Slits are mounted
in front of the tube and the detector, respectively, to collimate the beam
and define the tp.aximum "horizontal" divergent angles (i.e., in the diffractometer
plane) permissible in the incident and diffracted beams. Soller slits may also be
used in the incident and diffracted beam paths for better "vertical" collimation. In
this case the foils in the soller slits are parallel to the diffractometer plane.
During a normal run with a flat polycrystalline sample the detector is moved along
the diffractometer circle to detect the diffracted beam from the specimen. At the
same time the specimen holder is also rotated around X half the rotation angle of
the detector in order to maintain focusing, as is shown schematically in Fig. 4.23.
In this way, the divergence in the incident beam is made to converge or focus at the
receiving slit, because both sets of rays section equal arcs on the focusing circle.
The detection surface of a diffractometer, i.e., the surface the receiving slit
describes as it is rotated around the diffractometer center, is a cylindrical segment
of radius R (the diffractometer radius) and height I (the length of the receiving
slit). The detector in a diffractometer sees only the intersection of the diffracted
rays with this ~urface. The width of the receiving slit determines the accuracy with
which the diffracted intensity at any 2e position along the circumference of this
97
cylindrical segment is measured, while the area of the slit controls the total
intensity admitted into the detector.
Thus optimization of angular resolution with intensity usually results in a
rectangular slit (with its small dimension in the plane of the diffractometer circle)
which has a rather high aspect ratio (1/15-1/5).
The particular strategies for peak detection, slit arrangements and errors
caused by these will be discussed at length in Chap. 6.
d) Lorentz factor,
e) absorption factor,
f) temperature factor.
Of these, the structure factor and the polarization factor have been previously
discussed, and are given by equations (4.11) and (4.14) respectively. It may be
.'j
--
...
~
-
,--
98
4.18 Multiplicity
Multiplicity (p) is also an intrinsic property of the unit cell and the indices h,k,l of
the diffracting planes. This term describes the number of equivalent planes that
can diffract at a given Bragg angle, i.e., the members of a given form of planes
{hkl}. For example, for a cubic crystal all eight members of the {111} form have
the same d spacing (thus, Pill = 8) and any grains in which one of these planes
satisfy the Bragg conditions diffract at the same angle. By comparison there are
only six members of the {1 OO} form (p I 00 = 6 ). Thus, all other things being
equal, the diffracted intensity from the {1 oo} will be 3/4 of the diffracted intensity
from {111} planes.
Multiplicity is also a function of the unit cell of the crystal. For example, in a
tetragonal lattice (001) and (100) planes do not have the same spacing, and thus
can not diffract at the same Bragg angle, and do not really belong to the same
form (since they are not, in effect, equivalent planes). For this lattice PIOO =4,
and POOl =2.
99
with an area ofr082m [sin (90 -8)]. The fraction of the crystallites is the ratio
of this area to the total area of the sphere, 4m 2 :
AN
N =
( 4.20)
Thus the fraction of diffracting particles is proportional to cos 8 and is small for
large 8 (the back-reflection region).
The second factor, intensity per unit length of the diffraction cone, is
important because, as discussed before, in normal x-ray work only a small
segment of the intersection of the diffraction cone with the detection plane is used
in measuring intensities. However, since the radius of each cone is different, the
diffracted intensity into each unit length of the cone circumference is different. If
the radius of the diffractometer is R, the radius of the circumference of any
diffraction cone is 2nR sin 28. Thus, the diffracted intensity per unit length is
proportional to l/sin 28.
The third factor describes the variation of intensity with 28, when all other
factors are constant. It was previously shown that, when deviations from ideality
occur in the wavelength distribution of the x-ray beam, or in the degree of perfection
of the crystal, appreciable x-ray intensity is observed at angles 08 away from the
Bragg angle 8B, resillting in the broadening of the x-ray peak. Maximum intensity
on the other hand, occurs at 8B Thus, diffracted intensity is a function of 8.
9,
. \.
a
A. a
- Na- - -
Fig. 4.26 a,b. Scattering from planes that are inclined at angles 28 - 88. a Specimen geometry;
b geometry of the diffracting planes
100
(4.21 )
2a09 sin 9B ,
4.22 )
where, since 09 is small, sin 09 ~ 09. The phase difference between the rays
diffracted from the first and the Nth atom on the plane is
N09=N2a09sin 9B
(4.23)
':
A.
(09ho=o= 2Nasm
. 9B .
(4.24 )
At 09 less than this limiting value there will be some diffracted intensity, with the
maximum intensity at 09 = O. Thus the diffracted intensity varies as a function of
1/sin 9.
All the trigonometric terms discussed above can be combined to form a single
factor which describes the variation of intensity with angle 9. This factor is called
the Lorentz factor, and is given by
1
sm \J
L.F=K.~,
( 4.25)
where K is a constant. The Lorentz factor and the polarization factor are usually
combined together to form the L - P (Lorentz-polarization) factor:
(L.P.) = 1 ~:2S:29
( 4.26)
The constants from both terms have been dropped in this case since they are not
dependent on 9, and will not affect relative intensities. It may be noted that this
equation is valid only for an unpolarized incident beam. If an incident beam from
a monochromator is used in a particular experiment, the polarization factor for
this case, given in Sect. 4.12, should be used.
101
Fig. 4.27. The geometry of the specimen and the x-ray beams
for calculation of the absorption factor from a flat-plate
specimen in a diffractometer (a-goniometer)
diffractometer, (as given by Cullity [1 J , and Koistinen and Marburger [8J ), will
be treated, since this is the most common situation encountered in practice.
Consider the case where a beam of intensity 10 , of unit area in cross-section, is
incident on a flat plate at an angle (Fig. 4.27) . The total energy reaching a layer of
length 1and thickness dx, located at depth x below the surface, is proportional to al o
'e - IIAB because of absorption (here I.l. is the linear absorption coefficient of the
sample). The total energy diffracted by the layer is ablIoe - II AB dx, where a is the
volume fraction of crystallites that can diffract at this angle, and b is the fraction of
incident energy diffracted by unit volume. This diffracted intensity is also
attenuated by absorption along BC by a factor e- IIBC until it exits from the
material, thus the total diffracted intensity outside the specimen is given by
dID = albloe - II(AB + BC)dx .
(4.27)
smex
AB=-.-;
smex
thus,
dl D= (Ioab/sinex).ex
BC=~,
sm
smex
(4.28 )
sm p
In an experiment the angle 'l' can be measured conveniently. Thus, making the
substitutions
ex = e+ 'l';
= e- \jJ ,
J} 'dx
( 4.29)
102
ID=
x=o
dID,
I ab
(4.30)
Thus the angular dependence of absorption for this particular geometry is given
by the term (1 - tan 'V cot 9) which is called the absorption factor. We note that
for negative tilts (\jJ < 0) the factor becomes 1 - tan ( -ltVl) cot 9 = 1 + tanl'Vlcot 9.
Some examples of absorption calculations are given in Appendix E.
It can be seen from Eq. (4.30) that if the flat plate makes equal angles
with the incident and diffracted beams, i.e., 'V = 0, then the absorption factor is
equal to 1 for ~ll 9. This is the correct focusing configuration for diffractometers as
discussed before. Thus, there is no absorption correction for data obtained from a
29-9 run, where focusing is maintained. However, if 'V is non-zero, as during the
various tilts for a residual stress measurement, where the tilts are around the
diffractometer axis, a correction is necessary. The tilts required for residual
strain/stress determination can also be achieved by the geometry shown in
Fig. 4.28. This particular geometry is referred to as the 'V-goniometer. In this
geometry the tilts are around an axis parallel to the plane of the diffractometer and
the incident and diffracted beams have equal path lengths independent of the 'V-tilt
(i.e., in this case, the specimen behaves at all tilts as a flat plate in the correct
focusing condition since the 1:2 relationship between 9 and 29 is not affected by the
tilts). Thus, for this case, there is no absorption correction.
It may be noted that all the derivations so far have been based on flat
specimens. If the specimen surface has curvature, these formulae have to be re-
O-axis
~/-axis
(-
Incidence angle D
x- ray
source
103
evaluated in accordance with the specific geometry. Such curvature may also cause
other errors. These errors will be discussed in Chaps. 5 and 6.
104
Fig. 4.29. Typical electronics rack for an x-ray detector. a, High voltage supply for detector; b, preamplifier; c, SCA; d, timer/scaler; e, ratemeter; f,
chart-recorder; g, micro-processor for motor control
and data acquisition
set of electronics (Fig. 4.29) consists of a matched set of amplifiers (preamplifieramplifier) which amplify the output from the detector, a single channel analyzer
( SCA) 1 which discriminates on the basis of energy to reject unwanted radiation
(thus decreasing background), a timer/scaler which keeps count of the number of
incident photons (counts) per unit time, and a ratemeter that is an analog display
of the number of counts per second. The output from a ratemeter is usually fed
into an x-y recorder to obtain the variation of counts per second, cps, y with time
(x) . By synchronizing the x axis with the rotation of the detector, one can obtain
the cps vs. 29 plot which was previously shown in Fig. 4.24. Alternately the digital
output from the SCA can be interfaced with a computer for on-line processing of
the data. The detectors commonly used in x-ray diffraction work are discussed
below.
,
A proportional detector consists of a gas filled tubular metallic cathode with a
conducting wire (anode) running along the long axis in the center of the cylinder
(Fig. 4.30). During operation a high potential (800 -1200 V) is applied between
the anode and the cathode. X-rays photons entering the tube ionize the gas, with
the electrons moving quickly to the central wire and the positive gas ions moving
slowly to the cathode. During this motion, these ions collide with more gas atoms,.
In normal x-ray work a filter and an SCA are used together to achieve the maximum rejection of
unwanted energies. The filter is most effective in minimizing intensities from rays with energies
close to that of the primary wavelength used in the experiment (such as preferential absorption
ofK~ with respect to K.), while the SCA is used to minimize the background from wavelengths
further away in the energy spectrum.
105
level of detection
volts
time
causing further ionization. Thus, the amount of electrons (and ions) produced by
a single photon is amplified considerably (10 3 -10 5 ). This discharge produces a
current pulse, and momentary change in wire voltage, whose time duration can be
controlled by the composition of the gas in the counter. The quicker the pulse (i.e.
the discharge of the ions and electrons at the respective electrodes) , the smaller the
recovery time of the detector and the better the ability of the detector to detect high
count rates. In Fig. 4.31 the output of the detector in response to multiple pulses is
shown schematically.
Another feature of proportional counters is that the amplitude of the voltage
change in the wire is proportional to the energy of the incident photons. This
permits the use of pulse-height analyzers (PHA) which compare the amplitude of
the detector pulses to preset high and low voltage limits and record an event if, and
only if, the incoming pulse is in the interval. Thus only pulses within a given
wavelength band are recorded. This permits the rejection of unwanted radiation,
such as flourescence and white radiation, and also of the higher harmonics from a
crystal monochromator.
Depending on the type and resistivity of the wire used in a proportional
counter, it is possible to locate the position (along the wire) at which the photon
( or rather the ionization event caused by the photon) is detected. This is done by
measuring the relative time for the voltage pulse to reach the two ends of the
detector. A proportional counter used in this mode is called a position sensitive
detector (PSD). By curving the detector to fit the circle of the diffractometer, or
by using a short detector along a large diffractometer circle, it is possible to detect
the intensities over a range of two theta angles simultaneously, shortening
measurement times considerably. Such PSDs can achieve a spatial resolution
between 50-180 11m. Thus for a typical diffractometer radius of '" 15 cm, the
angular resolution is approximately 0.02 - 0.07 degrees two theta. (Another
interesting variation of this detector is the placement of PSD wires in a two
dimensional array. This set-up permits detection of diffraction spots referred to
two axes and, for e{(ample, may be used in real-time detection of Laue spots in a
camera.) Since the PSD substantially reduces the time necessary to record 20 vs.
diffracted intensity over a range of 20 (by a factor of ten in some cases), its
operation will be described in detail, following the summary given by James [9]:
In a PSD, the pulse on the anode wire can be used to determine the position of
the initial ionization (or the incidence position of the x-ray photon). There are
106
two methods that may be used to determine this position, utilizing the amplitude
or the rise time of the pulses occuring at two ends of the wire.
In the amplitude or current ratio method, a high resistance electrode is used. In
this mode the ends of the detector wire are effectively grounded and the charge
induced in the electrode leaks off to both ends. The sharing of the current i,
between the left (L) and right (R) flow directions is inversely proportional to the
resistive paths and, thus, directly related to the positions XR, XL:
here iL + iR = i and XR+ XL = Lo, which is the wire length. The position of incidence
is then determined by the use of a ratio circuit.
The rise time method utilizes the time difference between rise times exhibited at
each end ofth,.e anode in determining the position of the incident photon. The rise
time depends on the time constant RC, where R is the resistance along the anode
wire and C is the effective capacitance seen by the charge. For matched load
capacitance at each end of the wire, the time difference is directly related to the
resistance, and thus to the incidence position, if the distributed capacitance along
the wire is negligible. However, it has been shown that for such a design, a nonlinear region of position sensitivity exists within 20 % of the wire length from the
ends, which shortens the effective detector length by approximately 40 %. On the
other hand, rise time method allows the use of simpler (and cheaper) electronic
circuitry than that used for the current ratio method, with better angular
resolution. Thus, this method enjoys wider usage.
The basic circuit for a PSD utilizing the rise time technique for location of the
ionization event is shown in Fig. 4.32. The voltage sensitive preamplifiers are
located right next to the anode-cathode assembly (usually within the same box)
to reduce noise., The voltage induced at each preamplifier, Vo, is amplified further
in the main amplifiers. Shaping is accomplished by a double RC differentiating
and integrating circuit in the main amplifiers, producing a bipolar pulse. The rise
time of Vo can be referenced to the crossover point of the bipolar pulse by using a
crossover pickoff discriminator. When the amplitude of the input signal to the
discriminator exceeds a biased threshold level (a variable amplitude sensitive
register used to detect the leading edge of the signal) the pickoff is armed. When
the input reaches zero volts (the crossover point), an output pulse is generated.
The discriminator is reset when the negative amplitude from the bipolar pulse is
detected. The output signal at this point is a rectangular pulse of constant
amplitude, whi<;;h is used in timing.
Due to the different resistance of the wire segments, the crossover point from
the left and right sides will occur at different times as shown in Fig. 4.33. Thus each
event is characterized by two pulses which can then be used to operate a time to
amplitude converter (T AC). This circuit simply initiates the charging of a
capacitor at a linear rate when the start pulse from one end is received, and stops
107
LEFT
RIG HT
LEFT
RIG HT
Fig.4.32. Block diagram of the electronics employing risetime difference detection principle
-----v.:::C2
Dl-~
SUM
T SeA
Cl
T AC
charging when the stop pulse from the other end of the wire is sensed. Thus, the
charge in the capacitor is proportional to the time difference between the start and
stop pulses. If a second start pulse is issued before the stop pulse, it is ignored. This
effect contributes to the deadtime, i.e., the resolving time of the detector.
In order to make sure that the start and stop pulses are always in the correct
sequence, independent of where the ions hit the wire, delay circuitry is used. For
example, in Fig. 4.33, if the event takes place closer to the left end, a stop pulse is
issued before the start pulse. However, it is delayed a fixed time, adjustable at the
crossover pickoff analyzer, such that the start pulse reaches the TAC first.
The energy analysis in this case is performed in a timing single channel
analyzer (TSCA) which compares the sums of the amplitudes from both
preamplifiers (which have been summed concurrently by a summer circuit) , and
compares it to the user-set voltage limits. If the pulse is within this window, a
rectangular pulse is produced by the TSCA which can be synchronized with the
output of the T AC storage capacitor. If this pulse is absent, the output of the T AC
is grounded. Ifit is. present, the signal generated by the TAC, which indicates the
incidence of an x-ray photon of a given energy on the detector, and which contains
the necessary information about its incidence position, is sent to the storage device
which may be a multi-channel analyzer (MCA) 1, or a computer. A detector used
in this mode is terIJled to operate in the coincidence mode. A logical true pulse,
signifying correct energy from the TSCA must be present to validate the recorded
events, resulting in effective energy discrimination, which yields lower background intensities.
Another type of counter currently in use is the scintillation counter which
utilizes materials that produce visible light upon encountering an x-ray photon.
The visible light flashes are then detected by a photomultiplier tube and then
processed with various electronics. Generally these set-ups produce amplifications
In the MCA the pulses from the TAC are stored in memory locations (channels) according to
their amplitude. Every time a pulse of a given amplitude is received, it is processed by an analog
to digital converter and the memory location corresponding to that amplitude is incremented
by one.
108
of the order of 107 , resulting in voltage pulses of several volts. These pulses are also
proportional to the energy of the x-ray photons. However, the amplitude-energy
distribution is about twice as broad as for gas fllled proportional counters, so
energy resolution with a scintillation counter is poor. These detectors, coupled
with the appropriate slits, are widely used in step or continuous scanning through
peaks in diffractometers.
Solid state detectors (SSD) utilize a crystal of pure Ge or Li doped Ge or Si,
and are operated at liquid nitrogen temperature. The incident x-ray photons excite
electrons from the valence band or an impurity level into the conduction band,
producing electron-hole pairs. Under an applied voltage these pairs will produce a
current proportional to the number of incident photons and minute voltage
variations. These signals are amplified and anaiysed by electronics. SSD's are
operated at liquid nitrogen temperature to eliminate thermal noise. They have
very high energy resolution, typically better than AE=200 eV. With standard
electronics these detectors can exclude radiation outside a band of 0.02 keY,
which far exceeds the 20% resolution typical of gas proportional counters and
results in excellent background tp peak ratios for a given wavelength. However,
these detectors are cumbersome and expensive and thus enjoy limited use in
residual stress determination by x:-rays, although they are sometimes very useful
for this purpose.
(4.32 )
where 't is the time constant (dead time) of the system. Let the subscripts 1 and 2
refer to a foil in and out of the beam. Then
(4.33)
Defining the terms RT , Ro:
(4.34)
109
0.49
0.48
0.47
Cu radialion
35 kV -23mA
T=
(6.08
:t
N 10 (cps)
(4.35 )
(4.36 )
Here K is a constant that contains all the terms not dependent on 29, DT ( 29) is
the dead time correction and ABS (9,\jJ) is the appropriate absorption term
110
(Sect. 4.20) . The terms in Eq. (4.36) describe all the terms that contribute to the
angular variation of the observed intensity. These terms may cause distortion of
the x-ray peak, such that the apparent maximum is shifted from the position
dictated by Bragg's law. Thus, for high accuracy, the observed intensity at each
point on the x-ray peak must be corrected for these factors before the 29 position
of the maximum intensity is used in Bragg's law [Eq. (4.13)] for the determination of the plane spacing (d).
It~a.b
) .exp{-llx[ . (~
) + . (~
) ]}.dX.
+tp
sm +tp
sm-tp
dID= .
sm
The total intensity diffracted by the slab of material between this layer and the
surface, expressed as a fraction of the total diffracted intensity is thus given by
x
G =
x
xLJ dID
dID = 1-exP {-llx[
1
+ _ 1_ ] }
sin ( 9 + tp ) sin ( 9 - tp )
( 4.37)
x=o
(4.38)
111
It may be observed from Eq. (4.37) that the effective depth of penetration is
also a function of the 'I'-tilt as well as 29, and decreases with increasing '1'. Thus, if
the "d" spacing of the diffracting planes varies with depth over the maximum
(effective) penetration depth of x-rays, different parts of the gradient will be
sampled during successive "'I'''-tilts. This effect causes bias in the information
obtaned by the x-ray beam and may cause errors in the measured residual stress
values if not taken into account. Various stragegies for minimizing such errors and
correcting for them will be given in Chaps. 5 and 6.
(4.39 )
where T m is the moderator temperature. For T m;:;:: 600o K, the moderated neutron
energies are in the millielectronvolt (meV) range. The wavelength of a neutron
beam can thus be determined from the equation of wave-particle duality (Sec. 4.3 ) :
h2
A.m= ( 3mkTm) 1/2
'
(4.40)
As the mass of the neutron is app-roximately 10- 27 kg, the wavelength of the
moderated neutrons is around 1 A, which is appropriate for diffraction from
crystals. The neutron sources, like synchrotron sources, provide a white beam
without any sharp peaks of characteristic radiation ( Fig. 4.35a). This, as
discussed before, necessitates the use of a monochromator to obtain a
(monochromatic) beam suitable for use in structure or residual stress analysis.
Single crystal monqchromators are used for this purpose. Elimination of second
order wavelength (1../2) in such a beam can be achieved through the use of a
crystal whose structure factor is zero for the second order radiation, or through
filters.
A typical arrangement for neutron diffraction is shown in Fig.4.35b. The
hydrogen in the paraffin or masonite shield slows down any stray fast neutrons,
which are then abserbed by the boron. The lead shielding is to stop any x or yradiation from the reactor from reaching the diffraction area, thus decreasing the
stray radiation that can contribute to the background. Typical neutron fluxes at
the reactor core are about 10 14_10 16 neutrons!cm 2 !sec, and in order to attain
adequate intensity, the neutron beam at the reactor face has a rather large crosssection of 2 to 8 cm 2 This beam is collimated by the use of soller slits that are
112
wOler
Fig. 4.35. Distribution of intensity vs. wavelength in a steady-state neutron source. b Schematic
of a steady state neutron source and associated diffractometer
m---
NEUTRON SOURCE
COLLIMATOR #1
DISK CHOPPER
!!>----SAMPLE
28'1
~~COLLIMATOR #21
DETECTOR
113
."
40K
a:
I
~ 30K
(f)
420
331
311
II I
220
"
l-
200
>-
l-
v;
"
z 20K
UJ
I-
\..........
i\
CHANNEL NUMBER
Thus, if the incoming pulses are detected, processed electronically, and inputted
into a multi-channel analyzer which is re-started as each burst of neutrons leaves
114
Monitor
I
IHelium
chamber
atmosphere
Fig. 4.38. Schematic of the detector banks at the Intense Pulsed Neutron Source (IPNS) at
Argonne National Laboratories
the chopper, each channel in the MCA corresponds to a given wavelength. Typical
data. obtained in this manner, are shown in Fig. 4.37. This mode of analysis is
called time-of-flight (TOF) analysis, and has a higher resolution than neutron
diffractometers for d spacings larger than 1 A. For a detailed treatment of this
method the reader is referred to Schwartz and Cohen [2, pp. 250 - 252].
The time of data acquisition can be decreased even further if, instead of one
detector at an angle 29, as shown in Fig. 4.36, a bank of detectors is used, arranged
in a circle around the specimen. One such arrangement is shown in Fig. 4.38.
115
Table 4.4. Scattering factors of selected elements for neutrons (b) and x-rays (f)
f-10 14m
b10 14m
sin a/A.
Hydrogen
Copper
Tungsten
0.1
-0.378
0.67
0.466
0.5
-0.378
0.67
0.466
0.1
0.23
7.65
19.4
0.5
0.02
3.85
12.0
Table 4.5. True absorption coefficients for neutrons and total absorption coefficients for x-rays
for selected elements
Element
Be
Al
Cu
0.00003
0.0003
0.0021
0.0036
0.24
0.150
4.86
5.29
1.72
0.24
116
further in Chap. 5. For further information about neutron diffraction and neutron
sources the reader is referred to Bacon [6].
Problems
4.1. A Cu target x-ray tube is run at 40 kV and 20 rnA. The power input is given by
T/2
p=
B.D. Cullity, "Elements of X-Ray Diffraction", 2nd ed. Addison Wesley, Massachusetts, 1978
L.H. Schwartz and J.B. Cohen, "Diffraction from Materials", Academic Press, New York,
1977
3 L.V. Azaroff, "Elements of X-ray Crystallography", MacGraw Hill, New York, 1968
4 C.S. Barrett and T.B. Massalski, "Structure of Metals", 3rd. ed., MacGraw Hill, New York,
1966
5 H.P. Klug and L.E. Alexander, "X-ray Diffraction Procedures", Wiley, New York, 1967
6 G.E. Bacon, "Neutron Diffraction", 3rd. ed., Clarendon Press, Oxford, England, 1975
7 "International Tables for X-ray Crstallography I - IV", 3rd. ed., Buerger et al. eds, Kynoch
Press, Birmingham, England, 1976
8 D.P. Koistinen, R.E. Marburger, Trans. ASM, 51, 537 (1959)
9 M.R. James, "An Examination of Experimental Techniques in X-ray Residual Stress
Analysis", Ph.D. Thesis, Northwestern University, Evanston, II., 1977
5.1 Introduction
Up to this point the mechanical and micromechanical behavior of solids and basic
concepts of x-ray and neutron scattering from crystalline solids have been
presented. In this chapter these concepts are combined in the derivation of the
basic equations of residual stress determinatipn with diffraction. The fundamental
assumptions inherent in these derivations and the limits they impose on the
applicability ofthe,.stress measurement will also be discussed. Various problems in
an actual stress measurement, such as the effect of stress gradients, the separation
of micro and macrostresses, determination of stresses in thin films and single
crystals, etc., are also considered, with special emphasis on the interpretation of
the data within the limitations of the theory.
In this chapter, however, it will be assumed that a perfectly aligned x-ray unit is
used in the measurement of exact data from a flat sample. These ideal conditions,
of course, are not always available to the experimenter and in chapter 6 the errors
caused by deviations from ideality will be treated in detail.
118
Fig. 5.1. Definition of the laboratory coordinate system Lj , simple coordinate system S;,
and the angles <l>,1J'
where a 3k ,a 31 are the direction cosines between L3 and Sk> Sl respectively. The
direction cosine matrix for this case is
aik =
-sinlP
(5.3 )
cOSIP
2,J,. . 2
. 2,J,. . 2
(5.4 )
,
~
"tl
"tl
>/1>0
"tl
el/r<O
sin2",
sin2",
sin2",
Fig. 5.2. Types of "d" vs. sin21J' plots commonly encountered in residual stress analysis from
polycrystalline materials. The curves a,b exhibit regular behavior, the data of which follow
Eq. (5.4). The curve c exhibits oscillatory behavior which cannot be explained by this equation
119
or both of these components are non-zero, d measured at positive and negative 'I'
will be different due to the argument "sin 2'1''' associated with these terms, causing
a "split" in the d vs. sin2tp data (Fig. 5.2b). This effect is termed "tp-splitting"
[1,2,3]. Data exhibiting "regular" behavior can thus be analyzed by methods
based on Eq. (5.4). These methods are treated below. On the other hand, the
oscillatory d vs. sin2tp behavior shown in Fig. 5.2c cannot be predicted by
Eq. (5.4) without further modification. Analysis techniques for oscillatory data
will be treated in Sect. 5.13.
(5.5a)
(5.5b)
where 'I' _ = ( -1 ) ''1' + and sin2tp + - sin2tp _ = 2 sinl2tpl,
Equation (5.5a) predicts a linear variation of a 1 with sin 2tp, with the slope and
intercept given by
(m~)al =E 11 coS 2<1> +E 12 sin2<1> +E22sin2<1>-E33 ,
( 5.6a)
and
(5.6b)
respectively. Similarly, a 2 varies linearly with sinl2tpl. The slope in this case is,
( 5.7)
Thus, if d~1P data is obtained over a range 'I' at three <I> tilts (0,45,90),and a 1
vs. sin 2tp and a 2 vs. sinl2tpl are plotted for all '1', the quantities Ell - E33 ,
1/2(E11 +2E12+E22'-2E33)' and E22 -E 33 , will be obtained from Eq. (5.6a) (at
<I> =0,45,90respectively). The intercept of a 1 vs. sin1tp is equal to E33 at all 'I' tilts
[Eq. (5.6b) J 1. Similarly, the slope of a 2 vs. sinl2tpl, [Eq. (5.7) for <I> = 00,900J
yields the quantities E13 ,E23 .
1 This condition may be used to check the compliance of experimental data with theory.
120
A simpler procedure, requiring less data points, may be used for linear d vs.
sin 2tp plots (Fig. 5.2a) that exhibit no tp-splitting. In this case, the strain tensor in
the Si coordinate system is of the form
Eij=
Ell E12 0
0 E22 0
o 0 E33
and d vs. sin2tp data is required at positive (or negative) 'I' tilts only. For such a
strain tensor, equation (5.4) becomes
. 2'"
. 2",
. 2tp+E
d",..,-do
do
= {Ell COS 2",
",+E 12sm
",+E22 sm
",-E'33}sm
33
( 5.8)
The right hand side of Eq. (5.8) is equivalent to that of Eq. (5.6a) and a similar
analysis may be used to determine Ell,E12,E22,E33.
(5.10)
where ami are the appropriate direction cosines.
The procedlJre discussed above is the basis of all types of diffraction techniques
for stress determination. These techniques, however, usually express Eq. (5.4) in
terms of stresses, and simplify or modify the resultant equation according to the
properties of the material under investigation and according to the stress state
expected in the ~rradiated volume. In the following, these procedures are examined
in detail.
In the most general case, where an anisotropic material contains a general
triaxial stress tensor
O"ij=
( 5.11)
the strains in the sample coordinate system can be expressed in terms of stresses by
the inverse of Eq. (5.9):
(5.12 )
121
1_-
_\
~
I
C2
/1
where Sijkl are the elastic compliances. The equation linking stresses to measured
diffraction data may be obtained by substituting Eq. (5.12) into Eq. (5.4) for all
Eij.1t must be remembered, however, that the elastic compliances are also referred
to the Si system of axes, and must be obtained from the elastic constants referred to
the unit cell axes (Fig. 5.3 ), by the tensor transformation rule for fourth rank
tensors [Eq. (2.50)]. For example, for Ell:
(5.13 )
Here akO are the direction cosines between the crystal axes and the surface
coordinate system and Smnop is defined in the crystal axes. Equation (5.13) and
similar equations, written for the other components of the strain tensor, can be
substituted into Eq. (5.4) to obtain the general equation linking measured d
values to the stresses existing in the sample coordinate system, Si.
If the material under investigation is isotropic, Eq. (5.12) becomes (Sect. 2.7)
1+v
Eij
=E
(Jij -
oij
(Jkk ,
(5.14 )
( 5.15 )
122
It can be seen from Eq. (5.15) that, for isotropic materials, if the stress tensor
existing in the specimen coordinate axes, S;, is one of the following forms:
(T n (T
(T cr~J (T
0
0"22
0
g)
(5.16a,b)
0"12
0"22
0
b
0
0"22
0
c
0"12
0"22
0
d
cr~,)
(5.16c,d)
the d vs. sin2'1' plot obtained from the surface layers will be linear (Fig. 5.2a) . A '1'spitting in the d vs. sin 2'1' plot (Fig. 5.2c) on the other hand, indicates the presence
of the shear stresses 0"13,0"23.
do
where
O"~,
1 +v
. 2
V
= EO"~sm '1'- E (0"11 +0"22) ,
2,j,.
"'+O"22sm '"
2
O"~ = 0" 11 cos <j> + 0" 12sin2<j> + 0"22sin2<j> ,
O"~=O"l1COS
S~
(5.17 )
123
ofE and v. Sl,S2/2 may be obtained from the literature for a given material and
reflection combination. If experimental values are not available, they may be
calculated from single crystal elastic constants using the various approximations
discussed in Sects. 3.1 0 - 3.12. They may also be measured experimentally, and the
procedures used for such measurements will be discussed in Sect. 5.14.
(5.19a)
The term Ad/d may be written in terms of the shift in 28 of the diffracted intensity
maximum between these two tp-tilts. Differentiating Bragg's law, nA,=2d sin 8:
Ad
cot8A28
(f=2
(5.19b)
0'.=KA28,
where A28 is the peak-shift. K is called the stress constant, and is given by
K=
E'cot8
2( 1 +v) sin2tp .
(520)
.
This procedure is accurate for small A28, but substitution of Eq. (5.19b) into
Eq. (5.19a) may not be valid for large A28. In such cases, one may use Eq. (5.19a)
with two tilts without this approximation.
This method, as the name implies, acquires all the data required for a biaxial stress
analysis at a single tp'tilt, where tp O. The Debye ring from a stressed material at a
non-zero tp-tilt is non-circular as shown in Fig. 5.4a. This is so since the normals
N 1 ,N2 of the planes that diffract to points 1,2 on the diffraction cone are at
different inclinations (n 1 , n2) to the surface normal. Thus, the resolved strain on
these planes are different, and the plane spacing varies along the Debye ring
causing the deviation from circularity. Determination of the difference, A8,
between the Bragg' angles corresponding to the points PloP 2 from a film
( Fig. 5.3a), or from PSDs placed at the appropriate locations around the
incident beam (Fig. 5.4b), enables the calculation of the stress along S. from
}
E
{
cot [1/2(8 1 +82)]
0'.= (l+v)' sin 2 (p+n)-sin 2 (p-n) ,
.(5.21a)
124
--~ "
(~'I-------l-------- \I
\
1
1
:
~
:
I
;I1
"'-
P2
1
1
:
--.!.-
..,/
/i
Bi
:
-----t--...,...--+--T"'""'--+..:..--
film
~'"\
\
a
~s
:------~
X-Roy S
Position Sensitive 1
Detecto~~
1
I
I
Specimen
SUrface"
--~-7~------------------
~\\~I
b
Fig.5.4. a Geometry of the single-exposure technique for residual stress measurement with a
film at specimen tilt ~ and effective ~ -tilts n 1, n 2 b The same technique with position sensitive
detectors
125
crlj>= KL\9 ,
where K, the stress constant, is given by
K= ~.~.
1
9'" 9 1+9 2
2
180 1 + v 2 sin 2~ sin 29 '
It may be noted that the procedure is similar to the two-tilt method in that plane
spacings at two effective ",-angles, n 1 and n 2, are used to determine the stress. If
(9) Pl' (9) P2 are determined at multiple inclinations o,'" 1,... ,"'" one can use the
data thus acquired in the sin 2", analysis discussed above.
a 1 -_ {dlj>'P+ +dlj>'P_
2do
1}
1 + v {crdcos 2,l,.
2,l,.
2,l,.
2
E
..,+cr 12sm
..,+cr22 sm
..,-cr 33 } sm
'"
( 5.22a)
(5.22b)
Thus, the stresses cr11,cr12,cr22,cr33 may be obtained from the slope and intercept
of a 1 vs. sin 2", for <1>=0,45,90. The slope of a 2 vs. sinl2",1 for <1>=0,90,
respectively, yields the shear stresses cr 13'cr23. After the stress tensor in the sample
system Si is determined, the stress tensor in any other coordinate system, such as
the principal stresses and their directions, may be determined using the procedures
discussed in Sect. 2.6.
It has been noted in Sect. 5.4 that, if a triaxial stress tensor that does not
contain cr 13'cr23 exists in the irradiated volume, then d vs. sin 2", will be linear. In
126
(5.23 )
It may be seen from a comparison of Eqs. (5.17) and (5.23) that, if 0"33 is finite
within the penetration volume, the stress 0"1> determined by bi-axial methods from
the slope of the d vs. sin 2\jJ line will contain an error equal in magnitude to 0"33. In
such a case, the following method way be used [7]. If d vs. sin 2\jJ data is obtained
for two <\> tilts, <\>=<\>A' <\>=<\>A+90, where <\>A is the angle between Si and the
principal axis Pi (which is generally not known) , one can obtain from the slopes
of the (C~3) 1>", vs. sin 2\jJ plots,
l+v{
2,1,.
.
2
}
ml>A =
O"llCOS 'f'A + 0"12 sm2 <\>A + 0"22 sm <\>A - 0"33
1 +'v
(O"I>A -0"33)
(5.24a)
l+v{
2
.
ml>A+90 =
O"llCOS (<\>A +90) + 0" 12sm2 ( <\>A +90)
+ 0"22 sin2 (<\>A + 90) - 0"33}
l+v
=
(O"I>A+90-0"33)
(5.24b)
(5.25 )
The intercept, I, of (C~3) 1>", vs. sin 2\jJ does not depend on <\>:
1=
(5.26)
Equations (5.25), (5.26) may be solved together for 0"33 after which the stresses
O"I>A'O"I>A + 90 along the surface directions ~I>A'~I>A +90, may be determined from
Eqs. (5.24).
127
hand, utilize the difference, ~d = dcl>'P - do, in the calculation [Eqs. (5.5), ( 5.22) J.
The term ~dis very small for elastic strains. Consequently, even a 0.1 % error in do
can cause a large error in ~dl, and thus in the subsequent analysis. It may be seen
from these considerations, that in order to obtain stress results with acceptable
error from a triaxial solution, do must be within less than 0.01 % of its true value.
Determination of do to such accuracy may not be trivial and in the following,
various problems that may be associated with this measurement are discussed.
One method uses ftlings of the material under investigation. The powder
particles of such a sample cannot sustain a macrostress (the powder particles are
not rigidly bonded together and can not sustain macrostresses across their
boundaries) and, with small randomly oriented particles, the average microstress
in a representative volume is zero. Thus, the plane spacing determined from such a
sample will be that of an "unstressed" sample. In another variation of this method,
the ftlings are annealed to relieve all residual stresses and the plane spacing do is
determined from the stress-relieved powder. Alternately, one may anneal a solid
sample, such that all the residual stresses are relieved, and determine do from the
stress-relieved sample. These procedures, however, may also introduce other
factors that can affect the plane spacing. For FCC materials, a general formula
relating the change in 29 between an annealed sample and a cold worked sample,
to various parameters was given by Wagner2 [8J:
~29hkI = 29deformed - 29annealed
.
.~a
( 5.27)
a
~a
a
9
Thus, if filing or annealing for stress relief causes changes in ex, Ct, ~a , the do
a
values obtained from such procedures may be erroneous for stress measurement
purposes (Table 5.2). Such errors can be especially large in materials susceptible
to stacking faults. In such cases, the do measured from the annealed sample may be
corrected if, without annealing, one obtains the terms ex, Cl'
~a ,0", by measuring
a
1 For example, consider data from an iron sample. In this case, do = 2.8665 A. Assume that
d+",=2.8675 A. In this case, L\d=O.oo1. If do changes by 0.1 % due to an error, L\d becomes
0.00187, which is almost a 90 % change.
2 For ordered FCC structures, there are other terms that contribute to L\29hkl These terms are
discussed in [31]
128
j\
j2
Peak
j\
j2
100
110
111
200
210
211
220
-5.265
2.632
3.949
-7.897
-0.526
0
3.949
- 6.37
- 6.37
-23.87
19.10
10.82
- 6.37
19.10
310
311
222
320
321
400
331
-0.526
-1.436
-1.974
0.810
-0.188
3.949
0.831
- 6.37
- 4.34
-23.87
- 6.37
5.91
19.10
-38.20
The term j3 is the bulk modulus [Eq. (3.50)] for the particular material, and j4 is - 360/1t for all
materials.
Table 5.2. Variation oflattice parameter, ao, with cold work and various heat treatments in two
FCC alpha-brass alloys'
Material
Cu-30 Zn
Condition
Treatment
L~ttice
Filings
10 Mins. 300C
+ Water Quench
Room Temperature
1032 Hrs. 120C
3.6825
3.6832
3.6803
Filings
Filings
Cu-35 Zn
Filings
Filings
Filings
Filings
10 Mins. 300C
+ Water Quench
10 Mins. 300C +
1072 Hrs. 120C
Cold Worked Room Temp.
Cold Worked Room Temp.
+ 1031.25 Hrs. 120C
(A)
parameter,
3.6946
3.6940
3.6955
3.6918
L\29 of at least four peaks, and solving Eq. (5.27) for these terms through linear
regression. Then, the 29 of the material that is equivalent to the cold worked
specimen in stacking fault density and related terms, but has no stresses, is given
by
(5.28 )
do can then be obtained through Bragg's law.
For Bee structures Eq. (5.27) becomes [10]
A2e'
e'
L\a
e.
hkl=jzcxE 1tan 9
+hO"ltan
+J4-tan
il
(5.29 )
Thus, similar considerations may apply to Bee materials also, but the effects are
smaller since CXE 1 is a small quantity; the term in cx present for fcc system is absent
for bcc (and hcp) systems.
129
(5.30)
'
(5.31 )
where m 1 ,m 2 are the slopes ofd vs. sin 2\jJ at <\>=0,90 respectively and may be
determined experimentally. Thus sin2\jJ' may be obtained from Eq. (5.31) after
which do is obtained from the d vs. sin 2\jJ at <\> = 0.
A similar procidure for a triaxial stress state has also been suggested [11]. For
Eqs. (5.22a) or (5.23), sin2\jJ' is given by
(5.32)
(i) (1+
C~v)
m2)
m
1
(5.33 )
'
where the terms m 1, m 2 may be obtained from the slopes of d vs. sin 2\jJ for <\> =0,
90. The assumption that v =.5 in one term in the numerator, though, causes some
error in do determined from equation Eq. (5.33) [12]. This error may be obtained
by substituting Eq. ( 5.33) into Eq. ( 5.23 ):
( do ) ",' - do ~do
( 1 - 2v )
do
= do =
E
0"33 .
(5.34)
It may be seen that the error in do determined from Eq. (5.33) is a linear function of
0"33' Due to this error in do, the stresses, O"ii' determined from the triaxial methods
130
described above contain errors comparable to the value of 0"33 existing in the
irradiated volume. Thus, this method of do determination should not be used in
cases where a large 0"33 component may be present.
values to the strain tensor in the surface coordinate system, Eq. (5.4), contains no
assumptions about the symmetry of the unit cell of the material under
investigation. The procedure is based only upon the transformation law for second
rank tensors [Eq. (2.24)], and is applicable to all unit cells with arbitrary
anisotropy as well as to isotropic materials. The effect of anisotropy is taken into
account only~ when one tries to compute stress values from the strain tensor
[Eqs. (5.9), (5.13 ) ,( 5.15), etc.]. Thus, as long as the appropriate form of
Hooke's law is used, the methods are applicable to any type of unit cell. There are,
however, other implicit assumptions in the derivation and these are treated below.
In the derivation of Eq. (5.3) the position of the specimen axes, Si' is not
specified. The origin of Si can be at any point within the irradiated volume from
which d"[Eq. (5.1)] is obtained, and thus, the strain tensor, defined in Si is
assumed to be the same at all points, i.e., homogeneous in the irradiated volume.
Residual stress distributions, on the other hand, must be, by definition,
inhomogeneous. The stresses in one part of the body are balanced, according to
equations of equilibrium, with stresses in another part of the body, such that the
integration of stress over the entire volume is zero (Sects. 3.3 - 3.5 ) .
(3.11a)
Thus, in a given specimen, the dimension of the irradiated volume along a given
direction must be much smaller than the characteristic length along this direction
over which the residual stresses vary appreciably. Strain (and therefore stress)
values obtained from irradiated volumes with larger dimensions will be the
average of the actual stress distribution within the volume. The particular
averaging function in such cases is dependent on the distribution of the crystalline
regions within the specimen since only those regions that are diffracting can
contribute to the information obtained by the x-ray beam. Furthermore, the
diffracted intensity contribution from layers deeper in the material must be
weighted differently because of absorption (Sect. 4.20) . Finally, the desired strain
or stress components are obtained by least-squares methods from the average data
measured by x-rays. This, in effect, re-averages averaged data. Thus, the final
results are complicated averages of the local values, and unless the actual strain
distribution within the irradiated volume is known, interpretation of the average
data in terms of local deformation may not be possible.
131
,/~
,/
,/
,/
,/
d hkl
'/'
,, ' '
~,
,/
',
, ,
,,, "
CI
-...~
I diffracted
Fig. 5.5. Relationship of the crystal axes C; with the incident and diffracted beams and
the laboratory axis L3 = ~hkl when the Bragg condition of diffraction is satisfied for a
set of planes, (hkl)
132
position
sensitive
detector
Fig. 5.6. Parallel beam diffractometry from a single crystal using a position sensitive detector to
resolve the diffracted intensities from points on the specimen surface
For relatively perfect crystals, all points within the irradiated volume
contribute to diffraction because of the long range symmetry through the entire
volume of the crystal.
The strain at any given tilt is acquired from a homogeneous, continuous,
anisotropic volume and represents the average of the strains in this volume. The
calculation of the average stresses in the diffraction volume from the measured
average strains utilizes the appropriate elastic constants referred to the specimen
coordinate system and the general expression for Hooke's law.
If the single crystal under analysis has large subgrains with relatively large
misorientations, or the strain profIle is inhomogeneous within the irradiated
volume, it may be necessary to determine the strain in regions within the crystal
where the strain is relatively homogeneous. This may be achieved by a procedure
described by Mayo et al. [15], where a parallel x-ray beam impinges on a single
crystal and the diffracted beams are detected by a position sensitive detector
whose wire is parallel to the a-rotation axis of the crystal (Fig. 5.6) . The diffracted
intensity registered by the PSD at any position will correspond to a definite
position on the specimen. Thus, within the linear resolution of the PSD
( Sect. 4.22), the diffracted intensity from different positions along the intersection of the beam with the specimen may be stored in a channel of a multichannel
analyzer. If the specimen is rocked through the Bragg angle, the variation with
rocking angle of intensity in each channel is obtained, which is, in effect, the Bragg
peak profIle for each point on the specimen surface. The intensity maxima can
then be used to determine the strain corresponding to each position on the
specimen (Fig. 5.7). Rotating the specimen to bring other reflections into the
diffraction condition and repeating the procedure, provides the data required for
the strain analysis at each point along the intersection of the beam with the
specimen. Stresses may then be obtained through Hooke's law. It must be noted,
however, that if there is misorientation between the subgrains, the direction
cosines between the specimen axes and the crystal axes (and thus the elastic
constants referred to the specimen axes) will be different for each subgrain.
Furthermore, if the deformation distribution is inhomogeneous, reflections that
133
Uniform
Strain
a
~=O
--
"g
.J SI
QI>.
B
C
28
Nonuniform
Strain
Fig. 5.7. Variation of the intensity with rocking angle at the points along
the surface when the strain distribution along A,B,C is homogeneous
( a) and inhomogeneous (b)
involve <j>-rotations can not be used, since, for such rotations, the intersection of
the parallel beam with the crystal will move to a new surface direction Sci>'
(Fig.5.8) , and the points along this new direction may not have the same strains as
the points along Sci>' Depending on the particular experimental arrangement and
beam dimensions used in a given experiment, similar problems are possible with
other rotations.
Another point that must be considered in the analysis is the presence of strain
gradients with depth. In such cases, the d spacing, and thus the strain obtained by
the x-ray beam will be the average of this gradient over the effective penetration
distance of x-rays, t. This distance is limited by absorption and depends on 29,\1'.
In Sect. 4.20, it was shown that the diffracted intensity from a unit volume located
at a distance, Z, from the surface can be written as
dI '" e - "ldV ,
(5.35 )
134
tS3
I
Incident
Beam
Diffracted
Beam
Diffracted
--H- -
S2
1-
Scp'
~I
Fig. 5.8. Variation of the measurement direction and diffracting points in parallel beam singlecrystal diffractometry with a rotation (<l around ~h
where I is the total path length of x-rays within the specimen and ~ is the linear
absorption coefficient. For the a-goniometer (Fig. 4.27), the path length for any
\jJ-tilt is given by
{ 1
1=.
sm(9+\jJ)
1}
+ sm(9-\jJ)
.
'z,
(5.36 )
(5.37)
Similarly, for the \jJ-goniometer (Fig. 4.28):
2
z.
sm 9 cos \jJ
1= .
(5.38 )
(5.39)
Thus, the effective penetration depth for the a goniometer is given by [22]
(5.40 )
135
Goniometer
Goniometer
5
6.
4
6
u;
c:
e
0
'E
Eo<
(T 8 )""0
(micron)
2.
O.
O.
0.3
0.6
sin'v
20
60
100
140
Fig. 5.9. a Variation of the penetration depth with sin 2 ", for Q and", goniometers (29 = 1550 , Cr
radiation on Fe, 211 reflection). b Variation of the maximum penetration depth 1: ('" = 0) with
29. (Fe specimen, Cr radiation)
and by
sin e costp
211
't=---~
( 5.41 )
for the tp goniometer. In Fig. 5.9 a,b, the variation of penetration depth with tp
(at constant 2e), and with 2e (at constant tp) is shown.
Within this depth, the diffracted intensity from points deeper into the material
is smaller than the contribution from the points that are closer to the surface
because of absorption (Sect. 4.25). Consequently, the average strain obtained by
x-rays will contain a larger contribution from the strains in the shallower depths.
The average strain over the total penetration depth ('t1p) can be expressed as
T",
(5.42 )
where e - ziT"" the weighting function, describes the intensity diffracted from
depth z.
Since the path length of x-rays within the material, and hence the effective
penetration distance, is dependent on the angles e,tp, a different portion of the
gradient will be sampled for different reflections. This means that the average
strains referring to the sample coordinate system, <cij), are also dependent on e,tp,
and the final strain tensor, obtained from the least-squares regression is a
complicated average of all the <cij)o,1p' If, for all rotations, the penetration depth is
greater than the thickness of the specimen (for some thin-films for example) , the
total gradient is sampled at all times and this effect may not be important.
136
However, in relatively thick specimens that may contain steep gradients, OEij/OZ,
within the irradiated volume, this effect may cause deviations from regular
behavior in "d" vs. sin 2tp, and may cause errors in the results obtained from the
least-squares analysis. The effect of such gradients with depth will be discussed in
detail later in the text (Sect. 5.12) .
J f(z)dV
(E jj \,. = ----v.cN:=-------
L Vk
(5.43 )
k=l
where Ejj(X,y,z) is the strain at the point, A(x,y,z), in a diffracting grain in the
irradiated volume, Vk is the volume of this grain, f(z) is a weighting function
relating the variation of diffracted intensity to depth (z), and Nk is the total
number of grains diffracting at a tilt angle tpl. The summation is required since the
diffracting grains are not necessarily contiguous. Equation (5.36) describes the
average strain (Eij)q,. in the population of grains diffracting at tpl.
At any tp-tilt, the average strain (E~3)q,1p is related to the average strains in the
sample coordinate system through Eq. (5.4):
o
(E33, >cj>1p-_ (dcj>1p)-d
do
(5.4b)
where the terms (Eij)1p are the average strains in one population only. If the
experimentally determined (Ej)1p values vary regularly with sin 2tp, (Figs. 5.2a,b),
this indicates that the (Ejj )1p is equal in all the populations sampled during the tptilts, i.e., the average strain tensor {(Ej)1p} is homogeneous in these populations.
Non-regular (oscillatory) behavior, on the other hand (Fig. 5.2c), indicates the
137
28
::-L~ ----~
iii
1"1
I \
I \
28
Fig. 5.10. Diffracting grains in a polycrystalline specimen at (a) tp =0, (b) tp =tp, during a stress
measurement. The x-rays are diffracted from mutually exclusive subsets of the total irradiated
volume at each tilt
presence of an inhomogeneous average strain state; for each diffracting subset, the
strain <E;j)", along S; is different. Interpretation of such inhomogeneity in terms of
local strains is also complicated by the fact that the diffracting subsets are not
distinct homogeneous volumes in real space. Even though diffraction can easily
separate the grains' into the respective subsets, the grains for all subsets are
intimately mixed in the material. A grain that belongs to the population diffracting
at 'l'='l'A may be surrounded by others that diffract at another 'l'-tilt. Thus,
in going from one grain to another in a given subset, grains that belong to other
subsets must be traversed. Therefore, even though diffraction obtains data from a
given subset as if S; is continuous in that subset, the regions along S; that
contribute to the diffracted intensity are discontinuous in real space.
138
139
MPa
0
-100
-0
U~ - D
"
(1:'
-500
30
60
90
z-
120
150
~m
180
200
MPa
100
[]
c
c
+ +
c
[]
~
+ ~
[]
---- -~----
Vi
-200
-L.OO
b
(T_ - )(
x
x x
-300
0
-100
III
III
30
w w
60
,
x
o'-
90
u.''''
~
z-
u:- -
120
150
- 0
~m
180
contributions due to the microstresses and macrostresses [27]. The average stress
obtained from any phase [Equation (5.46)] may be written as
(5.45 )
where O"~ is the macrostress and <O"ij>~m is the average microstress (PM stress) in
that phase. For symmetric surface deformation O"g3'0"?3,O"g3 will be zero as noted
above. It can be seen that for the stress components 0"11,0"22,0"12 x-ray
measurements yield'two equations in three unknowns. For example, for 0"11:
(5.47 )
where f is the volume fraction of the second phase. Thus, one may solve for
<cr11>~m,<cr11>gm, which are the contributions from the microstresses and cr?1
which is the macrostress due to the constraining effect of the bulk.
140
This procedure requires accurate values for the unstressed plane spacing "do"
of both phases. However, even when these values are not available, it is possible to
separate the macrostresses cr? 1,crg 2 from the contributions due to micros tresses
[27]. For example, the slopes of d vs. sin 2 tp from both phases of a shot-peened
alloy are given by [Eq. (5.24)] for <l> = 0:
,'
v) .{ocr + <cr
II
ll
ll
)p.m
_ <cr33 )P.m}
II
II
(5.48a)
(5.48b)
<cr33)~m)
Thus, Eq. (5.48a,b) and (5.49) may be solved for the macrostress term cr? l ' and
the total micrestress terms in r:t and ~. In Fig. 5.11a,b the measured and separated
residual stress profiles from both phases of a shot-peened two-phase brass alloy
are shown. The second phase contains appreciable microstresses in addition to the
macros tresses imposed by the bulk.
where crij (t = 0) is the stress value at the surface, aij,n ij are constants over the
depth of penetration, and z is the distance coordinate along S3' measured into the
material.
1 A power law is assumed to represent the gradient in stress in the following discussion for
simplicity. For a more general discussion the gradient may be expressed in any functional form.
The general arguments, however, will be similar as long as the gradient is a monotonically
varying, single valued function of z.
5.12 Effect of Stress Gradients Normal to the Surface on d vs. sin 2 \jl Data
141
1-1
1-2
2.873
.. I-3
2.870
0
~
jl
c:t
52.867
i!
II
"0
2.864
iii
0.0
0:4
0.8
sin2 lY
The average sttess determined by x-rays at any tp-tilt is, from Eqs. (5.42) and
(5.43) ,
(5.51 )
where Kij is a constant, nij is the exponent of the stress variation and 'tlP is given by
Eqs. (5.40, 5.41).
Thus, if the stresses are functions of depth, instead of constant valued
unknowns, expressions of the form given by Eq. (5.51) should be substituted for
the stresses in Eq. (5.15). For example, for a stress tensor of the form
(
0"11 0 0
o 0"22 0 "
o 0 0"33,
0"33=K33't~33,
(dcj>lP)-d o 1 +v
. 2
2v
K33't~33 {
. 2
}
do
= E .0" 11 . SIn tp - E cr 11 +
E
( 1 + v )( 1 - SIn tp) - v .
(5.52 )
Here the first part of the equation is equivalent to the classical biaxial stress
Eq. (5.17) and exhibits linear dependence versus sin 2 tp. The second part (which is
the x-ray average of the 0"33 gradient for the particular tp-tilt) is not linear in sin 2tp.
In case of single valued, monotonically varying gradients, this term increases in
magnitude systematically with decreasing tp (increasing 't1), and thus causes a
progressively larger deviation (curvature) in the d vs. sin tp plot. If d vs. sin 2 tp
does not exhibit tp-splitting, such curvature can be easily observed (Fig. 5.12). In
such cases, the use of high tp-points for the linear regression analysis will minimize
142
18
2.8750
'10 4
40
14
30
12
.0/1> 0
20
10
,0/1<0
2.8700
6
4
-;..
-e-
1::J
70
60
-2
50
-4
40
-6
2.8630 0
0
b
8
'10 4
.. '" >45
'" ~45
6
5
4
3
2
0,2
0.4
0.6
0.8
sinI2if;1-
any curvature errors associated with the data, since the absolute value of the '1'dependent terms will be less in shallower depths. It must also be noted that the
other terms ofthe stress tensor such as a ll ,a22 may also possess gradients along
the z-direction, and thus may cause curvature in the d vs. sin 2 tp plot.
Similar effects must also be taken into account when the d vs. sin 2 tp exhibits '1'splitting (Fig. 5.13a). In such cases the stress terms a 13,a 23 may be finite, both of
which must exist as gradients in the irradiated volume, and the a 1 vs. sin 2 tp, and
a 2 .vs.sinI2tpl must be calculated [Eqs. (5.22a,b)] and plotted (Fig. 5.13b,c) in
order to separate the effects of curvature due to gradients from the curvature
caused by the trigonometric term sinl2tpl in Eq. (5.15). If any of the normal
stresses (ajj ) or the shear stress (a 12) exhibit gradients with depth, the behavior
of the term a 1 vs. sin 2 tp will be similar to d vs. sin 2 tp (Fig. 5.12, 5.13b), and to
minimize errors due to curvature high tp-points must be used. However, the
5.12 Effect of Stress Gradients Normal to the Surface on d vs. sin 2\jJ Data
MPa
400 f-
200
143
~1'~2
.. ~3>t/f
(033)t/f
t-
oC=::=~~---J
'b
-200 -
-400t~----~--------------
I
4
z-
2 IJ.m
argument sin 12", 1in a 2 is a multivalued function of", over", = 00 ,60 0 (which is the
commonly available ",-range for experiments). This, coupled with the fact that
different regions of the gradient are sampled at each ",-tilt, causes two branches in
the a 2 vs. sinl2",1 data (Fig. 5.13c). In such cases, either the linear part of a 2 vs.
sinI2",1, or non-linear regression over the entire ",-range must be used to obtain the
stress values. In Fig. 5.14 the average stress profiles used in simulating the d vs.
sin 2", in Fig. (5.13a) are shown. In Table 5.3, the solutions obtained from the
traditional methods in various ",-ranges are summarized. From a comparison of
the input values (Fig. 5.14) and the analysis results (Table 5.3), it may be seen
that gradients, if not properly taken into account, may cause large errors in the
stress results obtained from x-ray analysis.
Table 5.3. Analysis of ~l vs. sin 2\jJ, a2 vs. sinI2\jJ1, (Fig. 5.13b,c) over various \jJ-ranges. (These
plots were calculated from the input profiles shown in Fig. 5.14.)
\jJ-Range
(degrees)
al
0.00 -60
0.00 -33.21
39.23 -60
0'22
(MPa)
-442
-562
-412
-442
-562
-412
O'll
(MPa)
Error in
0'1 dMPa)*
(al3>
(al3>
107
55
81
42
162
12
50
86
278
0
0
0
(MPa)
96
-182
183
is defined as
(a 33 >
(a23>
(MPa)
0.00 -26.57
33.21 -45
50.84 -60
The error in
(MPa)
<al3>
\jJ-Range
(degrees)
a2
O'll
0
0
0
(O'll
(MPa)
(MPa)
Corr. coeff. of
a2 vs. sinl2\jJ1
0.9952
-0.913
0.992
144
In the discussion so far, the effects of gradients on d vs. sin 2 ", has been discussed
with particular emphasis on the errors they cause in x-ray stress determination.
Determination of the gradient in stress with depth is also an important
measurement, extensively used both in research and industrial testing [4.29].
Various methods are available for the determination of the stress profile with
depth. If the stress proflle within 10- 20 microns of the surface is required, one
may use various radiations, penetrating to successively different depths, to
determine the variation of the average stress state with depth. For example, in
steels, one can use Cr, Co, Mo radiations with maximum penetration depths
('" = 0) of 5.4 microns (211 reflection), 10.5 microns (310 reflection) , and 16.2
microns (732 - 651 reflections) respectively. On the other hand, interpretation of
data obtained by this method is not easy; the strains in the shallower depths are
also integrated by the x-ray beams penetrating to deeper layers. It is also possible
to utilize the curvature in d vs. sin 2 ", to determine the shape of the gradient by
curve fitting techniques. Several combinations of gradients in <1ij , however, may
cause the same curvature in d vs. sin 2 "" and the functional form (i.e. power series,
Fourier series,'cetc.) assumed to represent the variation of the components of the
strain/stress tensor with depth and the uniqueness of the solution obtained from
curve fitting must be carefully checked in order to obtain the true stress gradient.
The methods discussed above are limited in penetration depth by absorption.
Thus, they cannot be used to study the stress through the depth of the specimen.
This can be accomplished, however, by first measuring the stress at the surface of
the specimen and then exposing layers deeper into the material by removing the
surface through electrochemical or chemical polishing and repeating the stress
measurement. This is repeated until stresses through the depth of interest have
been examined. Mechanical methods, such as grinding, should not be used for
layer removal since they introduce residual stresses of their own and may cause
misleading results. If a mechanical method has been used to remove a large
quantity of material, the specimen should be electropolished to depths not affected
by the plastic deformation caused by the process. This permits access to the
original deformation distribution in the material.
Layer removal, whether by chemical or mechanical methods, causes rearrangement of the elastic strain/stress distribution within the material. For
example, if the plastically deformed surface layer in a shot-peened specimen is
removed by electropolishing, the residual stresses in the bulk will decay to zero
since the material responsible for the elastic constraint no longer exists (Sect. 3.2) .
Thus, x-ray stress values obtained from all polished surfaces must be corrected for
stress relaxation effects in order to obtain the correct strain/stress distribution in
the specimen. Such corrections may be obtained from elasticity theory, and will be
discussed for several geometries in Chap. 6. It must be noted here that electropolishing affects microstresses due to plastic deformation (Sect. 3.4) in a different
way; for example, if the grains of two phases mutually constraining each other are
polished away at the same rate, the volume fraction of both phases at the surface
will not change, and thus no relaxation of the micros tress in either phase will
occur. If, however, preferential etching removes one phase faster than the other,
relaxation of microstresses can also take place.
145
Fig. 5.15. A microcomputer controlled tensile device used in experimental determination of x-ray
elastic constants. A, tensile specimen; B, grips; C, diffractometer track; D, stepping motor;
E. load cell; F, gears; H, micrometer adjustment used in placing the diffracting volume over the
diffractometer surface. (From Perry et al. [371)
146
Here E~ is the homogeneous elastic strain that would be observed if the stress was
applied to a homogeneous isotropic material. The reaction strain component, E;j,
arises because of the variation of elastic constants along a given direction in the
surface plane of the sample (Sect. 3.4 ). The reaction strains depend on the
difference between the displacements, U b that have to be made compatible at a
point, and vary from point to point since the effect of surrounding grains at each
point is different. However, as long as the total stress at a point is lower than the
microscopic elastic limit at any point, the magnitude of the reaction stresses and
strains at any point will be directly proportional to the applied stress.
Thus, if a homogeneous stress CJ~l in the Sl direction is applied at the
boundary of the material, the components of the strain tensor at any point A in the
material may be expressed as
{1.
( 5.54a)
E13 (X,y,Z) =CJ~lK~(x,y,z)
E23 (x,y,z) = CJ~l'K~ (x,y,z)
Ell (x,y,z) =CJ~l'K~(x,y,z) .
Here x,y,z are the coordinates of the point A with respect to a coordinate system
describing the surface, and K; (x,y,z) are the proportionality constants at A
between the applied load and the resulting reaction strains. The constants
K~,K~,K~ may be finite depending on the symmetry of the constitutive grains of
the material or the symmetry of texture in the surface layers. Also, in certain cases
the local symmetry changes as one approaches a grain boundary. In the following
discussion it is assumed, for simplicity, that K~=K~=K~=Ol.
If the material also has an initial residual stress distribution caused by the
previous deformation history, the total elastic strain at a point, El j, will also have a
residual strain component in addition to the strains caused by the applied stress.
Thus, for this case, Eqs. (5.54a) become
(5.54b)
where Efj(x,y,z) is the residual strain at the point A(x,y,z).
Now assume that this material is placed (applied stress and all) on a
diffractometer and a beam of x-rays (whose edges extend from Xl to X2 along
Sl,yl to Y2 along::h and which penetrates a distance 't along S3 into the material)
1 If these terms are finite, the discussion follows along the same lines but the equations must be
modified to take into account the shear strains &13'&23'&12'
147
is used to measure the average strain along (L3 ) cjJ1jJ' From Eqs. (5.54b) and (5.4)
one obtains (<l> = 0),
(5.55 )
where the average strains, <Ei)~' in Eq. (5.55) are related to the strains at a point
through equations of the form of Eq. (5.43). [It must also be noted that because
x-rays penetrate to a different depth (z) for each tp-tilt due to absorption and, for
finite beam sizes, the intersection of the tilting specimen with the beam changes the
dimensions Xl -X 2'YI -Y2' the total irradiated volume.is also a function of the tilt
angle "tp". This means that parameters that are a function of volume such as K can
also be expressed as a function of tp.]
The evaluation of the average x-ray strains in terms of the strains at a point is
extremely complicated since the exact coupling terms in Eq. (5.54a) are not
known. However, by inspection of Eqs. (5.43), (5.54a,b), it can be seen that the
average strain may be written in terms of the average strain components
contributing to it:'
(5.56 )
or, in terms of stresses:
{1 ~v
A linear least-squares line fitted to the data described by Eq. (5.53), (as is usually
done in practice), implicitly assumes that the function,
(5.59 )
148
describes the relationship between d and sin 2tp. Here e is the random error
component. The regression parameters ~O'~l are then obtained from the equations
[30]
( 5.60a)
(5.60b)
where n is the number of tp tilts and
n
L sin2tpj
-'-2-
sm
j=l
tpj=~--
d",.
=
TJ
L ~J
j= 1 ':
(5.61 )
~-=-----
It must be noted that, if d vs. sin 2tp is oscillatory, the parameters ~O'~l cannot be
called "slope" and "intercept" of the least-squares line in the traditional sense
(e.g. as in the conventional analysis of linear d vs. sin 2tp plots). Here they are
simply mathematical functions described by Eqs. (5.60a,b)].
Substituting Eq. (5.58) into Eq. (5.60a) one obtains
~1 =~'{0"?1
L cf
.t
Cj[{( 1
)-1
j= 1
+ J.L= 1 Cj[{<ell>~J-<e33>~Jsin2tpj+<0"33>~J+1
n
- .L
J=1
(5.62 )
(5.63 )
where the function 82 [ (1
~ v) ,Kj (tp) ]
F ( <ejj)")
149
A similar equation can be written for ~o. However, this case is more
complicated and will not be treated here.
Equation (5.63) predicts a linear variation of the parameter ~I with applied
load cr? l ' This linear variation is independent of the shape of d vs. sin 2\jJ
(regular or oscillatory behavior) and thus of the distribution of residual
strains/stresses (homogeneous or inhomogeneous) in the irradiated volume.
Thus either linear or oscillatory data (Figs. 5.16a - d) will yield linear ~1 vs cr? 1
(Fig. 5.17). On the other hand, the cause of oscillatory behavior (Kj (\jJ) or
<Eij>~) is important in the interpretation of the x-ray elastic constants SI,S2/2.
In the case of a homogeneous, isotropic material, where the elastic interaction
terms K j ( \jJ) are equal to zero by definition, S2/2 will be equal to ( 1 ~ v )
independent of the particular distribution of residual strains, <Eij>~' in the
irradiated volume since these terms affect only the intercept term, F ( <Eij>~), in
Eq. (5.63). In the case of quasi-homogeneous materials (where all the grains are
distributed randomly) , such that along any direction all possible crystal directions
are encountered" and the same average elastic constant is measured, two
possibilities exist. In the first case, the elastic constant, S2/2, may be equal to
1 ~ v + Kj ( \jJ ) , where Kj ( \jJ) is an average interaction term that is the same in all
directions. Alternatively, the interaction terms may integrate to zero such that
S2/2 = 1 ~ v, where 1 ~ v is the average of the single-crystal constants. In all
cases, however, the term S2 will be isotropic in the irradiated volume. For inhomogeneous materials, Kj ( \jJ) are finite and inhomogeneously distributed
in all subsets. For such materials, the x-ray elastic constant S2/2 is equal to
-S2 (1E'
+v K (\jJ) ) gIven
.
by Eq. (5.62).
j
The terms K j ( \jJ) that may appear in S2/2 for inhomogeneous or quasihomogeneous materials are configurational parameters that are dependent on
both shape distribution of the grains and the texture in the irradiated volume.
Thus, when these terms are finite, S2/2 is a measure of the average elastic response of
the inhomogeneous material to an applied load cr? I' In these cases, S2/2 is not an
elastic constant (like Cjjkl,E,v) in the strictest sense. Rather, it is an "average
effective elastic constant" of the diffracting volume of inhomogeneous material.
Comparison of such values with values obtained from quasi-isotropic materials
can yield information about the deviation from "randomness" that exists in the
diffracting volume. The average nature ofS 2/2 in this case must also be emphasized.
It can be seen from Eq. (5.62) that both KI (\jJ) and K3 (\jJ) contribute to S2/2.
Furthermore, these terms themselves may not be constant in \jJ and vary from one
diffracting subset to another (this is the case if the oscillations are caused by
plastic deformation rather than <Eij>~!)' Thus, the interpretation of such
constants in terms of local reactions and elasticity theory is (in most cases)
difficult.
It must be noted that the linear response predicted by Eq. (5.63) is possible if
and only if no plastic deformation occurs during the elastic testing; plastic
deformation may cause total or partial relaxation of the elastic reaction strains at
1.3067 l-
.:: 1.3070
a
~ 1.3069
:;; 1.3068
1.3072
1.3071
"01.3067
~
1.3068
N
1.3069
1.3070
"01.3067
~1.3068
1.3069
1.307,0
0.1
ll.
b.
b.
0.2
b.
b.
b.
sin 2
0.3
PSI
b.
b.
b.
,.
b.
b.
I-
0::::7.4 Mpa
0.4
0.5
0.6
0::::97.2 Mpa -
b.
b.
0::::49.7 Mpa
b.
b.
1.2041
~ 1.2043
:;; 1.2042
1.2045 l-
1.2046
1.2041
.:: 1.2044
"0
~1.2042
1.2044
~ 1.2043
1.2045
1.2046
;:: 1.2041.
~ 1.2043
"01.2042
1.2041
1.2045
1.2046 l-
0.1
b.
b.
b.
0.2
ll.
b.
b.
0.3
sin 2 PSI
b.
b.
b.
"T
b.
0::::7.2 Mpa
ll.
b.
0.4
0.5
0::::9S.2Mpa
b.
0::::47.6 Mpa
b.
b.
...J
-I
'"
s::
=:I
a.
'"
>Tj
'"'"
Cf.l
8-
~.
Cf.l
o
...,
i.
VI
VI
1.1711
1.171L.
l-
l-
0.1
I!.
I!.
I!.
0.2
I!.
I!.
I!.
0.3
sin 2 PSI
I!.
I!.
I!.
I!.
I!.
O.L.
0.5
a==209Mpa
I!.
0.6
a==S.4Mpa-
I!.
a==10SMpa
I!.
I!.
I
<!
1.1700
1. 1696
1.1697
1.1698
1.1699 I-
1.1702
1.1696
1.1697
1.1698
-0
1.1796 I-
1.1798
:: 1.1700
-0
:: 1.1699
-0
1.1700 l-
0.1
I!.
0.2
I!.
I!.
0.3
sin 2 PSI
I!.
I!.
I!.
I!.
O.L.
0.5
a==192.Mpa
I!.
I:J.
a==10S.Mpa
.g
Ul
;...
w
tIl
0.6
Ul
--
!il"
(J
~
o.
o
g,
~.
~.
1- ~
a==S.Mpa
I!.
I!.
Fig. 5.16. "d" vs. sin 2 '1' plots at various tensile applied loads from (a) Ct-brass, (b) l3-brass, (c) 1008 steel, (d) 1075 steel. The specimens
were loaded in situ on the diffractometer with the apparatus shown in Fig. 5.15. (From Noyan [27])
1.1708 I-
U 1.1710 l-
::: 1.1712
<!
1.1708
1.1709
U 1.1710
1. 1712
<!
1.1713
1.171L.
1.1709
U 1.1710
1.1712
1.1711
<!
1.1713 l-
1.171L.
152
1l.1l1l16
1l.1l1l12
,..
~
)( +
B.IlIlIlB
II
II
1l.1l1l1l4
0
If.
)(
II
C>
1l.1l1l1l1l
a-Br.
p-Br.
1008
+1075
1
Sil.
100.
1SIl.
~1
21l1l.
the particular load, destroying the linear relationship between the applied load
and the reactien strainsl. The effect of plastic deformation, however, is not limited
to relaxation: extensive plastic deformation may cause changes in grain shapes and
grain orientations (texture) such that the elastic interaction components, K; ( tp ) ,
before and after deformation are no longer identical. Thus, if the "x-ray elastic
constants" of a specimen are first measured (with loads below the elastic limit as
discussed), then the specimen plastically deformed and the measurement
repeated, the interaction constants K; ( tp) and, thus, the x-ray elastic constants,
may change as a result of the plastic deformation. In the literature, changes up to
40 % have been reported for steels deformed in uniaxial tension [31]. These
changes are due to the changes in K; ( tp ), since E, v are not affected by plastic
deformation as discussed in Sect. 2.9.
If the material in the measurement volume also contains residual strains,
<Eij>~, the effect of plastic deformation on these strains must also be considered.
For example, if the local plastic deformation is such that the inhomogeneous
residual strains, <E;j>~' change, but the coupling constants are not affected, then
no change in th,e "x-ray elastic constants" will be observed even though the shape
of the oscillatory d vs. sin 2 tp plot changes. Even though such a residual strain (or
stress) distribution causes oscillations in d versus sin 2 tp, the residual strain
distribution itself is not a function of the elastic loads applied (after plastic
deformation) and will affect only the intercept of the ~l vS. cr? 1 plot [Eq. (5.63)].
Thus, it is not possible to determine the extent of the interaction effects on the
elastic constants just by observing the magnitude of the oscillations.
One other conclusion from this line of reasoning is that even if the oscillations
in d vs. sin 2 tp plots from two samples of the same material look alike, unless the
shapes of any precipitates that might be present and the distribution of
1 This property may be used to determine the microscopic yield point since the load at which
vs. cr? 1 deviates from linearity indicates non-elastic strain effects.
~1
153
o}
V
1 +V 0 . 2
{T
a l l sm tp- E all
+ { a? 1 [Kd tp) -
+ {[ <Ell>~ -
<E33>~]sin2tp + <E33>~}
(5.64) 1
In Sect. 5.13 it was shown that the first term in brackets in Eq. (5.64) is the
homogeneous strain that cause a linear variation of d with sin 2tp. The second and
third terms are inhomogeneous strain terms which cause the non-linearity in d vs.
sin 2tp. The second term is finite only when a? 1 ,Ki ( tp) are finite and describes the
average reaction strains to an applied or macro-stress in the population of grains
diffracting at the particular tp-tilt. The third term is the inhomogeneous residual
strain term in this population. This term may be finite, for example, if plastic
deformation is inhomogeneously distributed in the grains within the irradiated
volume such that various grains mutually constrain each other. The contribution
of all these terms must be taken into account for a general solution of the
strain/stress state in the irradiated layers.
Unfortunately, determination of the macrostress, a? 1, and the average
microstrains, <Eij>~' from Eq. (5.64) is not easy. If the interaction constants
Ki (tp) at each tp-tilt, as well as the functional dependence of <Ei)~ on tp are
known, d vs. sin 2tp plots may be analyzed by curve-fitting, or non-linear leastsquares analysis. However, in the general case, the equations describing
Ki ( tp ) ,< Eij>~ are not simple functions of tp and require the definition of a large
number of parameters 2 which can cause large errors in the results.
1 Here it is assumed that q, =0 and that only the applied and/or the macroresidual stresses cr? 1
are finite in the irradiated volume.
2 The interaction constants K j (II') are dependent on the texture function (which is usually
expressed as a spherical function [32]) and on the distribution of grain shapes in the given
population. The inhomogeneous residual strain distribution also depends on the texture
function (which determines the orientations of the grains) and on the type and direction of
loading during deformation (which determines the total load and consequently the plastic
deformation in grains of a definite orientation).
154
In special cases, analysis of oscillatory d vs. Sin2'l' may be easier. For example,
if the material under investigation has a large grain size such that a parallel-beam
geometry coupled with a PSD can be used to obtain the strain distributions in
discrete grains (similar to the apparatus described in Sect. 5.9) one can map the
average strains in discrete grains by treating each grain as a single crystal.
Similarly, if it is known, a-priori, that either of the components causing the
oscillations [terms II or III in Eq. (5.64)] is negligible, Eq. (5.64) may be
simplified accordingly.
Various other approaches have also been suggested to date for the treatment of
oscillatory d vs. sin2'l' data. These procedures are usually laborious and are based
on restrictive assumptions, however, and are of limited practical value. These
approaches are reviewed in Appendix B.
155
Diffractometer
/ ' Circle
Fig. 5.IS. Definition ofthe position and shape ofthe probe volume in a neutron experiment by the
divergent and receiving slit/soller collimator combination (a), experiment geometry (b)
Incident Beam
Diffracted Beam
Fig. 5.19 a-c. Spatial resolution obtained by various divergent and receiving slit combinations.
The dimensions of the probe region must be chosen such that there is negligible variation of
residual stress within the probe volume
section of the diffracting volume. By using various shapes of slits, the size and
shape of this volume may be changed (Fig. 5.19) to match the characteristics of
the strain distribution. For example, in Fig. 5.19b,c, the long dimensions of the
volume would be along the specimen direction where strains are relatively
constant with length. The height of the diffracting volume perpendicular to the
diffractometer plane is defined by the height of the slits as shown in Fig. 5.19.
The cross-section of the irradiated volume, on the other hand, is a rhombus whose
dimensions depend on the slit width, W, and diffraction angle, 29. The intersection
length of the rhombus along the specimen coordinates Sl,S2 also depend on '1'.
These relationships are summarized in Fig. 5.20. An interesting feature of the
neutron stress measurement is that in contrast to the x-ray methods, where 'I'
between 0 and 60 can be used for most experiments, any 'I' between 0 and 90
may be used as long as the path length within the material is not longer than the
critical absorption length that will decrease diffracted intensity to unacceptable
levels. It must also be noted that since neutrons penetrate deep into the material,
156
.,,=0
Xmin
Xmax
W = SLIT WIDTH
K = W/sln 28
Xmax =W/sln8
Xmax = W/cos 8
Xmln = W/cos 8
Xmln =.W/sln 8
L~." = Xmln
L~." =X max
Definition of
Specimen axes
28
. d,
, ,
-'_
'L '
'cfAIt
I
I
~ KI
L~." = Xmln cos."
all terms of the stress tensor, including (113,(123,(133' may posses macro and micro
components. Thus, the biaxial methods discussed in the x-ray measurement
should be avoided unless there is independent evidence (for example, from
elasticity theory) that for the particular specimen, these terms are zero. Similarly,
in materials subjected to surface treatments, such as shot-peening, grinding,
hardening, etc., where the variation of residual stress in the surface layers is steep,
the neutron beam should not border on the surface. In such cases, as discussed in
the previous sections, both the macro and micro stresses will be a function of
depth.
One other important consideration is the homogeneity of deformation in the
irradiated volume. As discussed above, this may be obtained from the behavior of
d vs. sin 2 tp. If, because of low diffracted intensities and long counting times,
measurement of d for a large number of tp-tilts is impractical, independent
confirmation from elasticity theory, finite element analysis, or x-ray measurements must be used as a check. The best method, however, is to use a position
157
Jz Jjj) macrodz = 0 ,
(3.5)
and the strains observed will be due to microstresses that are balanced between
various grains. These values will also be averages over the entire specimen volume.
Thus, materials that exhibit a deformation gradient from the surface into the bulk
should not be studied by this method. This method, on the other hand, has been
used successfully to analyze the average microstrains in the individual phases of
multi-phase materials where deformation is homogeneous through the sample
thickness [36]. Iftpeaverage strain in a given phase is inhomogeneous, however,
the results from this method are, as for all other methods discussed so far,
extremely hard to interpret.
Based on the discussion given above, one may conclude that x-ray and neutron
diffraction techniques of residual stress determination are complementary. By
using both these methods, which are sensitive to strain fields over very different
characteristic measurement lengths, it is possible to obtain detailed strain
information of the stress field in a given specimen. This has not yet been done.
158
where (ao) A> (ao ) B are the equilibrium lattice parameters of the solvent and
solute respectively, (a) S.s is the lattice parameter of the solid solution and fB is the
atomic fraction of the solute. Similar relationships apply for the other effects.
Thus, in most cases, it is possible to obtain empirical relationships, describing the
variation of the plane spacing, do, of any set of planes with composition of the
form:
(5.66 )
Here A,B are constants and nx is the solute concentration. In the case of austenite
and martensite, the dependence of the lattice parameters on the carbon
composition, nc, is given by [39]
.
c=2.861 + .116nc
a=2.861-0.013nc
for the body-centered tetragonal martensite structure and
a = 3.548 +O.044nc
for the FCC austenite structure.
Now consider the case where residual stresses are to be measured in the
austenite phase of a steel specimen in which the carbon concentration changes
from the surface to the interior (e.g., a caburized specimen). Assume, for
simplicity, that the residual stress tensor in the surface is biaxial. In this case, the
dependence of the measured plane spacing, d~, on the residual stresses is given by
Eq. (5.17):
d~",-do
. 2
(1-V) (all +( )
do = (1+V)
E
a~sm 'V+ E
22
(5.17 )
Here do is the unstressed plane spacing and the other terms have been previously
defmed. In this case, however, if the carbon concentration exhibits significant
changes over the maximum depth penetrated by the x-rays, the average
equilibrium plane spacing, do, measured at any 'V-tilt will be given by an equation
similar to that given for strains in Eq. (5.42):
J (A+Bnc(Z) )e-z/T'Pdz
Top
<do)~=
Tip
J e-z/T'Pdz
( 5.67)
Here nc (z) is the variation of carbon concentration with depth (z) and the other
terms are defined in Eq. (5.42). Thus, Eq. (5.17) becomes (by substituting
Eq. (5.67) and integrating)
159
It can be seen from this equation that, even when all the stress terms aij are
zero, d~ will change with tp-tilt creating a fictious stress. Thus, residual stress
values determined from such specimens must be corrected for the variation of
concentration with depth. This is possible if the actual concentration gradients
with depth and the functional dependence of equilibrium lattice parameters on
solute concentrations are known. In such a case, the terms K 1,K2 and <nc( t) >1p
can be determined from Eq. (5.67) after which Eq. (5.68) can be solved for the
correct stress values. A similar procedure can also be used for the triaxial formulas
[Eqs. (5.22) - ( 5.26). In this case, the procedure described automatically
corrects for the variation of the unstressed lattice parameter with depth. (On the
other hand, one must make sure that the total error introduced into the calculation
from the composition terms is within acceptable limits. This can be done by
straightforward propogation of error, similar to the procedures discussed in
Chap. 6.)
It must be noted that the effect described above will be pronounced only for
those cases where concentration changes appreciably over the penetration depth
for the radiation employed. This correction may also be especially important in
stress determination with neutron diffraction because of the much larger volumes
involved. Similarly, in the case of surface doped or irradiated thin films, or
otherwise surface treated materials with sharp concentration gradients, it may be a
consideration with x-ray diffraction. The use of highly absorbed, long-wavelength
radiations will minimize this effect, similar to the case discussed for the stress
gradients.
160
0'1
'u
Mechanical stress
a.
III
Q)
0..
a:::
5.18 Summary
From the discussions given in this chapter it may be seen that all diffraction
methods of measuring stress measure strains along various directions in the
specimen and then use these values to calculate the stresses along any direction
through tensor transformation formulae and the appropriate form of Hooke's
law. While this basic methodology permits the determination of general triaxial
5.18 Summary
161
162
Problem
5.1. Given the following "d" vs. sin21V data,
sin21V
d,A
sin21V
d,A
0.00
0.10
0.20
0.30
2.87206
2.87082
2.86965
2.86856
0.40
0.50
0.60
0.75
2.86753
2.86656
2.86563
2.86445
a) It is also given that dcp.p = d,p for all <1>. Plot "d" vs. sin21V, what can you conclude
from the shape of this plot? Describe the possible stress tensors. What can you
conclude about the strain distribution in the surface of the material?
b) Given tha~ the material is shot-peened steel
~ = 1.25 .10
MPa)
Determine the surface stress cr", using the biaxial sin21V method and the two
tilt method.
c) Using the triaxial analysis determine the stresses tensor over three IV-ranges,
sin21V=0-O.75, sin21V=O-O.3, sin21V=0.4-0.75. Assume d o =2.8665A.
d) Calculate the unstressed lattice spacing ( do) 'P* using the approximate formula
given in the text for the three IV-ranges. What is the error in do at each tilt?
e) Re-do (c) using do = ( do ) 'P*. Compare your answers with the results from
( c ); what are the errors.
References
1
2
3
4
5.18 Summary
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
163
A. Segmiiller and M. Murakami, in "Analytical Techniques for Thin Films", K.N. Tu and R.
Rosenberg Eds., Tratises on Mat. Sci. and Technology, Academic Press, New York (in
print)
M. Murakami, CRC Critical Reviews in Mat. Sci., 11, 317 (1983)
V.S. Speriosu and T. Vreeland, Jr., J. Appl. Phys., 56, 1591 (1984)
V.S. Speriosu, J. Appl. Phys., 52 6094 (1981)
A. Segmiiller, P. Krishna, and L. Esaki, J. Appl. Cryst., 10, 1 (1977)
A. Segmiiller, J. Angiello, and S.J. La Placa, J. Appl. Phys., 51, 6224 (1980)
U. Wolfstieg, Harterei-Tech. Mitt., 31 83 (1976)
I.e. Noyan, Mat. Sci and Eng. (in print)
e.M. van Baal, Laboratory for Metallurgy Report, Delft Uni. of Tech., Rotterdamsurg,
Netherlands (1982)
e.M. Brakman, J. Appl. Cryst., 16, 325 (1983)
V.M. Hauk, Adv. in X-ray Anal., 27, 101 (1983)
I.e. Noyan, Ph. D. Thesis, Northwestern University, Tech. Institute, Evanston II. 60201
(1984)
I.C. Noyan and J.B. Cohen, Adv. in X-ray Anal., 27, 129 (1983)
N.R. Draper and H. Smith, "Applied Regression Analysis", Wiley-Interscience, New York,
NNY (1966)
R. Marion, Ph. D. Thesis, Northwestern University, Tech. Institute, Evanston. IL 60201
(1972)
e.M. Sayers, Publication MPDjNBS/233, Materials Physics Division, Harwell Oxfordshire, England.( 1983)
L. Pintschovius, V. Jung, E. Macherauch, and O. Vohringer, Mat. Sci. and Eng., 61, 43
(1983 )
A. Krawitz, J.E. Brune, and M.J. Schmank in "Residual Stress and Stress Relaxation",
E. Kula, V. Weiss Eds., Plenum Press, New York, NY, 139 (1981)
C.W. Tompson, D.F.R. Mildner, M. Mehregany, R. Berliner, and W.B. Yelon, J. Appl.
Cryst. 17, 385 (1984)
A.D. Krawitz, R. Roberts, and J. Faber, Adv. in X-ray Anal., 27, 239 (1983)
W.B. Pearson, "A Handbook of Lattice Spacings and Structures of Metals and Alloys",
Pergamon Press, New York, 19-54 (1958)
C.S. Barrett and T.B. Massalski, "Structure of Metals", 3rd ed., McGraw-Hili, New York,
357-379 (1966)
C.S. Roberts, Trans. AIME, 191, 203 (1953)
S. Kodama, Proc. Int. Congo Mech. Behav. of Materials, Soc. Mat. Sci. Japan, Kyoto, 111
( 1972)
6.1 Introduction
The basic methods of residual stress measurements with x-rays and neutrons, as
well as the theory underlying the measurements, have been covered in the previous
chapters. In any scientific experiment, however, the error associated with the
measured quantity is just as important as the measured value itself and must be
known for the correct interpretation of the results. Evaluation of errors by
theoretical foanulae is also of primary importance in automating a measurement
such that the error in the measurement can be specified a priori by the operator.
In this chapter, the errors associated with the residual stress measurement will
be discussed. The discussion will be in two parts. In the first part, the selection of
the diffraction peak, methods of peak location and the statistiCal errors associated
with the maximum 28 value (and therefore the plane spacing "dcjl1jl") obtained
from these methods will be reviewed. This error will then be used to obtain the
statistical error in stress determined from the analysis of "dcjl1jl" vs. sin 2 \j.l data
through error propogation techniques. In the second part the instrumental errors
arising from diffractometer misalignment, specimen curvature and various other
geometrical factors, as well as errors due to specimen preparation techniques such
as electropolishing, will be reviewed and various techniques of minimizing such
arrors will be discussed. It must be noted, however, that the equations describing
the errors in stress/strain throughout the chapter have been derived assuming
regular "d" vs. sin 2 \j.l behavior and are not valid for oscillatory data.
165
700.-------------------------------,
MPa
""2"8
-+-__
- j -_ _
~~=35
500
500
t
~
400
I
I
I
300
I
I
Ktwotilt
Fe211
Cr
9Fig. 6.1. Variation ofthe stress constant K as a function of diffraction angle 9 for single exposure
and two-tilt methods
more sensitive to strains/stresses, i.e., for a given stress, a high angle peak will
display a larger shift in 29. This may be seen by differentiating Bragg's law:
nA.=2dsin9
0= 2d cos9L19 + 2L1d sin 9
or:
L19= -stan 9,
(6.1 )
L1d
s=d
Since tan 9 is larger for larger 9, the term L19 is larger for a given stress. It may be
seen from Eq. (6.1) that for a given strain in an iron specimen examined with Cr
radiation, the peak shift of the 211 peak at 1560 29 will be 3.6 times the peak shift of
the 200 peak at 1050 29 and 6.9 times the peak shift of the 110 peak at 680 29.
Because of this effect peaks with 29 values above 1400 are preferred for routine
stress measurements. It may be noted that, the term tan 9, which causes this
behavior, also appears in the stress factors K for the single exposure and two tilt
methods [where 0" = KL19, Eqs. (5.19), (5.20)]. Thus, the stress factor also varies
166
with 29. In Fig.6.1 the variation of K for steel specimens over the 29 range
frequently used for stress measurments in steels is shown. It may be seen from this
figure that the sensitivity of different methods to strains/stresses are different even
over the same angular range (the higher the term K, the poorer the sensitivity) .
dcj>1jl-d o
do
'
(5.1 )
where do is the ll;nstressed lattice spacing. Since the strains Eij are less than .01 % for
elastic behavior in most materials, the absolute value of the peak position, i.e.,
b
a
Fig. 6.2. Intensity vs. 29 profiles obtained from an (a) annealed and (b) cold-worked 1090 steel
specimens
167
the true peak maximum, is required for the accurate calculation of d..., from
Bragg's law and an appropriate method of peak location must be used [1].
In the following the various methods of peak location are reviewed. In all cases
it will be assumed that the appropriate angular corrections to the raw intensities
have already been performed.
(6.2)
where x 112 is the intersection of the profile and the straight line parallel to
the background at half the maximum intensity after the background has been
subtracted (Fig. 6.3a) .
In the centroid method, the center of gravity or centroid of the peak is defmed
as [2]
J29 I ( 29 ) d29
(6.3)
(29)peak = II (29) .d29
The centroid of a given profile may be calculated by a procedure proposed by
Baucum and Ammons [3]. This procedure is based on Simpson's rule for the area
under the curve. Consider the profile given in Fig. 6.3b. The centroid of this profile
is given by
k
LIDj
;=1
(6.4 )
X=-k-'
LA;
;=1
where
X;-h...J
x;
LX;+h
x-
a
b
Fig. 6.3. Calculation of the (a) half-value breadth and (b) centroid of a diffraction peak
168
and
=11=
of data points - 3 + 1
2
(6.5 )
since three data points are required for the first incrment and two are required for
the rest.
6.3.2 Functional Representations of X-ray Peaks
The methods in this group represent the x-ray peak as mathematical functions
which can approximate the various peak shapes encountered in practice with
simple modifications. These functions are expressed in terms of various parameters describing the peak shape and location. These parameters (which also
include the peak maximum) are then determined by matching the function to the
observed peak profile. Among the functions used for this purpose are the
modified Lorentzian [4, 5], Pearson type VIII [4, 6], Gaussian and Cauchy [4,
7] profiles.
The modified Lorentzian is one of the more popular functional forms used in
profile fitting [4, 5] and its applicability to peak location determination has been
investigated by Devine [4]. The function is of the form
1(28);=A { COS1t
( 28i - 28p a
())
}n . K2+ (28.-28
K2
)2 +SL28 +INT.
i
(6.6)
Here, I (28i ) is the calculated intensity profile, A,a,8 are parameters related to
the shape of the line profile (where' A' is related to the maximum intensity at the
peak, 'a' is related to the full-width of the profile from background to background
and '8' is used to account for small asymmetries in peak shape) , K is a constant
Lorentzian term and 28p ,28i are the two-theta values at the peak and at position i
along the profile respectively. The cosine term raised to the appropriate power 'n'
is used to force the curve to drop more rapidly in the tail regions of the line profile.
The terms SL and INT fit the tails of the peak profile to the background. If the
background is approximated by a straight line under the peak, SL is the slope of
this line and INT is the intercept respectively. This function generates profiles that
fit well to most observed x-ray line profiles (Fig. 6.4 ).
The Pearso~ Type VII function [4, 6] is of the form
1(28).=1 . {1 + (28i -28p )2} -m + SL28+INT ,
I
0
ma 2
I
(6.7)
where 10 , and a are constants optimized in the profile fitting process, the power
term 'm' is user-defined according to the sharpness of the peak, and the other
terms have been defined in Eq. (6.6).
169
.. .
1200
:c
'iii
Observed
Calculated
1000
:s
<lJ
800
600
i.
.
0067.6 0
00
..
..'.
.. .
'
... '
'
'
68,0 0
68.i.
68.8
26-
69.2
69.6
Fig. 6.4. Modified Loientzian function fitted to the 110 ferrite peak obtained from a cold-worked
1008 steel sample. (From Devine [4] )
(6.8)
This can be seen by expanding Eq, (6.7) in the form of a binomial series:
1(29d = 1 - m + ( - m)( -1) - m -
1.
X+ m ( - ; - 1 ) ( -1) - m - 2X 2 + ... ,
j
p
d ' fi'
h'
. b
h
were
x = ( 29 - 29
2) 2' A
S m ten s to In Imty, t e IntensIty ecomes
rna
1(29.) =1 '{1
I
+.
(29j~229p)2}
170
...;.ii ..,
1200
cps
Pearson type-m
900
I'
I'
,.
'
I'
:c- 500
......
'\Ii
c(\)
C
....
A; q~served
D:
.:
300
O.
aO., am:1
DD
DD
...
DO
"AOD
m=2
-3005~7~5~0--~5~8.-0~0----5~8-.4~0-----5L8.~8~--~5~9.-2~---5-"9.50
28Fig. 6.5. Pearson':type VII functions with m = 1,2, and 3 fitted to the 110 ferrite peak shown in
Fig. 6.4. (From Devine [4])
500r----------------------------------,
400
>.
300
~
c(\)
:s 200
100
-.-
I
r
/
,,---
.......
53.00
53.50
29-
54.00
54.5 0
The functions based on the Pearson type VII function are easier to use than the
modified Lorenzian because of the smaller number of unknown parameters. These
functions, however, do not exhibit as good a fit as the modified LQrenzian
function (Fig. 6.5 ) .
Various mathematical procedures may be used in fitting the functions to the
observed proflle. In the case of the simpler functions [Eqs. (6.7) - (6.9)] the
solutions may be found using either first or second order differential techniques
such as nonlinear least-squares procedures. In the case of the modified Lorentzian
function more complicated procedures must be used because of the larger number
171
of unknown parameters involved [seven in the case ofEq. (6.6)]. Devine [4] used
a modified "simplex" method, capable of handling up to twelve parameters, in this
case. Similar routines are also available in various program libraries. In the case of
neutron diffraction, the peaks are Gaussian in shape [8] (Fig. 6.6) and other
functional forms are not used.
6.3.3 Peak Determination by Fitting a Parabola
This method, which was first used by Ogilvie [9], is one of the most popular
methods today. In this method, it is assumed that a region in the vicinity of the
peak can be represented by a parabola. Expanding the Cauchy [Eq. 6.8 )] or the
Gaussian [Eq. (6.9)] functions as power series,
I ( 29i ) = 10 - 210 (2 9i - 29p) 2 + ...
a
(6.12 )
for the Gaussian case and similarly for the Cauchy equation.
If the third and higher order terms are neglected, it is seen that both equations
assume the form
(6.13 )
where C is a constant. Equation (6.13) is the equation for a parabola whose axis is
parallel to the intensity ordinate. Therefore, the peak position can be determined
by measuring a number of points (intensity vs. 29) along the peak profile, fitting a
parabolic equation to the measured data and determining the apex of this
parabola. Two factors are critical in this procedure: the region of parabolic fit and
the number of points used in fitting the parabola.
The region of the diffraction profile which can be fitted by a parabola is not
well defined. Thomsen and Yap [10] have shown that, for x-ray profiles
satisfactorily represented by the modified Lorenzian function [Eq. (6.6)], a
parabolic assumption is valid when the parameter V, given by the function
(6.14 )
is less than 0.32. Here W is the full width at half the maximum height of the
diffraction profile, Z9p is the peak position, 29min is the minimum 29 that is within
the parabolic region and it is assumed that the peak is symmetric around 29.
An empirical rule proposed by Koistinen and Marburger [11] indieates that a
parabola should be fitted over the region of the peak which is bounded by the
points that have 85 % of the maximum peak intensity (Fig. 6.7). This so called
"top 15 pct." rule has found wide acceptance in practice since, in contrast to
Eq. (6.14), the. total peak profile need not be determined accurately. Furthermore, both methods yield similar results for most cases as shown in Table 6.1
[12].
The number of points measured in the appropriate 29 range and used in
calculating the parabola describing this region affects the reproducibility of the
apex of the parabola, i.e., the calculated peak position. Originally Kostinen and
172
1200. en
Q.
900.-
..
>-
I-
en
~
600.1-
IZ
H
,.
.. ..
Observed
Calculated
'
..
300.1-
68.8
69.2
28_
Fig. 6.7. A 7-point parabola fitted to the top 15 % of the peak shown in Fig. 6.4 and 6.5. (From
Devine [4])
68.4
68.8
Table 6.1, Region of parabolic fit for the 211 Diffraction peak from various criteria. From James
& Cohen [12]
Steel
specimen
29 min
Eq. (6.15)
(29)
29 min
15% rule
CZ9)
29 min
15% rule
after background
subtraction (29)
1090-1
1045-1
1045-3
1045-2
1090-2
TBAG-5
0.45
1.5
3.4
5.1
6.0
5.8
156.07
155.65
154.99
154.68
154.50
154.33
156.05
155.61
154.76
153.20
152.67
152.69
156.05
155.65
154.93
154.40
154.16
154.29
60
3.5
2.0
2.6
1.3
1.3
156.14
155.89
155.63
155.50
155.46
155.29
Marburger [11] suggested the fitting of a three-point parabola to the top 15 pet. of
the peak. Further work by Marion and Cohen [13] showed that reproducibility
was dramatically improved by the use of multiple points. This was later confirmed
by James and Cohen [12,14], who showed that given a fixed time for data
accumulation, use of multiple data points (five or more points, typically seven
points with background subtraction is used) could improve the reproducibility by
a factor of three.
The formulae describing the parabola fitted to a given angular range may be
derived in the following manner [14]. Assume that the data is obtained at an odd
number of observation points, spaced at equal increments of29. Thus, there are 'n'
points on each side of the center point (usually termed the working origin) and
173
the total number of points is 2n + 1. If the increment between the points is 3, the
parabola to be fitted to these points is defined by
a+b3j+c3 2j2=Ij
(6.15)
01.
J
-0
o( 3j) - .
(6.16 )
The parameters a,b,c in Eq. (6.15) are obtained from a least-squares best-fit to
the data by minimizing
(6.17 )
with respect to the unknown parameters a,b,c. Equation (6.17) may be solved by
setting the partial derivatives of S with respect to a,b,c to zero.
For example: .
as
where ni =
j=-o
j=-o
j=-o
j=-o
(6.18 )
j=-o
Mi =3i + 1
L {Ij
(6.19)
j= - 0
=0
( 6.20)
n2a+0+n432c-3-3M2 =0.
Simultaneous solution of Eqs. (6.20) for a,b,c yields
a= (Mon432-M2n2 )/(nOn4 -n~)33
b=Mt/3 3n 2
(6.21 )
c= (n232Mo-M2nO)/( 35 (n~-nOn4) .
The apex of the parabola is [from Eq. (6.16)]
2ep = 2eo- b/2c ,
( 6.22)
where 2eo is the working origin. Thus, from Eqs. (6.22) and (6.21), the peak
position (that is, the apex of the parabola) is given by
(6.23 )
174
positions
step and
accummulate
move to
maximum
intensity
position
wgff~rl\
no
intensity
corrections
and curve
fit
calculate new
stePa~aan
step increment
and preset
counts
accummulate
data
Fig. 6.8. A typical flowchart for fitting a parabola to the top 15 % of a diffraction peak. (From
James [14])
175
The parabolic fit lends itself well to computer controlled data acquisition and
various software packages are available for such a fit. A representative flow chart
is shown in Fig. 6.8.
James and Cohen [12] have shown that subtracting of the average background from measured intensities before the parabolic fit is applied increases the
reproducibility of the peak position. The point where the background value is
determined is not critical in this case since it only affects the range over which the
parabola is being fitted and an approximate value for the 28, as well as for the
intensity, may be used.
6.3.4 Determination of Peak Shift
The methods discussed above determine either the true "peak" location or the
position of a reference point on the peak profile at any given 1.p-tilt. Peak shift
determination methods, on the other hand, determine the angular shift, A28, of
this point upon tilting. Significant among such methods are the "difference" and
"cross-correlation~ methods.
1) Difference Method
This method, originally developed for film methods [15], compares the variation
of intensity over the total profile for two 1.p-tilts and yields the angular shift, A28, in
the peak-maximum between these tilts. The difference function D (A) is defined as
[16]
D (A) = J[10 (28) - J'l' (28-A) ]d28,
(6.24 )
where A is the step size, 1,I'P are the intensities at 28 for 1.p = O,1.p respectively. The
peak-shift A28 is the value for which D(A) is a minimum [aD(A)/aA=O].
If a position-sensitive detector or a step-scanning counting method has been
used in the data acquisition such that, instead of a continuous profile, a discrete set
of points are available, Eq. (6.24) becomes [16]
Dr =
L (I
j;
j -
(6.25 )
,:l28''I'=C { k+
L Dj(j-k) }
j;k
'
(6.26 )
j~k Dj
where C is the increment in 28.
The difference method can also be used in a multiple 1.p-tilt procedure by
referencing the profiles obtained at all tilts to the profile of the initial1.p-position,
1.p0. If the peak position at the initial1.p-position is known, this method may also be
used to determine the absolute values of 28 at all other 1.p-tilts
(28~=28~ +A28''I').
176
2) Cross-correlation Method
The cross-correlation method also yields the peak shift .12<]> of the intensity
maximum between two tp-tilts. In this case a correlation function F'" (.129) is
defined such that [16, 17, 18]
F'" (.129)
00
J 1 ( 29 ) .I'" ( 29 -
(6.27 )
.129 ) d ( 29) ,
-00
where 1, J'l' are the (corrected) intensities at tp = 0 and tp = tp and .129 is the step
size.
/:,.-
(step size)
28-Fig. 6.9. Shift of the x-ray diffraction profile upon tilting in a stressed sample and the maximum in
the cross-correlation function P'
0.5 . . . - - - - - - - - - - - - - . ,
en
g-
0.4
~ 0.3
en
~ 0.2
I-
0.1
0.0
0.0
128.0
256.0
384.0
512.0
CHANNEL No.
0.5 . . . - - - - - - - - - - - - - . ,
en 0.4
Co
(,)
>- 0.3
I-
en 0.2
z
I-
z 0.1
H
0.0
0.0
128.0
256.0
384.0
CHANNEL No.
512.0
177
20.0.----------------.,
16.0
UJ
12.0
Q.
*
UJ
Q.
8.0
4.0
0.0
-500.0 -300.0
-100.0
100.0
300.0
500.0
CHANNEL INDEX
The function P exhibits a sharp maximum when the unknown peak shift
is equal to ~2e (Fig. 6.9). Furthermore, when the peak profiles are
similar in height and breadth, F'P is symmetric about ~2eQ,'P [16].
If, instead of a continuous profile, the data is measured at n discrete points
spaced in equal intervals along the profile for each 'V-tilt, Eq. (6.27) is replaced by
a summation [16, 17]
~2eo.'P
Fj= L Ip-Jr- j
(6.28 )
i= 1
and the function Fj must be evaluated at all points along the line profile. Once the
Fj vs. ~2e profile is evaluated, the position of the maximum in Ft can be estimated
from the center of gravity [16]:
1
~2e'P=C {k+
,L Fj.(j-k)}
j=k
LP.
j=k .J
( 6.29)
In Fig. 6.11, Fj evaluated from the line profiles shown in Fig. 6.1 0 is shown. It can
be seen that the profile is quite symmetric and exhibits a sharp maximum even
though the intensity profiles are not smooth.
The procedure described above may also be used in a multi-tilt procedure. In
this case, a series of cross-correlation functions are obtained by referencing the
line profile at any 'V-tilt to the profile measured at the preceding tilt [17]. The
peak position at any 'V-tilt is then given by
(6.30)
178
Here 28"', 28",-1 are the peak positions of the proflles measured at the nth and
n_lth 'V-tilts respectively, and d28",-1,,,, is the peak shift calculated from these
proflles by Eq. (6.27). Of course, the peak position of the first proflle must be
determined by one of the methods previously discussed if absolute 28 values rather
than peak shifts are required in the subsequent stress analysis.
+2
( 28i - 28 - 0) ] n
K2
a p
'K2+ (28i -28p )2
cos 1t
+ SL28i + INT.
In
K2
. K 2 + (28i - 28p - d )
(6.32 )
179
360
..
',',1"%0
0
.0
::- 300
0
0
'Vi
0
0
"
D _.
..
"
06"
:5 21.0 -
'
o~
.
0>
.D
a
..
..
""
,"D~
180
..... "'00
;I
120
1.50
<> "
<> "
.- -. '.
cps
1.00
o~
',
,
a.
ca,'
350 -
....C
300
0
0'
a'
a
00 , --,
0
0"
"
o.
o
250 -
a.
o
"'
'Vi
~
0 ,
<>
00.
.!> .
200 rb
I
150
11.3,1 11.3,1.
11.1..6
11.1.,9 11.5,2
Fig. 6.12. Modified Lorentzian function fitted to the 211 peak from the p-phase of 60 - 40 Brass
(a) with doublet term [Eq. (6.32] ) and (b) without doublet term [Eq. (6.6)]. (From Devine
[4] )
+
Z9 K
([1
29
,R
29 K
"' I
29 K
"'2
Z9 K
29
IXI
Fig. 6.13. Summation of two peaks (K."K. 2 ) and the shift in the apparent maximum of the
summed-up peak. The shift is proportional to the relative intensities of the peaks and to the halfwidth of the summed-up peak
180
H.W.
100
Correction
for
220 peak
0 - brass
28 K = 122.550
01
.050
Fig. 6.14. Variation ofthe peak shift with half-width in degrees 29 for (a) the 220 peak for IX-brass
and (b )211 peak for l3-brass. It may be seen that the correction is also a function of the 29 range
directly read from the chart for any given halfwidth. If such a correction is used, the
wavelength employed to determine the lattice spacing corresponding to the peak
position from Bragg's law must be that of Kill' not the weighted average of
K lll -K..2
Other methods of peak determination such as the centroid, etc., also require
this correction. The cross-correlation function discussed in Sect. 6.3.4, on the other
hand, is a symmetric function even for asymmetric peaks and does not require
6.5 Statistical Errors Associated with the X-ray Measurement of Line ProfIles
181
tIN.
cr 2 (X) = (dX)22
dX 1
cr (xd
+ (dX)22
dX 2 cr (X2) + ...
dX dX)
+2 ( dx l 'dx 2 COV(X 1 ,X2 )+ ...
(6.33 )
plus higher order differential terms. Here cr 2 (X) is the variance of X and
cov (xj,Xj ) is the covariance between variables Xj,X j. Neglecting the higher order
differential terms, Eq. (6.33) becomes
dX) 'cov(Xj,xj ) .
cr 2(X) = ~ (dX
-d '-d
1,]
Xj Xj
For linear functions, X =
cr 2 (X)
= L:afV(xd .
j
(6.34)
(6.35 )
The count rate, Ij == Xj is a random variable having a finite variance. Thus, all
quantities obtained by manipulating it also have a finite variance. Since the
182
(6.36 )
( 6.37)
This equation is also accurate for non-linear functions if the standard deviation of
the mean is small (less than 20 % of the mean);
From Eqs. (6.23) and (6.37), and substituting the counting rate I j for Xj one
obtains
0"2(29p ) =
)2
t ( d29
dI j
.0"2(Ij)'
P
(6.38)
The variance of the peak is dependent on the variance ofthe count rate, I j, which in
tum depends on how the data are accumulated. The two common methods of
determining the counting rate I j at the diffractometer setting 29j are the fixed time
and fixed count techniques. Defining tj as the time of data accumulation and C j as
the accumulated counts:
Ij = Cit
Ij = C/tj
(6.39 )
The variance (which is the square of the standard deviation) of the count rate is
derived by Wilson for both cases [19]:
( 6.40)
Equations (6.40) predict an asymptotical approach to the true value of the count
rate with increa'sing time or total number of counts collected. This behavior is
shown in Figs. 6.15a,b. It can be seen that there is a very good match between
measured and predicted errors for both cases.
The differential in Eq. (6.38) is now derived. Rewriting Eq. (6.23),
29p =290 and
(52 (n~-nOn4) {
2
2
Mt/(n 2() M o -noM 2 )}
n2
where
aMI = ()I"+1'"
__
J'
OIj
(6.41 )
(6.42)
6.5 Statistical Errors Associated with the X-ray Measurement of Line Proflles
183
50
+ Observed
o Statistical
Vi ['0 C
::l
0
U
-=~ 30 "a;
en
: 20
c:
j
II
::l
0
Gl
!jl
10 _
rIlJjl
I!!
0
L.OOOO
II
120000
80000
Counts
160000 200000
[,2
35 ~
+ Observed
o Statistical
Vl
628 i-
u
L
~ 21 i-
en
c:
1[,
i-
+
0
+
0
7i-
b
0
!jl
10
20
30
Time
III
I
['0
50
s 60
Fig. 6.15. Comparison of statistical error in intensity measurements with observed error for (a)
fixed counts and (b) fixed time measurement
Combining Eqs. (6.38), (6.40), and (6.44), the error in peak location due to
counting statistics can be obtained.
For accumulation of data by fixed time (at each observation point j) the
formula is
2
o4(n~-nOn4)2
cr (2ap ) = 4n~(n202Mo-noM2)4
n
j= -n
where cr ( 2ap ) is the standard deviation in the peak position and the term Mi is the
ith moment of intensity about the peak. For perfectly symmetric peaks the odd
moments of intensity will be zero and for small deviations from symmetry (at least
184
Table 6.2. Comparison of exact statistical formulae to approximate formulae for the counting
error in peak location using a parabolic fit". (The data is corrected for Lorentz-polarization and
absorption factors as discussed in Sect. 3.2 )
0"
er( 29p )
er(29p )
W
% Chang!
("29) (29) Eq.(3.32) (29) Eq.(3.33) (29) in er(29p )
Sample
II'
Degrees
1090-1
0
0
45
45
3
7
3
7
0.11
0.03
0.15
0.05
0.45
0.45
0.50
0.50
0.00085
0.00105
0.00139
0.00181
0.00085
0.00105
0.00139
0.00180
0
0
0
0.3
TBAG-5
0
0
45
45
3
15
3
15
2.83
0.38
2.35
0.38
6
6
6
6
0.01023
0.0134
0.0147
0.0146
0.01023
0.0133
0.0147
0.0144
0
0.8
0
1.37
No. of data
points
" 0 represents the 29 step increment between data points. W is the full width at halfthe maximum
intensity. The o/er. change represents the pet. difference in 29p between the statistical errors as
calculated from Eqs. (3.2) and (3.3). From James & Cohen [12]
in the peak region being fitted by the parabola) these terms will be negligible. In
such cases Eq. (6.45) becomes
2 9 _
04(n~-nOn4)2
n!:2
2 4'2
cr (2 p) - 4.. 2( 02M
M )4.L (n2u Mo-noM2) 0 J Ij
0 - no
2 J =- n
t n2 n 2
04 (n~ - nOn4) 2
4-t-n~(n202Mo-noM2)2
'04
f.
j=-n
j2I.
J
05 (n~-nOn4)2'M2
= 4.t'nHn202Mo-noM2) 2 .
(6.46 )
j= - 0
-n 203 M 1 ) 2If/C.
( 6.47)
2(29 ) _
P
08(n~-nOn4)2
0'2 2
4Cn 2(
02M 0 - no M 2 )2 J. =L- 0J I j .
2 n2
(6.48)
The validity of Eqs. (6.45) - (6.48) have been checked experimentally by James
and Cohen [12, 14] (Table 6.2). In practice however, the exact formula (6.45)
or (6.47) should be used. Although longer, these equations are easily in-
6.5 Statistical Errors Associated with the X-ray Measurement of Line ProfIles
185
corpora ted into software for microcomputer controlled experimentation and take
into account the presence of some asymmetry in the peak profIle.
Similar procedures may be utilized to determine cr 2 (2ep ) for the other
methods of peak location. For example, for the cross-correlation method the
variance in peak shift due to counting statistics is [16]
cr 2 (A2e) =
1(a (:~je) )
2 cr 2
(6.49 )
(Fj ) ,
where
(6.50)
and
cr 2 (Fj ) = L
i
{(12
(lP) + cr 2 (lr- j ) }
(6.51 )
cr' (Ale"") ~ t
'cr' (F
j ) ,
(6.52 )
where
(6.53 )
The calculation of the error in the case of the functional representation is not as
straightforward as the methods discussed above. A much larger number of
parameters are involved and propagation of error through non-linear regression
procedures may be necessary. One other problem associated with these methods
arises directly from the large number of definable parameters; the calculated
solution may not be unique and may not be the correct one.
In the discussion above, the general methods of peak location and the errors
associated with them have been discussed. There are numerous articles comparing
these methods for general and particular applications and usually there is little
agreement as to the"best' method of peak location for particular cases, although
the work by Knuuttila [16], James and Cohen [12, 14] and Devine [4] indicates
that the parabolic fit is usually the best choice. This method, and the error
equations associated with it, has been extensively treated in the literature and may
be used with confidence in most cases. In general a parabolic fit with 7 or more
points to the top 15 % of the peak with background correction appears to be the
most versatile method that can be applied over a wide range of peak shapes with
186
minimal error. The effect of doublet correction must be taken into account if the
stationary slit method is used.
6.6.1 The
8in 2,&,
Technique
In this method, the residual stress ad> is determined from the slope m of the
interplanar spacing "<1,.," vs. sin 2tp (Sect. 5.5). The terms "<1,.," are obtained from
the 29 values determined from the measured line profIles and, thus, will also
contain statistical errors. The variance in "<1,.," due to a 2 (29p ) can be determined
through Bragg's law:
(6.54)
nA = 2<1,.,sin 9p
From Eqs. (6.35) and (6.54),
a
2 ( rl
..",
~) 2
180'
(6.55 )
where 29 is in degrees and a 2 (29 p ), the variance in 29p is determined from the
variance equation for the particular method of peak determination [Eqs. (6.45),
( 6.47) for example]. The surface stress is given by m', the regression coefficient
describing the slope of a least squares line fitted to the data
a.
L
m'=
(Yi-Y)
L{Xi -X)2
(~-x)
(6.56)
Here x is the independent variable (sin 2tp) and y is the dependent variable (<1,.,).
Assuming that tp is determined exactly (this is a valid assumption for a well
aligned diffractometer and a flat sample) , and that all <1,., are measured to the same
precision, i.e., a 2 ( <1,.,) is constant (this would be approximately the case if a fixed
count procedure was used for all profIles) , the variance in m' is [from Eqs. (6.35)
and (6.56)]
a 2 (m') = -=Nc:..::..,F-------~,___-
N..,
(6.57)
187
where cr 2 ( d,.,) is given by Eq. (6.55). The surface stress cr, is given by
(6.59)
where the stress constant K is given by
K=
( 1 + v) . sin 2 ",
( 6.60)
If the peak shift is small, the two-tilt equation is commonly expressed in terms of 28
[Eq. (5.19)]. The variance in surface stress cr, in this case is given by
(6.61 )
In this equation it is assumed that the stress constant K' [which is, in fact a
function of 28, Eq. (5.20)] is known exactly. This assumption is valid for small
errors in 28.
188
2
( d a l ) 2 2 (d
)
.(J (d",'I'+)+ d(d",'I'_)
.(J
"''1'-
dal ) 2 2
+ ( dd o
. (J (do).
(6.63 )
(6.64 )
where the variance of the terms d~+,d~- are given by Eq. (6.55). Thus, the
variance of the slope of the a l vs. sin tp plot becomes [from Eqs. (6.55), (6.56),
( 6.57), (6.64)]
(6.65 )
(6.66 )
The triaxial analysis determines the strain E33 from the intercept of a l vs. sin 2tp.
The intercept la" of the least-squares line is given by
-.= L:(al )i
Y
,
(Na,) ,
No. of tp-tilts.
( 6.67)
la, =Yi-ma,X;,
N a ,:
The variance for the intercept of a l vs. sin 2tp can also be determined from the
application of Eq. (6.34) to Eq. (6.67). Determination of strain terms usually
involves the slopes of a l vs. sin 2tp at various <1>, for example for E 12 :
(6.68)
If this value is experimentally determined, the error term must be evaluated from the particular
"do" determination method and substituted in Eq. (6.63).
189
Thus, the variances of the strain terms are then determined from the variances of
the slopes of a 1 vs. sin2\j.l for tI> =0,45,900 and from the variance of the intercept
at a given tI> tilt. The variance of E12 is
cr 2 (E 12 ) = cr 2 (la!)4> + cr 2 (ma.)4>=45 + ~ (cr 2 (rna.) 4>=0 + cr 2 (rna! )4>=90) ) .
(6.69 )
After the strains are determined, stresses are determined from Hooke's law:
( 6.70)
The errors in stress can be determined from the propagation of the error through
Eq. (6.70) for any particular case.
6.6.4 Statistical
~rrors
In the procedures discussed above, it was assumed that the elastic constants viE,
( 1 + v) IE or CjjkJ have no errors associated with them. If, however, the x-ray
elastic constants 8 1 ,8 2/2 (8ect. 5.13) are used in the analysis, the error associated
with these terms must also be included in the overall analysis. In the following
formulas that can be used in evaluating the statistical errors in 8 1 ,8 2/2 are
discussed.
The experimental evaluation of 8 1 ,8 2/2 and the errors associated with this
measurement have been discussed by Perry and co-workers [21, 22] and was
reviewed in 8ect. (5.13). The basic flowchart of the measurement is shown in
(Fig. 6.16). Using the procedures discussed above, the error in the slope of the
"m" values versus applied load (Fig. 6.16b) will be
cr 2 ( mil) =
L [( crOPI No-a [
No-a
crOPI) 2 cr 2 (m j ) ]
2] 2 '
(cropi - crOPI)
(6.71 )
where N"a: no. of applied loads, cr4>1 is the applied load at ith experiment, and
cr 2 (m') is given by Eq. (6.72). The error in 8 2/2 is
cr 2 ( 82 /2)
cr 2 (mil)
(6.72 )
= ( do ) 2
1
cr 2 (8 ) 1 -(d o )2
L
No-a
[(crop-crop)2cr 2 (d'V=0)]
(
[L(crop-crop)2]2
6 73 )
.
No-a
\j.l =
0 at all
190
d
a'opp
./
= a'<t>1
, ------,
i) Data acquisitron
b
Analysis
191
(6.74a)
RGC
2sin9
for 1.1' = O. The correct focusing position is maintained in diffractometer by the 1:2
ratio of the 9/29 movement at all times. If, however, the specimen is rotated
around the center of the diffractometer such that 1.1' =F 0 (Fig. 6.18) , as in a stress
measurement, Eq. (6.74a) becomes
R
FC
RGC
(6.74b)
2 ( sin 9 +"'P )
Since the radius of the focusing circle changes with 1.1', the rays arriving at A will be
defocused and the mean position of the maximum intensity will be shifted,
creating an error in 29. One method of avoiding this error is to move the receiving
slit to the focusing point B. The distance from the sample to B is given by
R' - R
p-
Fig. 6.17
GC
. cos{l.p+ (90-9)}
cos{l.p- (90-9)}
E
0/=0
(6.75 )
Fig. 6.18
t=l/t
Fig.6.17. Focusing geometry for a specimen of ideal curvature for '1'=0. Here GC is the
goniometer circle and FC is the focusing circle
Fig. 6.18. Focusing geometry for a divergent beam when a specimen of ideal curvature is rotated
ljJ-degrees from the normal focusing position. It may be seen that the radius of the focusing circle,
and thus the radius of curvature for such an ideal specimen, is different than the one required for
focusing in the normal condition (Fig. 6.17)
192
This procedure is called the "parafocusing method". To maintain true focusing, the
position of the receiving slit must also be changed with 28 (at a given tp) as the line
intensity is being recorded. This is not always practical, however, and Marion and
Cohen [24, 25] recommend moving the slit into a compromise position
corresponding to the center of the peak and leaving it there as 28 is changed. If the
position of the slit is changed with 28, on the other hand, the length of the
diffraction cone seen by the receiving slit changes, and the scattering factor IF21 is
proportional to
IF21(XP2oRp,
(6.76)
where R~ is the distance from the specimen to the receiving slit [Eq. (6.75)] and
P~8 is the intensity measured at any point 28 along the line profile. The correct
intensity at 28 along the profile must be obtained by multiplying the observed
intensity at each point by R~.
Parafocusing requires the accurate positioning of the receiving slit during the
measurement. This is not always practical and usually the 'stationary slit' method
is used. In thi~ method the slit and the detector are left on the goniometer circle at
all times, deliberately not fulfilling the focusing condition. This procedure results
in lower diffracted intensity received at the detector. However, the complication of
moving the slit or the PSD exactly along a given radius is eliminated. Any
deviation from the radius will cause an apparent shift in 28 since the angular
relationship between the direct beam and the receiving slit or PSD changes during
the measurement. Even if parafocusing geometry is correctly used, however, xrays focus to an area, not to a point, due to the effect of sample shape and there is
still some residual error in the peak location. This effect is treated below.
6.7.2 Effect of Horizontal Divergence on Focusing
For finite x-ray beam dimensions, true focusing requires the conformation of the
specimen surface to the focusing circle at all tp-tilts. This requires a concave
specimen whose radius of curvature is continuously variable during the stress
measurement. Such specimens, however, are rarely encountered in practice. Nonconforming specimens produce a focusing aberration such that the focus is no
longer a point (such as A or B in Fig. 6.17, 6.18) but has a finite area. This
departure from the ideal focusing condition is shown in Fig. 6.19, 6.20 for a flat
specimen and a convex specimen respectively.
Marion and Cohen [24, 25] have given a simple equation relating the error in
peak location to beam divergence. Consider Fig. 6.19; using the law of sines for the
triangle XOD one obtains
o D = RGcs~n ( (X/2)
(6.77 )
smx
(6.78 )
193
\\
\ J
t---I
ormal to
diffracting plane
Fig. 6.19. Schematic of the effect of the horizontal beam divergence for a flat sample (IX is the
incident beam divergence, q,=90-9, d=90+1p-q,-1X/2 and X=90-1p+q,-1X/2)
?II
~J
/
I'
,I .{
a
l....
- --'r--- - /
Fig. 6.20 a,b. Departure from the ideal focusing condition for a convex specimen. Due to
the non-ideal curvature, the rays from left
(I), right (r) and center (c) do not meet at
one point causing a broad focus spot
1/
(L
co = RGcs~n
( r:t./2 )
sm.1
BO __ CO'sin (.1 + 29)
sin ( r:t./2)
(6.79)
RGc'sin (.1 + 29) /sin.1.
194
-D2
c:i
CD
Q)
<I
t.o
_DID
130
140
28
150
160
Fig. 6.21. Variation of the peak-shift as a function of 29 due to a horizontal beam divergence of 1
(a.=1)
( 6.80)
where AB = BO - AO and can be evaluated from Eq. (6.78), (6.79). The "peak
shift" due to this aberration in degrees 29 is given by
A29=~180
,
R'
p
(6.81 )
195
_.10 0
c
III
Q)
C\J
<J
IX)
-.05
t= 15~
130
140
28
150
160
Fig. 6.22. Variation of the peakshift as a function of 29 due to a horizontal beam divergence of 30
(a.=3)
upper limit. Zantopulos and Jatczak [23] have shown that the deviation of the
centroid [Eq. (6.4)] of the diffracted beam from the true value approaches a
limit of (1/3) of 0 (L\29) given by Eq. (6.82) (the centroid in this case was
determined by a computer iteration method in which the divergence angle was
divided into 1000 parts). James [14] suggests the use of 1/2 of the value of
o(L\29). As long as the divergence angle is small, however, (1 0 for example), the
error due to this effect is small over the tp-ranges usually employed (Fig. 6.21 ).
196
Table 6.3. Values to the constants 01 and 02 for textured specimens (From Ref. [24])
No soller slits
One soller slit
Two soller slits
Strong peak
01 02
01 02
2
1
0
1
0
0
2
2
2
constants of textured materials where analysis of oscillatory "d" vs. sin 2 '1' plots is
required.
In the discussion above, the effect of deviations from the focusing geometry
were reviewed. A quantitative comparison of the error introduced in the stress
determined from peak position data measured by the parafocusing and the
'stationary slit' methods has been given by James and Cohen [14, 26]. Using an
automated receiving slit bracket under computer control, they performed fifteen
replicate measurements on a steel sample (211 peak, Cr radiation) with and
without slit movement. They report an average stress value of -164 MPa for the
parafocusing geometry and -170 MPa for the stationary slit geometry. The
observed error of one standard deviation from the mean value is 3.6 MPa for the.
stationary slit geometry and 7.2 MPa for the parafocusing geometry. Even
though the repositioning of the slit during focusing was very accurate, it caused an
error of 4 MPa. Based on these considerations, the use of the stationary slit
method with appropriate slits limiting the horizontal divergence to less than 2 is
recommended.
b) Alignment Errors
As the name implies, these errors originate from instrumental misalignment. Three
important cases of misalignment contribute to errors in residual stress measurement: sample displacement from the center of the diffractometer, effect of'l'-axis
not corresponding to the 29 axis, and missetting of the true zero of the 'I'-rotation.
These effects are discussed below.
there is a relative peak shift between '1'=0 and '1'='1'. This is shown in Fig. 6.23
for the case of the O-goniometer. The shift in degrees, 29, is given by
() (t129) SD = t129..,= 0 - t129..,=..,
RGC
. .sin 9
] .
Rpsm (9 + '1')
(6.84 )
197
DISPLACED
SAMPLE
CORRECT
- - - - SAMPLE
POSITION
PEAK SHIFT
FROM 4.1= 0
TO 4.1 =\.1.1
VI
Q)
C\J
<I
130
140
28
150
160
Fig. 6.24. The variation of the peak shift due to sample displacement of 0.0254 mm back from its
proper position over the center of the diffractometer (Ax = - 0.025 mm)
Here.1X is the sample displacement, R~ is given by equation (6.75) and Rocis the
goniometer radius. The peak shift due to this effect is shown as a function ofe and
\jJ in Fig. 6.24 for .1X= -0.025 mm.
For cubic materials a simple method for checking sample displacements on a
diffractometer has been discussed b, Cohen [29]. Consider Fig. 6.25 (\jJ = 0):
.1X/sin e
sin .12e
'" Roc _
Roc
Roc
sin ( 2e - .12e) - sin 2e 2 sin e cos e
( 6.85a)
198
+------~**~=-~\
sin 8
(6.85b)
(6.86 )
ahkl-a O
AX
= - - 'cot ecos 9 .
RGC
ao
(6.87 )
Here ahkl is the lattice parameter calculated from the peak maximum and a is the
extrapolated true lattice parameter.
Equation (6.87) can be used in measuring AX via x-ray diffraction. The lattice
parameter ahkl is determined for various reflections (at 'I' = 0) and plotted vs.
cos 2 e/sin 9. The slope of this line is equal to - AX/RGc, For a o one can take the
intercept of the plot. In this type of analysis a positive slope indicates negative
displacement, that is the sample is displaced to a position behind the center of the
diffractometer, -away from the x-ray source and the detector.
If the material is susceptible to stacking faults, however, this method may yield
an erroneous displacement. The lattice parameter in such cases is also affected by
other factors, as discussed in Sect. 5.7. When the specimen displacement is finite
Eq. (5.27) becomes
+ (_
(6.88 )
where the terms are defined in Sect. 5.7. In such a case A29hkl must be measured for
at least five reflections and the unknown parameters, including AX, must be
determined from a least-squares analysis of the measured values as discussed in
Sect. 5.7.
1 This term is for stationary slit geometry. If another method is used, the appropriate equation
for sample displacement must be substituted here.
199
ABsintp
sin ( 180-tp-9)
(6.89)
AC~~29
( 6.90)
(6.91 )
( 6.92)
'l'A
(6.93 )
The effect of this displacement is shown in Fig. 6.27 for various 29,
tp (AX' = - 0.025 mm).
--+-------~~-7~.-~--+------
SAMPLE
0/=0
200
.02
<l
Q)
<J
fA)
.01
130
140
28
150
160
Fig. 6.27. Variation of the relative peak-shift due to the presence of a 'I'-axis displacement of
-0.025 mm
~ (29)1jl =
(6.94 )
GC
The peak shift between 'P = 0 and 'P = 'P is then given by
3(~29) = R2
GC
.COS9[(_1cos 'P
( 6.95)
201
_specimen
.-'
." aXIs
..
..
( 6.96)
Mm.
This effect is due to the deviation of the specimen surface from the focusing circle.
For flat specimens, the error in 29 is given by
1
sin 29
a(29)= 12sin2 (9+'I')
where
(1.
( 6.97)
.(1.2,
Circle
/
RGC
202
In the case of cylindrical geometry (Fig. 6.29), the displacement of the x-ray
peak due to this effect is
_ x( 3) . e. {RGC
1-4 sin 2e sin2'P}
- 3R2 cos
R cos 'P +
. e
GC
1
sm
+
A 2 -A 1
.
3
3
R
cos e sm'P, x(3) = (AI +A 2 )/(A 1+A 2 ),
GC
(6.98 )
where the terms are defined in Fig. 6.29. The peak shift error between two 'P-tilts
'P = 0, 'P = 'P is given by
.O(A2e)=cose.z 2 .(_1__ 1),
3RGC Rl
cos 'P
(6.99)
From Eq. (6.101) it is seen that an error A from the true 'P-position will cause
splitting proportional to K",sin2A for positive and negative 'P. The shape of the
X-ray
tube
detector
region
I
I
I
N8 I
I
I
203
~I
I
I
I
I
I
I
~----:::::=r-::::;:::::::----I TA
90-t t
split d vs. sin 2 \jJ pf-ot will be the same as the psi-splitting caused by 0" 13,0"23 (with
.::\ = 0) since in both cases the effect is caused by the argument sin2\jJ. However,
while for true \jJ-splitting the dcjJljJ+ ,dcjJljJ_ will be interchanged if <I> is rotated 180, no
such change will occur in the case of the split caused by .::\ since
(6.102 )
If the specimen surface exhibits curvature, the true \jJ-position will vary along the
surface. In those cases where the dimensions of the beam are large compared to the
radius of curvature, the measured d value will be an average over a range of \jJtilts. If the odometer of the diffractometer is showing \jJ = \jJ A for the center of the
specimen, the true \jJ at any point within the irradiated area will be
(6.103 )
where 90-\jJI is the angle between the tangent to the surface at that point and the
normal to the diffracting planes at that point in the irradiated area (Fig. (6.31 ). It
may be seen from Fig. 6.31 that the maximum deviation from the mean value will
depend on the specimen radius and width of the i~radiated area.
Various estimates of the error this effect causes have been given. For biaxial
stress states the errol is less than 5 % [27] for situations where the ratio of the halfwidth of the irradiated area to the specimen diameter is less than 0.13. No work on
triaxial analysis is yet available. The best method of dealing with this situation is to
use a narrow beam such that there is little curvature within the irradiated region.
The loss of intensity due to the narrow incident beam may be compensated by
increasing the height of the beam.
6.7.8 Alignment Procedures
In Table 6.4 the effect of some of the errors discussed above are shown. It can be
seen that the most important sources of error are the displacements of the sample
and the \jJ-axis from the center of the diffractometer. The effects of the sample
displacement may be minimized by using the analysis method discussed above to
204
Table 6.4. Typical instrumental errors in peak location for 2!bd56 (approximately the 211
CdC" peak from iron) (From Ref. 14)
Cause
Horizontal beam
divergence (IX = 0.5)
(Taking 1/2 (o(~26hD) see text
Vertical beam divergence
(Assuming strong texture
using divergent Soller slit
no receiving Soller slit)
Sample displacement
~= 0.025 mm
II'-axis displacement
~x' = 0.025 mm
Maximum total errors+
a) in - 26 direction
b) in + 26 direction
Maximum error in
stress for steel'
-0.0006 26
-0.0025 26
- 0.002 26 or
+0.002 26
-0.002 26 or
+0.002 26
-0.0034 26 or
+0.0034 26
- 0.002 26 or
+0.002 26
-0.0088 26 or
+0.0088 26
-0.0068 26 or
+0.0068 26
-0.008 26
+0.0068 26
-4.74 MPa ( -690 psi)
or
+4.0 MPa ( -585 psi)
-0.0201 26
+0.0149 26
-7.0 MPa ( -1150 psi)
or
+5.9 MPa (+860 psi)
+ Note: Maximum error is either one of these but not the total range.
Calculated for steel from 0"<1> = K.v (26J. - 26'l') where K45 = 593 MPa;o26 and
396 MPa;o26.
K60
measure the offset and displacing the specimen to the correct position. Alternately,
it is also possible to evaluate the error in stresses such a displacement causes and
correct the measured stress values. One method of stress measurement that
minimizes the effect of specimen displacement is the parallel beam method
(Fig. 6.32) where the 20 position is determined uniquely by the angular
relationship between the parallel slits (these are usually soller slits placed with the
baffles perpendicular to the goniometer plane). In Fig. 6.33 the effect of specimen
displacement is shown for parafocusing, stationary slit and a parallel beam. The
~etector
X-ray tube
5011""'\'
\
,\ ,,
,, \ \ \ \ \
\
-------
'
\ , \' ,
~~
\
Specimen position
---- ------
Fig. 6.32. Schematic of parallel beam geometry. The diffraction angle 26 is uniquely defined
by the angular relationship between the two
sets of soller slits and is independent of sample
position (dashed lines or the solid line)
205
350.-.----.-----,----.-----,-----,----,-----.-----r~
300
250
o
~ 200
il
.:: 150
V1
7-
___Parallel beam
-_-_~_--_--_6--
Stationary slit
50/
100
O~~--~--
-2.0
-1.5
__- L_ _ _ _
-1.0
-0.5
0.5
1.0
1.5
2.0
Displacement (mm)
Fig. 6.33. The dependence of stress upon three geometric focusing conditions on a 1405 steel
sample. The solid lines represent the error as calculated from Eq. (6.84). The dashed line
represents the slope of the actual data with a parallel beam. From James [14]
error is maximum for parafocusing and negligible for parallel beam geometry. The
barnes, however, restrict the amount of diffracted intensity received by the
detector and for a comparable statistical error counting times up to three times
longer may be necessary.
An alignment method that will indicate the presence of all aberrations except the
tp-missetting error [Eq. (6.101)], or variation oftp within the irradiation surface, is
the "annealed powder" method. In this case a very thin film of annealed powder is
brushed on the surface of the specimen irradiated by x-rays, and the stress in the
powder is measured by the residual stress determination procedure that will be
used on the actual specimen. The position of the specimen is then adjusted until the
stresses measured f:t;"om the powder are negligible within the statistical error. The
error from the powder can then be used as an estimate of the error in the
stress determined from the specimen after the powder is brushed away.
However, since all errors are strongly dependent on 29, the powder peak from
which the errors are measured must be close in 29 to the position of the specimen
peak. It must be noted that this method can not detect the presence of "tpmissetting error" since the stress term Kq, in Eq. 6.101 and thus the term Kq,sin2tp
which causes the split is zero, independent of!l. and an unsplit plot will be obtained
even if !l. is finite.
206
stresses which can also act in the direction of the surface normal. It was also shown
that if steep stress gradients exist within the maximum penetration depth 't'P' "d"
vs. sin 2 \jJ would exhibit curvature. One way of minimizing the effects of gradients
is to use high 'l'-points in the analysis as discussed in Sect. 5.12. This method is valid
both for micro- and macroresidual stress gradients. An electropolishing method
has also been suggested to compensate for the variation of stress with depth [7].
This method, which is valid only for macros tress gradients, is discussed below.
For an x-ray beam penetrating a distance 't into the material, the average 29
measured will be a function of the variation of the true 29 with the penetration
depth:
J 29(x)dI
x=o
9
(6.104)
2 obsv. = - - 0 0 - - - dI = Ke -lI x /'dx
<X)
x=o
dI
J29(x)dI
JdI
(6.105 )
:/1 .d(2:;bs.) .
(6.107 )
Thus, if one obtains the variation of the observed 29 angle as a function of depth
(by successive measurement and electropolishing) it is possible, theoretically, to
determine the true 29 as a function of depth. Of course, observed 29 data over all
the \jJ-tilts examined must be measured at every etching level to obtain the
necessary corrected data for stress analysis. The problem with this method is the
assumption that electropolishing does not alter the stress distribution. Some
relaxation will invariably occur. If a very thin layer is removed this relaxation may
be negligible. However, if successive electropolishing oflayers results in substantial material removal, relaxation effects must be taken into account.
207
relaxation effects. In the limit, if one part of the body that is constraining the other
part is totally removed, the stress will decay to zero in both parts. Since with x-rays
one measures the stress after a volume is removed, the measured stress must be
corrected for the effects of such relaxation. The initial stresses in the body are
related to the relaxed stress state through the equations of compatibility and the
equations of equilibrium, and for a given specimen/stress distribution combination
it is possible to use these equations to determine corrections to the measured
values. Such treatment has been formalized in closed form for various geometrical
shapes [7,30,31]. These solutions involve evaluation of definite integrals of the
measured residual stress distribution. For example, in the case of a flat plate,
which contains a biaxial macroresidual stress tensor, the components of which
vary only as a function of depth, the correction is given by
er (z ) = er
x
Xobsv
(z)
1
(z)
+ 2 Her
S XobsvZ
ZI
Her
(z)
dz - 6z S Xobsv
dz
1
ZI
Z2
'
(6.108 )
where H is the original thickness of the plate, ZI is the distance from the lower
surface to the uncovered depth of interest, erx (ZI) is the true stress and erXobsv' is the
measured stress value. For complicated shapes and/or stress distributions, the
correction becomes more involved.
A series correction for layer removal is possible where the integrands in
Eq. (6.108) are expanded in the form of Taylor series referred to the surface
values and the integration is performed term by term:
1 )
H-Z
erx(d
z -erXmeas ( z d -- -4erXmeas (H) . ( H-
+ [er
Xmeas
H -_
z 1 ) 2 + ...
(H) +2H oerXmeas ( H ) ]. ( _
oz
H
(6.109 )
For small etching depths and shallow gradients, the first terms of the series may be
used:
Az
Aer=erx(zd -erXmea.(zd = -4erxmeas (H)'If'
(6.110)
This equation may be used to determine the polishing thickness that will yield a
small correction. For example, for Aer to be less than 5 %:
AZI
= 4'0.05 H.
(6.111)
208
6.10 Summary
Residual stress values determined by diffraction methods have two types of error
associated with them:
a) statistical error, which arises due to the random arrival of x-ray photons at the
detector, causing an uncertainty in the absolute intensity at any 29 position;
b) instrumental error, which arises due to specimen alignment, effect of beam
optics, etc.
The variance in the peak position is the sum of the variance due to these effects
[26]:
0- 2 (
stress) = 0- 2 ( stat.)
+ 0-2 ( instr.) .
(6.112)
The statistical variance in peak position can be obtained from the variance in the
intensities over the pertinent 29 range. This is accomplished by propagating the
error through 'the equations used in peak location determination. The instrumental errors are frequently determined from geometrical considerations and are
dependent on the particular experimental configuration and beam optics.
Various strategies are available for peak determination. The most widely used
method is the fitting of a parabola to the top 15 % of the peak and then
determining the apex of this parabola. Various studies have shown that this
procedure can be used for the majority of peak shapes encountered in practice.
Furthermore, the calculation of the statistical error for this method is relatively
straightforward. These formulae have also been tested by comparing the standard
deviation calculated from one measurement with the standard deviation obtained
from multiple measurements, and excellent agreement has been reported [12, 14,
26].
If the equations for error determination are known for a given measurement
configuration, the stress measurement may be automated such that an experiment
can be carried out to an operator-specified precision. This may be accomplished by
writing a code that first requests the various experimental parameters from the
opera,tor, calculates the 0- 2 (instr.) from these parameters using the equations
given in this chapter, determines the maximum statistical error permissible for a
specified total error from Eq. (6.111) and then calculates the total accumulated
counts or time required for such an error. Intensity vs. 29 data is then obtained to
this specification. If the diffracted beam intensity is known (this may be obtained
from a fast preliminary scan of the peaks involved) , such a procedure can also be
used to estimate the time required for the stress measurement.
6.10 Summary
209
Problems
6.1. Given the following five points on a diffraction profIle.
Angle (29)
Corrected CPS.
Time
159.845
160.305
160.765
161.225
161.685
502.5
524.5
526.7
513.4
499.2
39.9
38.2
37.9
38.9
39.9
(i) Calculate the peak position by fitting a parabola to these points. (ii)
Calculate the statistical error. (iii) Calculate the "d" value (Co radiation is
used). (iv) Calculate the statistical error in "d".
6.2. Given the following "d" vs. sin 2 tp data.
sin 2 tp
d,p(A)
Statistical
error (d,p)'10- 4 (A)
0
0.1
0.2
0.3
0.4
0.5
0,90795
0.90735
0.90505
0.90669
0.90698
0.90607
0.569
0.432
0.568
0.390
0.367
0.398
(i) Calculate
0"<1>'
0"<1>'
References
1
2
3
4
5
6
7
8
9
J.B. Cohen, H.Dolle, M.R. James, NBS Special Publication 567, 453 (1980)
A.J.C. Wilson, "Mathematical Theory of X-ray Diffractometry", Philips Technical Library
(1963)
W.E. Baucum and A.M. Ammons, Adv. in X-ray Anal., 17, 371 (1973)
T.J. Devine, Comparison of Full-Profile Peak Finding Methods For Use In X-ray Residual
Stress Analyses, M.S. Thesis, Northwestern University (1985)
J. Mignot and D. Rondot, J. Appl. Cryst., 9, 460 (1976)
M.M. Hall, V.G. Veeraaghavan, H. Rubin, and P.G. Winchell,J. Appl. Cryst., 10, 66( 1977)
Soc. Automotive Eng., Residual Stress Measurement by X-ray Diffraction, SAE J784a, 2nd
Ed. (1971)
H.M. Rietveld, J. Appl. Cryst., 2, 65 (1969)
R.E. Ogilvie, Stress Measurement with the X-ray Spectrometer, M.S. Thesis, MIT (1952)
210
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
J. Thomsen and F.Y. Yap, J. of Res. of Nat. Bureau of Standards, 72a, 187 (1968)
D.P. Koistinen and R.E. Marburger, Trans. ASM, 51, 537 (1959)
M.R. James and J.B. Cohen; Adv. in X-Ray Analysis, 20, 291 (1977)
R. Marion and J.B. Cohen, Adv. in X-ray Anal., 18,466 (1975)
M.R. James, An Examination of Experimental Techniques in X-ray Residual Stress Analysis,
Ph. D. Thesis, Northwestern University (1977)
M.A. Korhonen and V.K. Lindross, Scandinavian Journal of Metall., 2, 100 (1973)
M. Knuuttila, Computer Controlled Residual Stress Analysis and its Application to
Carburized Steel, Ph. D. Thesis, Linkoping Univ. of Tech., Linkoping, Sweden (1982)
H.K. TonshofT, E. Brinkmeister, and H.H. NOlke, Ztsrft. f. Metalkde, 72,349 (1981)
H.K. TonshofTand E. Brinkmeister, Annals ofCIRP, 29,519 (1980)
A.J.C. Wilson, Brit. J. Appl. Phys., 16, 665 (1965)
P.J. Rudnik and J.B. Cohen, Adv. in X-ray Anal., 29, 79 (1986)
K.A. Perry, Experimental Determination of X-ray Elastic Constants, M.S. Thesis, Northwestern University, (1982)
K.A. Perry, I.C. Noyan, P.J. Rudnik, and J.B. Cohen, Adv. in X-ray Anal., 27 (1983)
C. Jatczak and H. Zantopulos, Adv. in X-ray Anal., 14, 360 (1970)
R. Marion, X-ray Stress Analysis of Plastically Deformed Metals, Ph. D. Thesis,
Northwestern University (1973)
R. Marion, ibid. Appendix B
M.R. James and J.B. Cohen, O.N.R. Technical Report, No. 14, Northwestern University,
Mat. Sci. & Eng. Dept., Evanston, 11. February, 1977
Centre Tech. des Indus. Mech., Les Mem. Tech. du Cetim, 33 (1978)
E.R. Pike, J. Sci. Instr., 34 355 (1957)
J.B. Cohen, "Report on Tungsten Lattice Parameter Round Robin", X-ray Subcomm. of
SAE Iron and Steel Tech. Comm., Division 4, (1964)
M.G. Moore and W.P. Evans, SAE Trans., 66,340 (1958)
D.P. Koistinen, R.E. Marburger, M. Semchyshen, and W.P. Evans, SAE Information Rep.
TR -182, A.L. Christianson ed., SAE, New York (1960)
7.1 Introduction
In this chapter, we consider the various ways to make measurements of residual
stresses on real parts, either in an ordinary x-ray laboratory (Sect. 7.2) to which
such samples may be brought occasionally, in a factory where frequent inspection
is required, or in the field, for example at large construction sites, on oil-rigs or
pipelines or power stations, or for parts which are too large for a commercial
diffractometer. Tliere are several units now available for such situations, but this
equipment is new and can be expected to change frequently. Therefore we prefer
here to provide a list of ideal requirements for the software and hardware
(Sect. 7.3), against which the reader can examine what is available commercially,
emphasizing his own priorities in these lists. (Also, it is always advisable to contact
several users of such equipment, as well as the supplier.) We will then briefly
describe the available equipment at this writing (Sect. 7.4 ), and conclude with a
detailed examination of several examples of the use of stress measurements in such
situations (Sect. 7.5).
212
1) There should be a high level of safety, such as scatter shields. Also, the shutter
should remain closed unless the device is in contact with a part, and there
should be warning lights. In-field equipment may be operated by persons
with minimal skills in diffraction!
2) Some form of position-sensitive detector should be incorporated to minimize
measurement times.
3) The equipment should be rugged and transportable.
4) Protection from dust and moisture may be necessary.
5) To reduce weight and bulk, use should be made of miniature components,
such as the x-ray tube and generator.
6) There should be flexibility so that the device can be employed in a variety of
situations.
7) It should 'be possible to choose parallel or divergent beam geometries.
8) A microprocessor control and data processor is essential.
9) There should be a choice of (\jl or Q) rotations.
10) The <l> rotation should be possible, so that the entire three-dimensional tensor
can be measured if necessary.
11) Is there a means for oscillation to reduce the effects of coarse grain size? (This
is especially important with a PSD, as with such a detector seeing the whole
peak at one time, texture can distort the peak shape.)
12) It should be simple and rapid to change the x-ray tube.
13) It should be simple and rapid to choose different Bragg peaks.
14) It should be possible to use it at large distances from the electronics (8 -10m
or more).
15) Light weight is important for ease in handling and positioning.
16) Completely automated operation should be available (including tilts,
shutters et~.)
17) Suitable procedures and attachments are needed to measure the x-ray elastic
constants.
18) A graphics display (and final hard copy) of a peak during measurements is
essential, as well as "d" vs. sin 2 \jl.
19) Is maintenance available? Can parts be replaced in a matter of days?
20) Are there adequate yet rapid means of locating the unit relative to a part.
B. Software
1) An easily readable menu of all options and required input should be available
on the screen.
2) "Help" instructions should be provided.
3) Are appropriate corrections (f2, L.P. etc.) made to the data (including
detector nonlinearity, background)? For this non-linearity, how long does it
take to gather the data, and how often must it be repeated.
4) The output should be well organized and clear.
5)
6)
7)
8)
9)
10)
11)
12)
213
This class of field devices offers sufficient flexibility to permit at least some choice
of techniques.
1) Strainflex (RigakujUSA Inc., Danvers, MA. 01923)
This instrument can be described as essentially a full diffractometer with a
standard x-ray tube (and its associated large transformer) mounted on a
mobile hoist. An ordinary detector is employed. Calculations and operations
are "hard-wired" so that changes are not feasible. A similar instrument is
available from the Siemens Corp. and Shimadzu Co.
2) PARS (Portable Analyzer for Residual Stresses, Technology for Energy
Corp., Knoxville, TN 27922).
A position-sensitive gas filled proportional counter is employed, as well as a
miniature x-ray tube and a miniature high-voltage generator. It incorporates
micro-processor control and calculation. [This device was invented by M.
James and one of the authors (J.B. Cohen) J.
214
attendant delays for development and reading, these commercial products all
involve detectors.
1) F ASTRESS (American Analytical Co., Grafton, OH 44044 ).
Two standard x-ray tubes with different incident directions and two conventional detectors are employed. Peak position is located automatically when the
intensity reading is the same in both halves of each detector.
2) EMSAM, Paris, France
Two gas fIlled position sensitive detectors straddle both sides of a standard xray tube to record both sides of a diffraction cone in the back reflection region.
Control and data processing is through a microprocessor.
3) HITECH Canada, Ltd., Ottawa, Ontario, Canada KZC3N6
This is similar to item # 2.
4) Dr. C. Ruud, Materials Research Laboratory, The Pennsylvania State
UniversitY'eUniversity, Part, PA 16802
This is similar to both (2) and (3), but utilizes a miniature x-ray tube and
special miniature position sensitive detectors built with channel plate. The
instrument is sufficiently compact to be placed inside a large pipe. The detectors
produce analog signals rather than the counting pulses produced by gas-filled
detectors, so that calculating the statistical error is not straight-forward.
We turn now to several examples of in field measurements. Our aim in this
section is three-fold: 1) to demonstrate the actual use of the techniques, 2) to
show how such measurements can be employed to resolve important problems,
and 3) to illustrate typical output data.
215
Fig. 7.1 a,b. Photographs of the portable x-ray unit built at Caterpillar Tractor Co.
in the peak 2,3,5 or9 at a time) is available in the software to help smooth the data.
This data is screened (using 80 pet. of peak maximum) and a least-squares fit
to a parabola is employed to determine peak position. Statistical and geometric
errors are included in the calculations. Correction for doublet overlap is also
included in the two-tilt technique.
In what follows, the two-psi tilt technique (0 and 45 degrees) was used unless
otherwise noted. Counting times of 40 - 60 seconds were usually employed and
data on peaks were collected in the multi-channel analyzer at gain settings of
(usually) 512. The averaging option of 3 was most often used. The detector was
covered with 0.004 mm of V foil and Cr radiation was employed. Channels were
calibrated with a Cr-Fe powder mix using literature values for the peaks positions.
216
Order of
Hardening (H)
Welding (W)
Loc,
deg
H-W
-30
Measured
+30
W-H
-30
+30
H-W
-30
+30
W-H
+30
+30
W-H
-30
+30
-302.0
- 358.5
-271.7
- 351.6
-307.5
-3123
175.1
317.8
236.5
112.4
(127.6)"
( 38.6)
( 78.6)
( 38.6)
( ~6.2)
( 66.2)
( 50.3)
(136.5)
( 60.0)
( 66.2)
- 6.9 ( 57.9)
- 43.4 ( 42.1)
- 557.8 ( 65.5)
-644.0 ( 57.9)
816.3 ( 55.2)
538.5 ( 40.0)
160.6 ( 64.8)
201.3 ( 45.5)
Mean
-310.7 ( 44.1)"
- 323.8 ( 24.2)
246.5 (100.9)
174.4 ( 87.8)
- 25.2 ( 25.8)
- 600.9 ( 60.9)
677.4 (196.5)
181.0 ( 28.8)
- 48.3 ( 40.7)
- 28.3 ( 42.7)
Statistical and geometric counting error (geometric error due to beam divergence, IV axis
misplacement, and sample displacement) .
.. Std. Dev. of the Mean.
217
of a piece of 5 mm weld rod near the right end to simulate a "worst case" situation.
The data shows an average change ofl147.21MPa after bolting. This could result in
residual tensile stress on the inside face as shown in the table. To eliminate this
possibility, the ()Ut-of-flatness tolerance was reduced and delayed cracking was
subsequently minimized.
Table 7.2. Residual stresses in a bolted assembly of plates
Plate
Assembly No.
Outside face
middle
2
3**
Inside face
left
middle
right
Outside face
left
middle
right
Inside face
left
middle
right
Outside f~ce
left
middle
right"
After bolting *
Change due
to bolting
- 265.5 (76.5)
-357.8 (77.2)
- 92.4
-115.1 (24.1)
102.7 (55.2)
- 35.9 (51.0)
151.1
- - 64.9
34.5
179.3 (64.1 )
- 296.4 (40.0)
-168.2 (44.8)
- 86.9 (41.4)
-128.9 (50.3)
- 238.6 (45.4)
22.8 (71.0)
-319.2 (70.3)
- 206.2 (70.2)
- 5.6
-458.5
70.3
-263.4 (47.6)
-432.3 (77.2)
-463.3 (62.1)
- 280.6 (64.1)
- 293.0 (58.6)
-739.8 (78.6)
Ave. change
-266.2
-167.6
- 70.4
- 17.2
139.3
-276.5
1147.11 (97.6)
218
(7.2)
r__ *_
600
RC~4~
/HARDNESS__
--"'--*~ ~
400
219
35
___ ~~:.
200
~ O/~/ )(/~
~
c91j
-200
~ -400
<
:::)
x
x/x
o - LONGITUDINAL
.=RADIAL
~ -600
-800~011
0
_1000X~~
-1200
x - TANGENTIAL
-1400~1__~~'~~~'~~~'__~~'__~~
' ~~~'~~!
0.0
2 .0
4.0
6.0
8.0
10.0
12.0
14.0
DEPTH, mm
Long forces
( x W"N)
Tang forces
( x 103 N)
Depth
Long forces
( x 10 3 N)
0.0508
0.1270
0.2692
0.5079
1.2699
1.4071
1.5240
2.7939
2.9971
4.9530
- 5.37
- 9.10
-16.09
-25.12,
-59.73
- 8,95
- 8.03
-64.33
- 7,03
-27.20
- 1.40
- 2.58
- 4.66
- 7.04
-17.13
- 2.45
- 2.21
-20.47
- 2.75
-17.76
5.0799
7.5183
7.6199
10.0329
12.5729
15.2399
17.7799
20.3199
0.29
30.28
2.08
54.50
58.45
45.81
26.31
9.70
Totals
-3,58
Tang forces
(xl0 3 N)
0.33
2.94
0.38
11.25
14.55
15.93
15.61
15.61
-
2.52
The force balance is an interesting exercise but can only be done if measurements
are made near the bar center, and only if microstresses are negligible. It is an
indication of reliability in the test, that as stressed layers are re~oved the bar
relaxes and obeys conditions of equilibrium (as it certainly must) , and that most
of the stresses are macrostresses.
220
The test crank was a steel forging ofSAE 1034 steel. It was normalized, machined,
and heat treated to give a hardness of Rc 48 minimum. The journals are finished
ground to size and polished to improve surface finish. The problem was to
quantify the effect of polishing on residual stresses in the journal bearing areas.
Measurements were made at mid-length of both pin and main journals as
shown in Fig. 7.5. The outboard side of the journal was used which was set
adjacent to the goniometer alignment plate. In this way, measurements could be
made non-destructively, without sectioning the journals. Results are shown in
Table 7.4, comparing as-ground to ground and polished journals. Significantly
higher compression is seen in the polished journals. Scatter is also somewhat less.
Table 7.4. Residual stresses in crankshaft journals comparing as-ground and ground and
polished journals
Residual stress
Measured
As-ground
Pin
Pin
Pin
Pin
- 504.0
-600.5
- 562.6
- 277.2
-431.6
- 251.0
(46.9)*
(40.7)
(42.1)
(53.8)
(60.7)
(49.9)
No.2 Pin
No.4 Pin
-934.9
- 955.6
-920.5
- 862.5
- 662.6
- 753.6
-819.1
(49.0)
(62.1)
(59.3)
(43.4)
(45.5)
(73.8)
(80.7)
No.2
No.4
No.6
No.5
No.6 Pin
No.1 Main
No.5 Main
.... Same as meaning in Table 7.1
MPa(ksi)
Mean
-555.7 (48.6)"
-319.9 (97.6)
-918.4 (39.9)
-745.1 (78.6)
221
Engine PLT
Crankshaft
T
HAR
DEP
DIR
BEAM
400F
RC 52-58
SURF
AXIAL
1 DEG BEAM
Location
Stress, MPa
Standard Deviation,
MPa
FILLET, FRONT
FILLET, FRONT
FILLET, REAR
FILLET, REAR
MID-LGTH
FILLET, REAR
FILLET, FRONT
FILLET, FRONT
FILLET, REAR
MID-LGTH
FILLET, FRONT
MID-LGTH
FILLET, FRONT
FILLET, REAR
MID-LGTH
FILLET, FRONT
MID-LGTH
FILLET, FRONT
FILLET, REAR
MID-LGTH
MID-LGTH
FILLET, FRONT
MID-LGTH
FILLET, FRONT
FILLET, REAR
MID-LGTH
FILLET, FRONT
FILLET, REAR
MID-LGTH
FILLET, REAR
MID-LGTH
FILLET, FRONT
MID-LGTH
-275.8
-341.3
-377.8
-341.3
-548.8
-295.1
-299.9
-255.1
-233.0
-320.6
-302.7
-722.6
-396.4
-395.8
-490.2
-471.6
-571.6
-455.1
-330.3
-509.5
-604.0
-365.4
-334.4
-313.7
-295.1
-481.9
-454.4
-351.6
-485.4
-268.9
-348.2
-408.9
-364.7
36.5
46.9
37.9
63.4
46.9
42.1
44.8
41.4
37.2
44.8
38.6
45.5
50.3
49.0
57.2
38.6
60.0
31.7
35.2
43.4
52.4
42.1
53.8
35.2
37.2
55.2
34.5
35.2
48.3
38.6
42.1
42.1
40.0
LNO
Date
REQ
COM
TC
MAT
HT
30224
6-3-83
R. Shafer
Fillets were peened
Jour were sectioned
SAE 1552
IND HARD
SID
No 1 PIN
No 1 PIN
No 1 PIN
No 1 PIN
No 1 PIN
No 1 PIN
No 2 MAIN
No 2 PIN
No 2 PIN
No 2 PIN
No 3 MAIN
No 3 MAIN
No 3 PIN
No 3 PIN
No 3 PIN
No4 MAIN
No 4 MAIN
No 4 PIN
No 4 PIN
No 4 PIN
No 4 PIN
No 5 MAIN
No 5 MAIN
No 5 PIN
No 5 PIN
No 5 PIN
No 6 PIN
No 6 PIN
No 6 PIN
No 6 MAIN
No 6 MAIN
No 7 MAIN
No 7 MAIN
This is believed typical of polishing (or lapping) and is often used as a residual
stress leveler for this reason.
The data bank display of data for another sized crank shaft, material, and its
heat treatment is shown in Table 7.5. The material was an SAE 1552 steel forging.
Such data represents a base line and is of great value in quality control (QC) and
for comparing processing and manufacturing trends.
222
""
-200
Q.
:Iii
u)
(/)
w
a:
!n -300
..oJ
""
::::I
Q
en
~ -400
-500
0.0
10.0
60.0
70.0
223
hub. The multi-psi tilt method was used with tilts of 15,30 and 45 degrees; the
zero-degree position was also used in a few cases. Counting times of 120 seconds
were used for each peak. The beam was 2 rom in diameter.
The results at various points along the flank are shown in Fig. 7.7. A significant
decrease in residual stress is shown in locations 5 -13 mm from the suspect edge.
Sectioning verified the findings as shown in Fig. 7.8. After the fact, measurements
closer to the tooth tip should have enhanced the effect, and a smaller x-ray beam
might have helped as well.
Example 6: Measurements on a Shot-Peened Reference
A known reference is of great value to any laboratory making routine residual
stress measurements. Such a sample can be run from time to time to examine
equipment stability, electronics, detector, and calibration. It is also useful in
evaluating particular running conditions.
We use a shot-peened reference for this purpose. It is a plate ofSAE 1045 hot
rolled steel with dimensions 140 x 28 x 6 mm. Hardness before peening was RB
92.5 (Rc 12). One face was shot-peened with 230 shot to an estimated Almen A
intensity of 0.25 - 0.30 mm.
Over the past several years, we have run many hundreds of measurements on
this specimen. A sampling of recent data is shown in Table 7.6. The average of29
measurements of surface residual stresses is - 438.08 (22.46) MPa. The effects of
some important miming conditions are shown in Table 7.7 and show good consistency over the ranges examined.
Example 7: Triaxial Residual Stresses
In situations where the surface has plastically flowed or when high stress gradients
exist close to the surface, triaxial equations and methods must be used, as
224
Table 7.6. Reference data semi-portable x-ray residual stress data file
LAB NO. 30632
MFG. PLTfDATE ID:TECH CENTER/JUNE 1980
SAMPLE IDENT: PEENED REF
MAT SPEC: SAE 1045 STEEL
H.T. SPEC/QUENCH: HOT ROLLED
HARDfTEMPfYlELD: RB 92.5 (RC 12)
TEST LOCfDEPTH: MID-LGTH/SURF
DATE
BEAM GEOMETRY
1-12-84
1-19-84
1-19-84
1-20-84
1-20-84
1-20-84
1-20-84
1-20-84
1-23-84
1-30-84
2-16-84
3-05-84
3-07-84
3-13-84
3-23-84
3-30-84
3-30-84
3-30-84
3-30-84
3-30-84
3-30-84
3-30-84
3-30-84
4-03-84
4-04-84
5-21-84
5-21-84
5-24-84
6-08-84
0.1" DlA
0.1" DIA
0.1" DIA
0.06" DlA
0.06" DlA
0.06" DlA
0.06" DlA
0.06" DlA
0.1" DIA
0.1" DlA
0.1" DlA
0.06" DlA
0.06" DlA
0.1" DlA
0.1" DlA
0.1" DlA
0.1" DlA
0.1" DIA
0.1" DIA
0.1" DlA
0.1" DlA
0.1" DlA
0.1" DlA
0.1" DlA
0.1" DlA
0.1" DIA
0.1" DlA
0.1" DlA
0.06" DlA
Requested
by:WPE
STRESS
DIRECTION:
A-B
COMMENTS:
ROUTINE
CHECK
STRESS
MPa (KSI)
-450.2
-403.3
-446.0
-447.4
-444.7
-408.8
-434.3
-433.6
-443.3
-418.5
-443.3
-457.8
-466.7
-448.1
-431.6
-461.2
-405.4
-467.4
-421.9
-448.8
-462.6
-454.3
-425.4
-448.8
-393.0
-410.9
-474.3
-398.5
-454.3
-438.08
.< - 63.54)
ERROR
MPa (KSI)
33.0
34.4
29.6
41.3
51.7
112.3
30.3
26.8
35.8
33.7
29.6
50.3
37.9
28.2
28.2
31.0
31.0
28.2
33.0
36.5
37.2
29.6
30.3
29.6
128.2
31.0
39.3
30.3
35.1
22.46
(3.26 )
225
Counting time
Beam geometry
Averaging
Gain
Screen
(with 0.06 in. dia. beam)
lOs
20s
40s
80s
160s
-498.4
-375.7
-450.9
-466.0
-413.6
(86.8)
(59.9)
(28.2)
(24.8)
(27.5)
-432.9
-424.0
-419.2
-464.9
-386.1
- 509.5
- 448.8
-418.8
-430.2
(33.0)
(44.8)
(40.6)
(44.8)
(87.5)
(40.6)
(34.4)
(35.8)
(38.6)
Av'g by 1
AV'g by 2
Av'g by 3
Av'g by 5
Av'g by 9
Av'g by 9
Av'g by 5
Av'g by 3
Av'g by 2
AV'g by 1
-460.5
-424.7
- 421.9
-404.7
-431.6
-461.2
-490.9
-457.1
-457.8
-461.9
(49.6)
(33.0)
(36.5)
(35.8)
(26.2)
(24.1)
(39.3)
(28.9)
(33.0)
(41.3)
256
512
1024
2048
-418.5
-404.0
-460.5
-478.4
(36.5)
(38.6)
(83.4)
(92.3)
0.7 in.
0.75
0.8
0.85
0.9
-433.6
- 434.3
-447.4
-444.7
-408.8
(26.8)
(30.3)
(41.3)
(51.7)
(112.3)
-440.9 (47.5)
(-64.0 (6.9
-437.1 (34.6)
( - 63.4 (5.0
-447.2 (25.6)
(-64.9 (3.7
-440.4 (34.9)
(63.9 (5.1
-443.8 (15.2)
( -62.9 (2.2))
226
PO(K,J)
('" tilt)
EP(K,J)
(micro inches/inch)
(+",)
(-"')
( -"')
2
3
4
0
15
30
45
1.172026
1.172053
1.171510
1.170636
EN(K,J)
1.171727
1.171209
1.170140
1.169298
*
*
*
*
1521.6
1545.2
1081.0
334.4
1266.1
823.9
- 89.4
-808.9
1.171786
1.171172
1.170236
1.169330
*
*
*
*
1446.5
1327.0
735.8
136.8
1316.6
792.5
- 7.6
-781.7
1.171803
1.171457
1.170785
1.169606
*
*
*
*
1439.5
1095.1
413.3
-358.1
1331.3
1036.1
461.3
-545.5
0
15
30
45
1.171938
1.171798
1.171106
1.170405
0
15
30
45
do = 1.170245
1.171929
1.171526
1.170729
1.169826
Austenitizing, C
Quenchant,
Temper,oC
Hardness, Rc
1018
1045
52100
870
water
430
29
820
water
430
30
840
water
430
50
Basic data was obtained by the multi-psi tilt method. Lattice parameters were
determined as a function of both positive and negative psi-tilts. Psi-tilts of zero, 15,
30 and 45 degree were used. This is done for three <p tilts (zero, 45, and 90
227
E12=
83.0
E22= -2269.5
E32=
-5.0
E11 = -1 949.3
E21 =
83.0
E31 =
475.6
E13= 475.6
E23= -5.0
E33=1346.6
Stress tensor
(MPa)
SI 12=
15.4
SI 22 = - 688.0
SI32=
0.9
SIll = -628.5
SI 21 =
15.4
SI 31 =
88.3
SI13= 88.3
SI 23= - 0.9
SI 33= -16.6
Principal stresses
(MPa)
SI 1 =642.6
Vl (for SI 1)
SI 2= -636.4
V2 (for SI 2)
X -0.283
Y 0.958
Z 0.038
0.948
0.286
-0.134
SI 3= -4.1
V3 (for SI 3)
-0.140
-0.001
-0.990
Fl =2.343750E-02
F2 = 4. 765625E - 01
F3 = 1.044921 E - 01
D (0) = 1.170245
degrees). Phi is the angle between a reference line in the surface and the plane of
the goniometer. In effect, six plots of d vs. sin 2 ", were obtained.
Running conditions for all peaks were as follows:
2.5 mm dia. beam
30 seconds count time
averaged by 2's
512 gain
228
Table 7.10. Key triaxial results for three steels
Material
Peen direction
(degrees)
Tensor results
Stress tensor, MPa
Normal
Shear
SI11
SI22
SI33
SI 12 SI13 SI23
52100
90
30
-695
-629
-703
-688
-33
-17
24 -2
15 88
4
-1
1045
90
30
-627 -627
-572 -699
9
-12
9 -2
8 56
-3
-5
1018
90
30
-547 -561
-526 -612
-2
-7
-5
15
5
30
4
1
Peen
Principal Stresses
direction
(degrees)
S1
S2
S3
52100
1045
1018
90
-723
-675
-33
30
-693
-636
-4
90
-635
-618
30
-700
-577
- 7
90
-563
-546
-2
30
-614
-525
- 5
V1
V2
V3
-0.65
0.76
-0.006
-0.28
0.96
0.04
0.76
0.65
-0.002
0.95
0.29
-0.13
0.71
0.70
0.004
0.99
0.07
-0.01
0.95
-0.30
-0.006
0.98
0.17
-0.06
0.002
-0.006
-0.99
-0.14
-0.001
-0.99
0.002
0.004
-0.99
-0.1
0.006
-0.99
-0.008
-0.008
-0.99
-0.06
-0.002
-0.99
0.70
0.71
0.001
-0.07
0.99
0.01
0.30
0.95
-0.01
-0.17
0.99
0.007
Sample computer printout of input used for the triaxial calculation is shown
in Table 7.8. Strains were calculated from the lattice parameters computed for
no stress. All terms are matrix arrays. Using methods discussed in Chap. 5, a
strain matrix is computed which also defines the stress tensor, principal stresses,
and directions. An example of the complete triaxial (tensor) results for one
of the steels is shown in Table 7.9 Psi-splitting for that steel is shown in Fig. 7.9.
Key results for the three steels are compared in Table 7.10. As is seen,
229
1. 173
r.J)
~ 1. 172
:. ----0______...
~
!'17' .~ ~O
~~
t;jl . 170
~
~~
~ 1.169
i=
~ 1.168
...J
1.167L.---~--...J....._-""""----'-----'
0 .0
0.1
0.2
0 .3
SIN2 (PSI)
0.4
0.5
Reference
1 M.G. Moore and W.P. Evans, "Mathematical Correction for Stress in Removed Layers in
X-ray Diffraction R;esidual Stress Analysis", SAE Trans, 66 (1958)
8.1 Introduction
During processing, the shape of a diffraction peak can change (as well as shift)
and this is called "X-ray Line Broadening". This broadening can be an important
signature. For example, as shown in Fig. 8.1 (from [1] ), for peened soft steels this
can be even more important in controlling fatigue life than the induced stress. For
a well-annealed sample, the peak shape depends on the size of the source, finite
divergences of the slits at the x-ray tube and the receiving slits, the range of wavelengths in the beam, and the fact that in a diffractometer a flat specimen is only
tangent to the focusing circle at one point. 1 As a soft sample is deformed, there are
local strains due to the strain fields from dislocations and dislocation arrays. The
material is broken into regions with slight tilts with respect to one another due to
these arrays, subgrain boundaries, etc. Constructive interference occurs only
within each such region, and the peak (from such a region) is larger in angular
extent the smaller is such a region. This is so because when the region is small there
are not as many planes to cause destructive interference away from the exact Bragg
angle. To see this more clearly we adopt a treatment by Cullity [2].
Suppose that the crystal has a thickness t measured in a direction perpendicular to a particular set of reflecting planes (Fig. 8.2 ). Let there be (n + 1 )
planes in this set. We call e p the angle which exactly satisfies the Bragg law for the
particular values of A and d involved, or
A=2dsinell
(8.1 )
In Fig. 8.2, rays A,F, ... ,K make exactly this angle with the reflecting planes. Ray F',
scattered by the first plane below the surface, is therefore one wavelength out of
phase with A', and ray K', scattered by the nth plane below the surface, is n
wavelengths out of phase with A'. At the diffraction angle 2ell , rays A',F', ... ,K' are
completely in phase and add to form a diffracted beam of maximum amplitude,
hence the beam of maximum intensity (as intensity is proportional to the square
of the amplitude).
When incident rays that make Bragg angles only slightly different from e p are
considered, destrllctive interference is not complete. Ray B, for example, makes a
slightly larger angle e 1 , such that ray L' from the nth plane below the surface is
At low scattering angles, all of these factors are important. However, at high angles, where
stresses are normally measured, the dominant effect in focusing geometry is the wavelength
distribution. Even if only a K" line is employed ~},p. . = 1/2000. By differentiation of Bragg's
law (with d constant), ~2e, the range of angles, is 2 (!!J,}. .j)...) tan e ~ 10- 3tan e. At 1562e this
~0.3.
8.1 Introduction
231
Surface macro residual stress
cancelled
Surface macro residual stress
not cancelled
40
en
c
'cOJ
30
.8
OJ
- 20
::J
"0
OJ
::J
.Q\
. 10
OJ
Ul
OJ
L..
ct.
0
20
30
40
50
Hardness before peening, Rc
60
Fig. 8.1. Percent increase in fatigue limit due to peening as a function of hardness, showing the
separate contributions of x-ray line broadening and stress; SAE 86B45 steel. (These percentages
were obtained by cancelling the stresses with applied loads.) From Ref. [1]
F
O----~~~~_7~------~
1 ____________
2 ____________
__________
~_
__________
3 __~------------~-----K
L
L/ K'
N
'
"
/./ / -"N'
Fig. 8.2. Effect of crystal dimension on
scattering
(n + 1) wavelengths out of phase with B', the ray from the surface plane. This
means that midway in the crystal there is a plane scattering a ray which is an
integer plus one-half wavelength out of phase with ray B' from the surface plane.
These rays cancel one another, and similarly for the other rays from other pairs of
planes throughout the crystal, so that rays scattered by the top half of the crystal
cancel those scattered by the bottom half. The intensity of the beam diffracted at
an angle 2e 1 is zero. It is also zero at an angle 2e2 where e2 is such that ray N' from
the nth plane below the surface is (n -1) wavelengths out of phase with ray C'
from the surface plane. We have therefore two limiting angles, 2e 1 and 2e2 , at
232
I
Measured peak
29
Fig. 8.3. A diffraction peak is made up of many peaks from different subgrains. Their shape
depends on crystal size, their position on the local microstrain
which the diffracted intensity drops to zero. Thus, the diffracted intensity at angles
near 29 p (yet not greater than 29 1 or less than 29 2 ) has a value intermediate
between zero and the maximum intensity of the beam diffracted at an angle 29 p
The smaller the thickness, t, the wider is the range 29 1 - 29 2
We can think of the diffracted beam as a sum of many peaks. Each of these is
shifted due to the local strains in it, and each has a shape that depends on the size of
the region. This is shown in Fig. 8.3. The measured peak shape will depend on the
range oflocal strains and on the size distribution. Our goal in this chapter is to see
how to obtain such information from x-ray line broadening, and to compare and
contrast it to the strain obtained from peak shifts.
The shape of a diffraction peak from a monochromator on a neutron source or
synchrotron source can sometimes be adjusted to be a simple function, such as a
Gaussian curve. However, the shape of an emission line from a normal (sealed) xray tube defies such a simple desc~ption. Because of this, corrections for the shape
of a peak (takeI!: with a sealed tube) due to instrumental factors can be done only
very approximately by assuming such simple functions. Fofexample, if the shape
is assumed to be a Lorentzian function, the half-width of a peak from a well
annealed standard is merely subtracted from the broadened profile's half-width to
obtain a corrected profile's width. If a Gaussian function is assumed, the squares
are subtracted. Because it is well recognized that neither approach is generally
correct, an average of these two procedures is sometimes employed when
examining broadening. After this correction, with some further simplifying
procedures, we can get some qualitative information on the subgrain size and
microstrain. The size, D, affects peak broadening in the following manner:
A290=
A 180
Dcos9 1t
( 8.2)
(8.3 )
233
Actually, from our discussion above, peak broadening is related to the standard
deviation, (( ~: )
~2eocose=
2)
180[ D
A -2 ((~d)2)1/2
]
1t
d
sine.
(8.4 )
From a plot of ~2eo cos e vs sin e, D is obtained from the intercept and the rms
microstrain from the slope. Multiple orders of an hkl peak should be employed,
not just any peaks, as most materials are elastically anisotropic. The size is actually
an average over the volume of the x-ray beam.
Actually, there is a better way with fewer assumptions - using Fourier series.
Twenty years ago this was a bit tedious, but with small ( or large) computers this is
a relatively simple task. We will follow this approach in this chapter. If the reader is
unfamiliar with such series, Appendix C will provide the appropriate background.
J g(z)f(x-z)dz.
+00
oo
(8.5 )
234
f(y) -slit
h(x)
9 (z) - true
function
measured function
_~+~ u>O
flu)
={
!!+~.
2, 2
u< 0
I -3S x sol
IUI>3
u< x
u >x
/S/&,
1-6sxS-31
y(xl =
-3
f(x)~g(x)
x+3
J (~+~ )(-~+~+~)
J\Q+~)(Q+~-l!.)dU
2 2 2 2 2
-3
u 3
u 3 x
(-+-)(--+-+-)du
2 2
2 2 2
J f-~+~)(- ~.~.~)du
"3
du =?
-3
y(x)=f(x)~g(x)
x+3
f(u)
_L---X.._..L..---'-_"'---"o._u
-3
x
0
= ;>
We now write the functions in the convolution Eq. (8.5) as Fourier series:
1
h(x) = Ay
= ~y
+00
Joo g(z)f(x-z)dz
):
/
"Gn,exp (-21ti[n'-n]z) exp (-21tinx)dz .
-~~
A +S3 2 "F
~ n~
y -a/2
n'
(8.6 )
235
{To see this we examine the Fourier transform of the convolution y (x) .
y (s) = Jy( x)exp( + 21tisx)dx
(8.7 )
Letting x-u=w,
Yes) =Hf(u)g(w)exp[ +21tis(u+w)Jdudw,
=Jf(u)exp( +21tisu)duJg(w)exp( +21tisw)dw
=F(s)G(s) .
(8.8 )
Following the same approach, the reader can readily prove that if
w(x) =f(x)g(x), the transform ofw(x), Tw(x), is
Tw(x) = W(s) =JF(s-u)G(u)du
(8.9)
(8.10 )
(8.11 )
We need only have tbe Fourier coefficients for our broadened peak and those for a
peak from a sample that has few defects to obtan the coeffiCients of the true
diffraction peak without the effects of slits, source size, etc. To facilitate
computation, this equation is generally separated into sine and cosine terms (G~
and G~, respectively):
G~ +iG~ = [(H~ +iH~)/(F~ +iF~)] (Ay/a) .
a'
Gi _
n-
H~F~-H~F~ ) Ay
(F~)2+ (F~)2
(8.12 )
F~ - iF~,
(8.13a)
(8.13b)
This entire procedure was first developed by Stokes [3J and his original paper is
still well worth reading! A program for carrying out the Stokes' correction is given
in [4].
236
If the measured functions are symmetrical, the sine terms of the series vanish
and we have
G~ = (H~ap") A,.
(8.13c)
In other words, if the slit and measured functions are symmetrical, so is the true
function.
With these coefficients G, we can synthesize the true peak. And if you wish to
have the true function in absolute terms, instead ofjust its shape, it is vital to keep
track of all the constants, a and Ay (An easy way to do this is to choose a function
for which the Fourier coefficients can be readily evaluated analytically, and with
the same period as the function to be evaluated" numerically. The numerical
solution can then be normalized to the analytical solution.)
It is possible to obtain the Fourier coefficients of any real function by replacing
the integral for these coefficients by a sum for practical evaluation on a computer: 1
1
(21rinx)
Gn=-Lg(x)exp
- - ax.
(8.14a)
For evaluation, let x/a be t/120 (the function is divided into 120 parts,
ax=a/120). Then:
a 1 1=+60
(21tint)
G n= 120 1=~60 g(t)exp 120
or:
(8.14b)
where the sum is over integers t in the interval a. Now the true peak g (t) = g (x)
can be written as:
(8.15 )
Therefore,
1
G n= 120
+60
1=~60 ~Gn'
(21ti[n-n /]t)
exp
120
(21ti[n-n /]t)]
1
[
= 120 ~Gn' ~exp
120
.
(8.16 )
The exponential term is zero unless (n-n') /120 is an integer. Thus, G n is the sum
ofG n, values for '(n-n') equal to an integral multiple of 120. That is, n-n' =0,
120,240, etc. Hence n'=n, n'=n-120, n' =n+ 120, etc. If the coefficients fall to
nearly zero values as n increases in the range of n from - 60 to + 60, there will be
1 Alternately, a least-squares fit to the series can be employed; uncertain regions of the peak can
then be ignored. [Kidron, A., and DeAngelis, R.J., "Symposium on Computer Aided
Engineering" (G.M.L. Gladwell, ed.), p. 285. Univ. of Waterloo Press (1971).J
237
only one coefficient in this sum for each n; this then is the required test that our
numerical analysis is correct. Furthermore, only as many independent coefficients
as there are data points can be obtained, in this case, 120. Additional coefficients
are related to these by the periodicity. The function is only defined by those
coefficients at the discrete data points and all 120 coefficients are, of course,
required to properly reproduce the function.
It often happens that it is not convenient to use the same period for the "slit"
function and the measured function because the latter is so much broader; if we do
use the same period with the sharper function, we will have many intervals (t)
with zero height. A Fourier series representing a diffraction peak, say a 001' peak
for an orthorhombic cell (we can always choose such a cell) , is in terms of a period
which is the inverse of the fictious cell parameter a~ 1:
21tnx
- - = 21tnxa 3
(8.17 )
(2 sin ed"-)
(8.18 )
In this way the large regions between two orders of a peak where there are no data
are not included in the analysis.
The sum involving the Fourier coefficients will produce peaks with period
(l/a~) even though all of these but the first really do not exist. However, it is only
the actual peak that concerns us in this analysis and we may ignore the others.
Thus we see how to actually obtain the Fourier coefficients of our true peak
without the effects of slits and other broadening factors. Our "slit" function is
simply the same peak recorded from a sample that is well annealed. If we wish to
do so, we can then ~ynthesize a diffraction peak from a sample with distortions,
without these "slit" effects, employing the Stokes-corrected Fourier coefficients.
Then the effects of various treatments of the specimen could be compared by, say,
comparing the breadth of the peaks. This is really unnecessary, however, for we
shall see in the next section that we can learn a great deal about the specimen from
the corrected Fourier coefficients themselves! Note below that it will only be
necessary to obtain the coefficients and normalize them in this procedure; it is not
necessary to keep track of constants.
In this Fourier analysis, it is a good idea to record at least four to five times the
breadth of a peak on either side of it, and to compare the background of a
standard and the pattern to be analyzed; the background in both should be the
same and this comparison will help in any extrapolation of overlapping peaks on
the broadened pattern. These precautions will minimize oscillations in the
coefficients. The peaks to be analyzed should be at least 20 % broader than the
1 The series is in terms of a reciprocal space variable b~ = lja~. That is
21tnxja = 21tnxjb~ = 21tnxa~. lfthe reader is not familiar with reciprocal space he should consult
any text on x-ray diffraction.
238
standard peaks, or else the analytical procedures will result il! considerable scatter.
(This means, e.g., that a particle siZe larger than about 1000 A cannot be measured
this way, because of the instrumental broadening.) If the broadening is less than
this, there are special techniques to eliminate the K"'2 peak [5] that enable sizes as
large as 2000 A to be studied. The errors in the particle size and in the strains are
generally about 10 % via this procedure. We turn now to see how these sizes and
strains can be obtained from the Fourier coefficients.
The subscript "eu" means that we have left out such terms as the polarization
factor. We will bring this back later. The term s is the diffraction vector
(s=htb t +h2b2+h3b3 where the b i are reciprocal lattice vectors, and the hi are
continuous variables) and Cn is the position of a unit cell in terms of the axial
system: cn=nta t +n2a2+n3a3+Acn. The n i are integers. The term ACn is the
displacement of the nth cell. Carrying out the dot products:
Ieu(s) =
L
n
(8.19)
We will henceforth assume that each and every cell has the same structure factor,
F.
We measure power (P) not intensity, that is, the intensity integrated over the
number of grains (n) oriented to diffract and the area (A) of the receiving
surface (Fig. 8.6) .
P=HIdndA.
( 8.20)
Now:
( 8.21 )
where m hkl is the multiplicity. The angle 90 - e is that between the plane normal
and the incident beam. The equation for dn is the fraction of the surface of a sphere
of radius R covered by plane normals in the angular range dcx (assuming a random
distribution) .
239
da : d(6 S Ja
(8.22 )
Now, the angles dcx,d~,dy also describe a volume in reciprocal space, Fig. 8.7, so
that:
d V = dcxd~dy sin 29 .
(8.23 )
Also
d V = Adh l b l
( 8 2. 4a)
(8.24b)
mnR 2A,3
4V
c
HI SlD.eu9dhldh2dh3
( 8.25a)
and:
(P') eu = Peu/ (21tR sin 29) ,
(8.25b)
where P~u is the power per unit length of diffracting cone; a powder sample gives a
cone of diffraction with semiapex angle 29, but with a slit, say of unit height, we
measure only a piece of this cone, 1/21tR sin 29. Also, hence forth let M ( = mn)
represent the number of domains or regions of diffraction.
240
We can always defme a unit cell, such that the hkl diffraction peak is a 001' peak
from this new cell, as mentioned in Sect. S.2. Now, the distance from the origin in
reciprocal space to the diffracting point is the same regardless of the coordinate
system chosen, so that
(S.26 )
We continue with this new cell in order to simplify the mathematics; the variable is
now only h~, which is along the normal to the diffracting planes. Since
h~ b~ = 2 sin 6/A., then dh~ = ( cos 6 d26 ) / (b~ ) A.. Hence, replacing the integration
with respect to h~ with this expression and dropping the integration over 26,
(because we are measuring the shape of a peak vs 26):
(S.27)
+s (Arn-Arm)] }dh~dh~.
The factors sin 26 and F2 are removed from the integral because they vary slowly
compared to the exponential terms. The preintegral factor will be written as
K (6) 1. The integration is a projection along h~ and h~. Consider only one peak,
say the 001'. Then the limits of the integrals with respect to h'l and h~ are from -1/2
to +1/2.
Also:
Afn=xna'l +yna~+zna~,
(S.2Sa)
s~l'b~
(S.2Sb)
and
(S.2Sc)
s (Arn-Arm) =1'(zn-zm) .
Therefore, performing the integrals, and with these substitutions:
(P20)eu =
1t(n2-m 2 )
( S.29)
The sine terms are each zero unless m 1 = n 1 ,m 2 = n 2 in which case they are unity, so
that the sum over m 1 m 2,n 1 n 2 becomes N h, N h2 , where the N's are the average
number of columns in a plane perpendicular to the [001'] direction in a mosaic
regio~.. The remaining terms
are the sums between pairs of cells,
(L L)
m383
1 K (6) is an angular factor, and we can include in it the polarization we ignored earlier, so
1 +COS226)
that for flltered radiation the angular dependent portion is F2 ( sin 2 6
.
241
+00
-00
(P~8)
eu
= K (9) Nj,)~j,2Nj,3 {
. cos21tnh~ -
oo
-00
~n
(8.30)
< sin21tl'zn ) sin21tnh~ } .
h3
Equation (8.30) is in a form suitable for one dimensional Fourier analysis, as it is
a Fourier series with coefficients, A..,Bn. That is, we record power vs. 29 (which
can be converted to h~) and we have an equation which has the same variable.
Now:
A.. = (N.JN~3) <cos 21tI'Zu) ,
(8.31a)
(8.31b)
The coefficients An,Bn are those due to sample only, without instrumental
broadening; it is assumed that the Stokes' correction has already been applied.
Let us look at the various terms in this equation. Those involving displacement
depend on 1', or order, as we predicted in our qualitative considerations, while N n,
the particle size term, does not depend on 1'. The peak will be asymmetric if there is
a net displacement, i.e., if the sine term involving Zn does not average to zero, the
peak will be asymmetric toward lower angles for a positive net qisplacement, and
in the opposite direction for a negative net Zn' If there are many sine terms, i.e., if
the strain exists over a large distance, the peak will actually shift. Note also that:
Bn = -
n-+O
(~nh3 ),21tl<Zn),
(8.32)
(8.33a)
or:
(8.33b)
so:
(8.34 )
242
Therefore, information about the average strains could be obtained from the
initial slope of Bn vs n. However this is certainly a much more cumbersome
approach than measuring a peak shift!
Because the part of the Fourier coefficients due to particle size does not depend
on l' while that due to distortions does, these parts can be separated. Several orders
of a peak, e.g., hkl = 200,400,600, are analyzed and a plot is made of An versus l' for
each n and extrapolated to l' =0. The ordinate is N.JN~3' Unless the material is
elastically isotropic, the displacements will vary with crystallographic direction;
thus we cannot mix peaks representing different directions. However, with a
powder or a polycrystalline material, the third order often overlaps with another
peak. For example, with an fcc material the 600 peak-occurs at the same position as
the 442. We can eliminate the need for a third-order term if the strains are small, so
that the term cos (21t1' zn) in An can be expanded (cos x = 1 - x2/2 + x4 /24 + ... ).
Including only the first two terms, and taking the logarithm of the expansion:
In ( (cos 21tI'Zo> ) == -
21t2
(1') 2(Z~> .
(8.35 )
(8.36a)
or:
(8.36b)
where L = na~ is the true distance between cells in a column normal to the
diffracting planes. If there are no strains, only small particles, InAL versus h~ (for
each L) will be a horizontal line. If there is no particle size broadening but only
strains, all the lines for various L intersect at L = 0 at InAL = O. Note also that we
obtain (El//2 from the cosine coefficients, not the average strain.
According to Eq. (8.36b) only two orders of a peak are needed to separate the
effects of particle size and strain and obtain N.JN~3 and (El)1/2 vs. L. This is
because InAL vs. h~ is a straight line according to this equation (with a slope
yielding (El> ); it is possible to do the analysis with a powder or polycrystalline
specimen. However, Eq. (8.36b) resulted when we neglected higher terms than the
second in the expansion of the cosine. How valid is this? The term a~/ao is typically
5, (El)1/2 is at most 0.005. Substituting these values in the expansion of
cos 21tl'zn = cos 21t (hoa~/ao) nED' it will be found that nho can be 6 with the third
term in the expansion still only 6% of the second. Thus for the first few harmonics,
n, InAn versus h~ is, in fact, linear. 1
We have seen that if there are net strains over large distances, the peak will
shift. On the other hand, ifin the analysis the center of the actual peak is used, the
measured strain is the value above or below the long range (or mean) strain:
(El>meas = ( ( EL - Elong range) 2> = (El> - 2( ELElong range> + E210ng range'
(El>meaS=(El>-E2Iong range'
1 AL itself, as welI as InAL is approximately linear with h~: AL~Nn;Nh; [1-21t2h~U/a/)
(r.t> )], Delhez, R., and Mittemeijer, E.J., J. Appl. CrystalIogr. 9, 233 ( 1976), and this equation
may be used instead of Eq. (8.36b).
243
En
because
(8.37 )
The average <EL> is the long-range strain. In an analysis with the center of the
actual peak, we are therefore measuring the deviation from the mean or longrange strain, not the average strain. There have been attempts to use the values,
<E~>1/2 to calculate the stored energy due to strains. However, it is not the average
strain that we measure, but rather the width of the strain distribution <El>1/2at
each L or n, Fig. 8.8. The average strain could be zero, as shown, but there would
still be a range of strains.
Some typical data are presented in Fig. 8.9.
It is easy to show that NJN~3 ~ (1 = n;N~3) for small L. Take a column of,
say, five cells and evaluate N n. (The terms in the sum involving - n include counts
in the other direction. ) For this column, No = 5, N 1 = 4, N 2 = 3, N 3 = 2, N4 = 1,
N5=O. The term Nl;N~3 is 4/5, which is the same as (1-1/5). This implies that
Nn/N~3 decreases r~pidly with L if N\ is small; the peak will be broader for
smaller regions, as we anticipated. If the values of Nn/N~3 obtained from the
intersections of the curves with the ordinate in Fig. 8.9 [see Eqs. (8.36a,b)] are
plotted vs. L, the initial slope is:
-,
d(NnINh.}/dnln_o = -
N'
h3
(8038a)
(8038b)
244
10
v.
z09
...w~ 08
8 0 .7
O .OL---~----~-----L-----L----~----~----~--~~--~--J
20
40
60
eo
100
120
140
160
180
(200)
(400)
16
L: 201
0.2
L : 40A
L ~ 60A
0. 3
1.0
N n 0.8
0 .5
0 .6
= BOA
= 100A
N"30.6
L = 120A
0.4
L = 140 1.
0.2
0.0 '---:4;;';0:;---;;8';:;0--:1*20
;:;-~16"::0:-:::*:::~~<;;:'
- 0 .7
L : 160A
UA)_
~--------------------~----------------------~
Fig. 8.9. a Fourier cosine coefficients of 400 peaks, from Ag electrodeposited from
(KCN + AgCN) solution, and from a well-annealed standard. b Separation of particle size and
strain and (insert) the determination of particle size, using the corrected Fourier cosine
coefficients, AL from a. [From R.W. Hinton, LH. Schwartz, and J.B. Cohen, J. Electrochem. Soc.
110,103, (1963).]
245
area of the peak (see Appendix C), its value will be too small. The values from
beyond n = 2 - 4 should be extrapolated to n = 0 in doing this normalization. As
In (NJN~3) versus L is generally linear for n> 2, such a plot is a simple procedure
for this extrapolation. This has been justified theoretically, on the basis that the
strains are due to dislocations [7].
With a minimum of assumptions, we are able with this analysis to obtain the
rms strain (f.t)1/2 as a function of column length in a given crystallographic
direction and the mosaic size (Derr) in this direction. From this information we
can proceed to learn about the degree of anisotropy (from the size and rms strain
in different directions) and the imperfections. In a deformed material, (t/Derr) 2
can be taken as a dislocation density; that is, Derr is the spacing of such
imperfections. From the formulas for strain around a dislocation, the data on
(f.t)1/2 can also be used to obtain a density [8]. These two should agree if the
dislocations are randomly arranged, but if (t/Derr) 2 is smaller than the value
obtained from the strains, the dislocations may be clustered. The densities
calculated in thi~ way are in agreement with those observed in the electron
microscope [8]. (If there are cells or clusters of dislocations, Derr is a measure of
the cell size not the dislocation spacing, but this can generally be ascertained by
comparing the densities obtained with (f.2) and D as mentioned.) This technique
is especially useful for high concentrations of dislocations as this is exactly where
the electron microscope is least useful because of overlap of images. By combining
the two tools, a whole range of concentrations can be studied, with a region of
overlap sufficient to allow comparison of the two,
With materials like polymers, there is often only a single peak. Techniques for
obtaining the mosaic size and (f.~) for a single peak have recently been described
[9]. Finally, equation for the errors in D and (f.~> based on the counting statistics
have been developed [to]. Just as for the residual stresses, software can be
developed to obtain these quantities to an operator-specified precision [10].
Finally, composition gradients can cause peak broadening, particularly peak
asymmetry, due to the range of interplanar spacings produced by the gradient.
Thus, the sine coefficients can be employed to obtain information on the gradient
after correcting these for the strain and particle-size effects with information from
the cosine coefficients; see [11].
We have now examined all the signatures of residual stresses and strains on the
diffraction pattern.>We hope the reader feels equipped and ready to start his own
measurements!
Problem
(Fig. 8.1 0 )
Notes:
1) Given profiles are symmetrical (for simplicity).
2) The period (from 29.4-30.6 deg.9) is the same for both.
3) The number of intervals ainstrumental and abroadened are different. (Usually
ainstrumental should be a multiple of (abroadened) 12 to give Fourier coefficients at
the same L values.)
246
-3
29.L.
81
~------------ a 3 ------------~
10
Instrument profile
(12 intervals)
0
- L.
-6
L.
29.L.
30,0
81
x-
8-
1------------------- a 3 ------------------~
~
Fig. 8.10
4) The period is divided into intervals of equal L\9 (for 9> 60, equal intervals of
L\ sin 9 have to be used, i.e., intervals of h~ ) .
5) Origins, 90 , are at centers of gravity of peaks. The 90 's need not be the same.
6) Background is assumed to be zero.
7) Wavelength is 1.5406 A.
The Fourier cosine coefficients, An, are given by
An= -1 a/2
L
a
x= -a/2
(21tnX )
247
References
2
3
4
5
6
7
8
9
10
11
W.P. Evans, R.E. Ricklefs and J.F. Millan in "Local Atomic Arrangements Studied by X-ray
Diffraction", (eds: J.B. Cohen & J.E. Hilliard) p. 351, Gordon and Breach, New York
(1966 )
B.D. Cullity, "Elements of X-ray Diffraction", 2nd Edition, Chap.3, Addison Wesley,
Menlo Park, California (1978)
A.R. Stokes, Proc. Royal Soc. London 61, 382 (1948)
R.I. DeAngelis in "Local Atomic Arrangements Studied by X-ray Diffraction" (eds: J.B.
Cohen & J.E. Hilliard), p. 271, Gordon and Breach, New York (1966)
R.J. De Angelis, ty1etallography, 6, 243 (1973)
B.E. Warren, "X-ray Diffraction", Chap. 13, Addison-Wesley, Reading, MA (1969)
R.L. Rothman and lB. Cohen, J. AppL Phys. 42, 971 (1971)
D.E. Mikkola and J.B. Cohen in "Local Atomic Arrangements Studied by X-ray
Diffraction" (eds: J.B. Cohen & J.E. Hilliard) p. 289, Gordon and Breach, New York
(1966)
R.K. Nandi, H.K. Kuo, W. Schlosberg, G. Wissler, J.B. Cohen, and B. Crist, Jr., J. AppL
Cryst. 17, 22 (1984)
W.H. Schlosberg and J.B. Cohen, J. AppL Cryst. 16, 304 (1983)
R. Delhez and E.M. Mittemeijer, J. AppL Phys. 49, 3875 (1978)
Chapter 2
1. a) From the formula
cr'ij = aikajlcrkl, where cr;j is defined in L ,
( cr~3) = a3ka31crkl
=a~lcr11 + 2cr 12a 31a 32 +2cr13a31a33 +2cr23a32a33 +a~2cr22 +a~3cr33
The direction cosine matrix is given by
a ij =
035 0.61
-0.87 O. 5
0.35 0.61
-0.71
0.71
cr~2 =
92.0MPa
cr~3= - 225.0MPa
cr~3 =
31.0MPa.
249
Chapter 4
1. a) P = 122 calories/sec. Enthalpy to melt 100 gms of Cu is 11.1 kcalories.
Melting occurs in 91 sec, if the heat capacity is 6.65 cal/deg. mole
b) At steady state all of the heat goes into the water. A1: = 3. 7C.
2. tan(1800-29) =rjD (back-reflection geometry).
a) Bragg's Law:
nA. = 2d sin 9
A. = 1.54178 A
(aO)Fe = 2.8665
d = 1.43325 A .
r = 0.114m
1P
I
(2S)b - (2s)A
---+---~-----'";B
= 2.6
Chapter 5
a) Since there is curvature in "d" vs sin2 tp:
(i) O"ij = O"ij (z) .
(ii) The stress state in the surface is homogeneous;
O"~=constant
sin 2 tp
0"33
Total tp-range
Low tp-range
High tp-range
-466
-629
-414
-466
-629
-414
146
73
113
(MPa)
250
d)( d o )1p
'V-range
2.86734 A
2.86692
2.86715
Total
Low
High
e) 'V-range
0'11
0'22
0'33
Total
Low
High
-612
-702
-527
-612
-702
-527
0
0
0
(MPa)
Chapter 6
1. (i) 160.729
(ii) 0.029929
(iii) (~=Q.) =0.90795 A
(iv) Error'{ ~= 0) = 0.00006 A
2. 0'., = 608.8 MPa
. Stat. error = 20 MPa
Chapter 8
a) For each n, take the sum over all values of x. Do it for n=0,1,2 for the
instrumental profIle.
1
a/2
(21t(0)X)
:.Ao=12x="'fa/2f(x) cos 12
(1)
1
a/2
(21t( 1
12
)x) (1)
(1)
251
All sine coefficients are zero because the profIles are symmetrical.
Likewise for the broadened profIle:
1
a/2
(21t (0)
x)
6
(1) =20/6=3.3333
a/2
a/2
where Hn are the broadened peak coefficients, Fn the instrument peak coefficients
and Ay the area of the instrument peak. The term Ay/a can be set = 1. Thus for our
simple profIles, Stokes corrected coefficients are
0.6500
0.2500
Go=1/1 =1;G t = 0.87028 =0.7469;G2= 0.60194 =0.41532
Appendix B
B.l Introduction
In Sects. 5.13, 5.14, the meaning of oscillations in "d" vs. sin 2 tp and the causes for
such behaviour were discussed. It was shown that such oscillations could result
from an inhomogeneous distribution of elastic residual strains. Such an inhomogeneous distribution can arise from an inhomogeneous distribution of plastic
deformation on a micro scale and/or from interaction strains generated in an
inhomogeneous material in response to an applied or macrostress. Over the years,
oscillatory "d" vs. sin 2 tp plots have been the subject of numerous studies and much
controversy. Various approaches, from elaborate non-linear least-squares curvefitting to tota-l disregard for oscillations by using two-tilt analysis for oscillatory
data, have been proposed and used. In this appendix some of the more applicable
methods are reviewed briefly. The reader is warned that at this point, none of the
techniques discussed below, or indeed any other techniques, have been able to
satisfactorily solve this problem.
253
Diffractometer axis
Incident beam
Diffracted beam
4. The lattice constant "d", measured by x-rays, possesses a maximum, dmax> for
each orientation of the sample. From this maximum value, d max, the lattice
constant varies with orientation of the sample according to a distribution
function, until ethe "dB" value of the B regions is reached.
With these assumptions, the dependence of the interplanar spacing on the
orientation may be expressed as:
(B.1)
Here f( (l,~) is the distribution function of a particular (hkl) plane relative to the
sample coordinates and (l and ~ are defined in Fig. B.t.
If in addition to the microscopic strain distribution there are macroscopic
stresses in the material, the combined equation is given by:
(B.2)
{Here it is assumed that the macrostresses contributing to cr~ yield a linear "d" vs.
sin 2 '1' dependence. Thus, reaction strains, tiT, are assumed to be zero
[Eq. (5.53)].}
254
Appendix B
0.8382 ,..---...,----,-----.--,---,---,
0.8381
t 0.8380
u
0.8379
0.8378
a
1.0
0.8
-:T
0.6
o'
0.4
0.2
b
0.1
0.2
0.3
0.4
0.5
Fig. B.2. "d" vs. sin 2 \jl (a) and f( (X,~) vs.
sin 2 \jl (b) behaviour required for the use
of Marion-Cohen Method. (In both cases
similar oscillations are observed.) (From
Marion [1] )
sin 2 tjJ
not be true for all cases. When a textured material (which had been stressrelieved) is stressed elastically, oscillations appear in the "d" vs. sin 2 tp curve,
which, upon unloading, vanish [2,3]. This observation was utilized by Dolle and
Hauk [4] in a different approach. This method is discussed below.
<'
dq,,,,' + t33ij
, ) 'aij >,
do do = E33 >= <(S33ij
(B.3)
where S~3ij are the single-crystal elastic compliances in the laboratory co-ordinate
system, Lj, and t~3ij are the elastic interaction terms of a grain and the surrounding
matrix. The carats in (B.3) indicate that the average is taken over all the
255
1.06210 rN
-1.06200
f-
CfA-21MPa
1.06220
1.06210
f-
-1.06200
f-
f-
42MPa
I---,I_-,I_ _IL..-_L..-I_-,---I_.L.1---1
1.06190 L..L.-
1.06220 r-
1.06210 fN
-1.06200
f-
1.06190 r-
,
0.1
I
0.2
63 MPa
1
1
0.3 0.4
sin 2 ",
I
0.5
0.6
0.7
Appendix B
256
(1::~3>"''I' = ~ Bo + Bicos <I> + Al sin <I> + B2coS 2 <1> + A2sin 2 <1> + ... .
(B.4)
The Fourier coefficients A;,B; are then evaluated by integrating Eq. (B.4) over
3600 in <1>:
1t.
Ak
B =
k
360,
J0 (1::33 \'1'.
sin k<l>
kA.. d<l>.
cos ~
(B.5)
These coefficients are linear functions of the strains in the surface coordinate
system [these equations can be obtained by comparing Eq. 5.4 with Eq. (B.4)].
Thus, it is possible to determine the strains from the Fourier coefficients, and the
stresses from the appropriate form of Hooke's law.
The 'P-integ~al method is similar to the <I>-integral with one exception. The
strain (1::~3> is expressed as a polynomial in terms of'P and integrated over
'P from -45 to 45 in order to obtain the coefficients from which the strains are
obtained.
These methods are not widely used. The <I>-integral technique is a very time
consuming procedure and is rarely used. It does yield values in excellent agreement
with the standard methods (discussed in Chap. 5) for regular stress/strain
Or7----------~~--------~~
'-_/
"
" 0
References
257
distributions and has the added advantage that for a given tp-tilt, variation of <I>
does not change the penetration depth t, so that the same x-ray average is seen at
all <I>-rotations [9, 10J. The coefficient matrices A~k,B~k for the tp-integral method
are usually ill conditioned, which magnifies experimental errors, causing large
errors in the final stress values [11]. In these methods, however, causes of
oscillations other than macro-stress gradients in the z-direction are not taken into
account. These methods should not be used for analysis of oscillatory data unless
it is determined independently that the oscillations are indeed caused by a macrostres gradient. The idea that a stress gradient similar to that shown in Fig. B.4
causes oscillations in "d" vs. sin 2 tp is quite valid and such a gradient can occur in
practice due to a peculiar load distribution during deformation processing.
References
2
3
4
5
6
258
7
8
9
10
11
Appendix B
W. Lode and A. Peiter, Hiirterei-Tech. Mitt., 32, 235 (1977)
W. Lode and A. Peiter: Metall, 35, 578 (1981)
C.N.I. Wagner, B. Eigenmann and M.S. Boldrick, preprint of The Phi-integral method for
X-ray Residual Stress Measurements, Dept. of Mat. Sci. & Eng., University of California,
L.A, CA 90024 (1986)
B. Eigenmann, Computer-aided X-ray Residual Stress Analysis in High Strength Aluminum
Alloys for Production Control during the Manufacturing Process, Master's Thesis,
Universitiit Karlsruhe (TH), West Germany
C.N.I. Wagner and M.S. Boldrick, The Psi-differential and Integral Methods for Residual
Stress Measurements by X-ray Difraction, Dept. of Mat. Sci. & Eng., University of
California, L.A, CA 90024 (Paper presented in the 1983 Denver X-ray Conference)
If a function, f( x), is periodic with period (a), has no more than a fmite number
of discontinuities in a fmite interval ofx, and the following integral is finite (these
restrictions are satisfied by most functions encountered in natural phenomena):
a/2
-a/2
If(x)ldx,
then f( x) can be decomposed into an infinite Fourier series of sine and cosine
terms:
co
21tnx
co B . 21tnx
f(x) =Ao+2 n"f 1 ~cos-a- +2 n"f 1 nsm-a-
(Col)
+Ja / 2 cos--cos-21tnx
21tmx d
{O
X=
-8/2
if n =4= m,
.
a/2 if n=m,
21tnx
21tnx
cos--sin--dx=O,
-a/2
a
a
+ 8/2
(C.2b)
. 21tnx . 21tmx
+Ja / 2 sm--sm-d X= {O
-8/2
(C.2a)
ifn=4=m,
.
a/2 if n=m.
(C.2c)
( C.3a)
21tmx
f(x)sin--dx =Bma,
-a/2
a
(C.3b)
+a/2
+a/2
+a/2
-a/2
f(x)dx
=Aoa.
(C.3c)
The last relation tells us that the area of the function in one period is proportional
to the first coefficient, Ao. Furthermore, if the function is even (i.e., symmetrical
about the x = 0 axis) , then from Eq. (C.3b) all Bn = 0 and a cosine series results. If
260
f(x) is odd, or inverted through the origin (i.e., antisymmetric), then all the
Au = 0 from Eq. (C.3a) and a sine series results. For a general function, f( x), both
terms are necessary.
We can write our Fourier series in a slightly different way if we note from
Eqs. (e.3a,b) that ~-n)=Au and B<-n)= -Bn. Then,
f(x) =
+ 00
21tnx
+ 00
21tnx
Aucos-- + L Bnsin- - .
-00
a
-00
a
(e.4 )
The restrictions we have placed on the coefficients maintain a general series for
f(x). For example, when n= -4 the sine term is negative, and if Bn did not
change sign in Eq. (e.4) this sine term would cancel the term for n = + 4 and
similarly for all n, -n; only the cosine series would remain. Note that Bo =0, so it
may be included in this compact notation.
We can write the series in a still more compact way if we define a complex
coefficient:
(C.5)
Cn=Au~iBn ,
f(x) =
+00
-00
C ne- 2"inxa.
(e.6a)
+ 00 (
21tnx
L Aucos--00
a
. 21tnx )
+ Bnsm-
. +00 (
. 21tnx
21tnx)
L Ausm-- Bncos-- .
-00
a
a
-1
(e.6b)
The second sum must be zero to correspond to Eq. (C.4), which holds for a real
function. This condition is satisfied since ~ _ n) = Au and B( - n) = - Bn ( i.e.,
C(-n)=C:, where the asterisk denotes "complex conjugate"). Using the orthogonality relations, Eqs. (e.2a - c ) , the reader may show that the complex Fourier
coefficients C m can be obtained from
aCm=
+a/2
f(x)e<+2nimx /a)dx.
(C.7)
-a/2
Consider two functions f1 (x) and f2 (x) each with period a, multiplied together
and averaged over this period,
-1 +a/2
J fdx)f2(x)dx = -1 +a/2
J
a
-a/2
+ 00
-a/2
n=-oo
1 +00
= - L
(Cdn
n=-oo
+00
n=
-00
}
(Cdne(-2ninx/a) f2(x)dx
+a/2
-a/2
f 2 (x)e(-2ninX/a)dx
(Cdn(C 2 ):,
(e.S)
261
Using the Fourier series representations of these functions, we have shown that
the average value ofthe product of the functions is the sum of the products of the
coefficients. Suppose the two functions are identical. Then we are taking the
average value of [f( x)] 2 over the period. This result may be written as
1
+~2
-~2
- J
(f(x) )2dx=
+00
L IC nl2
n=-oo
+00
n=
(C.9)
-00
According to Eq. (C.9), which is known as Parse val's theorem, the sum of the
squares of the Fourier coefficients will give us the average "intensity" of the
function. We can see this result directly from the series itself; look at Eq. (C.4),
and consider the average value of the square of one term, say, A2cos 21t2x/a. The
average value of the square is 1/2(A2) 2. But there are +n and -n values, so the
average of the pair of these is (A 2 ) 2. The same is true for all terms. The sum of the
squares of the coefficients is merely the sum of the average "intensity" in the unit
cell of each wave in the series, and this is the same average we obtained by squaring
the total series to arrive at Parseval's theorem. This is so because the terms do not
interact.
Ifwe plot the coefficients An and Bn as a function ofn/a, such a plot will consist
of a series of discrete lines spaced l/a apart. As the period a increases, these lines
move closer together, and as the period approaches the limit of infinity, a
continuous curve of coefficients develops. This limiting case of a Fourier series will
allow us to represent non periodic functions as combinations of orthogonal plane
waves. Rewriting the series, Eq. (C.l ), and using the definitions of the
coefficients,
1 +a/2
00 1
21tnx +a/2
21tn~
f(x)= - J f(~)d~+ 2 L -cos- J f(~)cos--d~
a -a/2
n=l a
a -a/2
a
00 t
21tnx +a/2
21tnll
+2 L -sin-- J f(ll)sin--dll
n=la
a -a/2
a
1 +a/2
2 00 +a/2
( X -11 )
=- J f(~)dll+- L
J
f(ll)cos21tn
dll,
a -a/2
a n=l -a/2
a
( C.10)
where 11 is a dummy integration variable. Let the period a approach infinity; the
first term becomes zero, and if the function still satisfies the conditions for a
Fourier series, the integral is finite. If we further state that when l/a approaches
zero as n approaches infinity, n/a approaches zero, then n/a can be considered as a
continuous variable, which we shall call s. With these conditions, Eq. (C.1 0)
becomes
00
+00
f(x) =2 J ds J f(ll)cos21ts(x-ll)dll.
(C.1l )
o
-00
This important result is known as Fourier's integral theorem.
262
f( x) = 2 Jds
o
co
-co
f( 11) {cos 2nsll cos 21tsx + sin 2nsll sin 21tsx} dll
co
co
-co
= 2 Jcos 21tsxds
co
co
-co
+ 2 Jsin 2nsxds
( C.12)
Representing the cosine and sine integrals of f( 11) by a (s) and b (s),
co
a ( s) =
(C.13a)
J f(ll)sin2nslldll,
(C.13b)
-co
co
b(s) =
-co
1/2 {
a (s)
[a2(s)+b2(s)]1/2cos2nsx
b(s)
.
}
+ [a2(s) + b2(s)] l/2sm2nsx ds.
Now, letting Rs= [a 2 (s) +b 2 (s)]1/2 and tanO s = -b(s)ja(s),
co
JRscos{2nsx+<I>s}ds
f(x)=2
=
co
i ( 2nsx + <l>s) ] } ds .
<I>-s= -<I>s
b( -s) = -b(s),
Rs=R-S'
co
JRsexp ( o
co
JRsexp ( o
(C.13c)
263
Thus,
f( x ) =
00
JRsexp ( o
-00
00
-00
Finally, letting
F ( s) = Rsexp ( - i<l>s) = a ( s) + ib ( s) ,
f ( x) =
00
F ( s ) e - 2lt;SXds .
(C.14 )
(C.15 )
-00
This is the more common expression of Fourier's integral theorem. Note from
Eqs. (C.13a-c) that when f( x) is real and even, b( s) =0 for all s, while for f( x)
real and odd, a (s ) = 0 for all s.
Substituting Eqs. (C.13a - c) in Eq. (C.14), we obtain
F(s) =
+00
f(x)cos21tsxdx+i
-00
+00
f(x)sin21tsxdx,
-00
or
F ( s) =
+00
J f ( x ) e + 2lt;SXdx .
( C.16)
-00
The function F (s) is known as the Fourier transform off( x). Note the similarity
between Eqs. (C.15) and (C.16). The two functions F (s) and f( x) related by
these equations are known as a "Fourier pair", and the variables s and x are
known as a "conjugate pair". We can abbreviate these two equations as:
Tf(x) =F(s)
(C.17a)
and:
T-1F(s) =f(x) ,
(C.17b)
where T and T- 1 are read as "transform of' and "inverse transform of',
respectively. We can think of Eqs. (C.15) and (C.16) in terms of two spaces: a
Fourier transform space, s, for F (s), and a "real" space, x, where our function
f( x) is plotted. From the nature of the Fourier transform, we can see certain basic
properties:
F(O) =
+00
-00
f(x)dx, or f(O) =
+00
F(s)ds.
(C.18 )
-00
The integral of a function in one space equals its transform at the origin of the
other space. Other important properties to note, which the reader can readily
264
F(S)
fIx)
-II
-I
+11
x-
+I
5-
prove, are
Tcf(x) =cF(s) ,
(C.19a)
TLCifi(x) = LciFi(s) ,
(C.19b)
(C.19c)
where c is a C6nstant. An important example occurs for c = -1 in (C.19c):
Tf( -x) =F*(s) .
( C.19d)
+00
f(x)e+2nisxdx=
-00
+1/2
-1/2
e+2nisxdx,
( C.20a)
and
F(O) =
+ 1/2
J' f(x)dx=l.
-1/2
(C.20b)
265
Now, if t is large the tranform is sharp, and if t is small the transform is broad.
Thus the transform has a reciprocal nature with respect to real space. This is also
true of the Fourier coefficients of a function; they fall off with n more rapidly if the
function is broad than if it is sharp.
A very useful treatise on Fourier mathematics is "An Introduction to Fourier
Analysis", by R. D. Stuart, Methuen Co., Ltd., London (1961).
1)
X-ray Wavelength
2)
3)
4)
5)
6)
7)
1 "International Tables for Crystallography", Vol. I (1952), Vol. II (1959), Vol. III (1962)
(K. Lonsdale, ed.), Vol. IV (1974) (J. A. Ibers and w. C. Hamilton, eds.). Kynoch Press,
Birmingham, England.
mU/Q, crn1/g %
Mass Fraction
108.000
1.000
100.000
mu total = 849.9600
Depth ip microns
G.
1jl=0
18
26
32
39
45
0.50
0.67
0.95
3.988
6.379
17.238
3.775
6.038
16.316
3.546
5.672
15.327
3.323
5.315
14.360
3.008
4.811
12.999
2.693
4.307
11.638
0.140
0.223
0.603
0.131
0.209
0.565
0.118
0.189
0.512
0.106
0.170
0.458
Depth in Mils
0.50
0.67
0.95
0.157
0.251
0.679
0.149
0.238
0.642
mU/Q, cm1/g %
Mass fraction
AI
158.000
1.000
100.000
mu total =426.4420
Depth in microns
G.
0.50
0.67
0.95
7.612
12.176
32.900
18
26
32
39
45
7.133
11.409
30.828
6.614
10.580
28.587
6.103
9.762
26.378
5.374
8.595
23.225
4.630
7.406
20.012
0.260
0.417
1.125
0.240
0.384
1.039
0.212
0.338
0.914
0.182
0.292
0.788
Depth in mils
0.50
0.67
0.95
0.300
0.479
1.295
0.281
0.449
1.214
268
mujQ, cm1jg %
Mass fraction
Ni
Co
W
Cr
Mo
145.700
124.600
495.500
85.710
457.400
0.562
0.082
0.257
0.065
0.034
68.500
10.000
10.000
9.000
2.500
mu total = 2008.720
Depth in microns
G.
11'=0
18
26
32
39
45
0.50
0.67
0.95
1.553
2.485
6.714
1.441
2.305
1.319
2.109
5.699
1.197
1.915
5.174
1.022
1.635
4.418
0.842
1.346
3.638
0.052
0.083
0.224
0.047
0.Q75
0.204
0.040
0.033
0.053
0.143
6.i27
Depth in mils
0.061
0.098
0.264
0.50
0.67
0.95
0.057
0.091
0.245
0.064
0.174
Element
Fe
Cr
C
Mn
Mo
Si
mujQ,cm1jg %
Mass fraction
108.000
85.710
14.460
96.080
457.400
202.700
0.813
0.169
0.002
0.005
0.008
0.002
79.800
17.800
1.030
0.480
0.480
0.410
mu total=811.2000
Depth in microns
G.
11'=0
18
26
32
39
45
0.50
0.67
0.95
4.179
6.684
18.061.
3.956
6.327
17.095
3.716
5.943
16.059
3.481
5.568
15.047
3.151
5.041
13.620
2.821
4.513
12.194
0.146
0.234
0.632
0.137
0.219
0.592
0.124
0.198
0.536
0.111
0.178
0.480
Depth in mils
0.50
0.67
0.95
0.165
0.263
0.711
0.156
0.249
0.673
269
= 4.460000 g/cm
e=70.50000;
Element
mU/Q,cm 2 /g %
Mass fraction
Ti
Al
Sn
202.400
50.230
253.300
0.911
0.028
0.061
92.500
5.000
2.500
mu total = 892.0000
Depth in microns
Ox
\jJ=0
18
26
32
39
45
0.50
0.67
0.95
3.662
5.858
15.829
3.437
5.498
14.855
3.194
5.108
13.803
2.954
4.725
12.767
2.612
4.178
11.290
2.265
3.623
9.789
0.126
0.201
0.543
0.116
0.186
0.503
0.103
0.164
0.444
0.089
0.143
0.385
0.144
0.231
0.623
0.135
0.216
0.585
Material
Radiation
hkl
(1+v)/E
x to- 8 psi
Ref.
Aluminum
A15083-H23
A15083-H23
A15083-H23
Al2219-T87
Al 7075
Co
Cr
Co
Cu
Cr
Cr
420
311
420
511/333
311
311
14.09
12.53
12.55
12.55
11.71
11.33
[6]
[3]
[3]
[3]
[8]
[7]
ARMCO Fe
0.39 %C steel
0.73 %C steel
0.73 %C steel
Fe (4.3 %C, 0.57 %Si,
3.96 %Mo)
Fe(O.1 %C,0.82 %Mn,0.3 %Si
4.9 %Ni,0.55 %Cr,0.57 %Mo
D-6ac
200 Maraging steel
Railroad steel
HSLA 328
1045
1045
4820, carburized
4340, Rc50
410SS, Rc22
4tOSS, Rc42
422SS, Rc34
422SS, Rc39
304SS
Cr
Cr
Cr
Co
211
220
211
310
2.41
3.88
4.38
5.16
[5]
[6]
[6]
[6]
Fe
4.76
[2]
Cr
Cr
Cr
Cr
Cr
Cr
Co
Cr
Cr
Cr
Cr
Cr
Cr
Cr
211
211
211
211
211
211
3tO
211
211
211
211
211
211
220
4.38
3.24
4.26
4.06
3.50
3.49
4.99
3.87
4.08
3.91
3.98
3.79
3.83
4.95
[2]
[8]
[8]
[8]
[10]
[5]
[5]
[4]
[7]
[7]
[7]
[7]
[7]
[7]
Incoloy 903
Incoloy 903
Incoloy 800
Cr
Cu
Cr
220
331
220
3.21
7.09
4.27
[7]
[8]
[7]
[ 6]
[ 7]
[ 8]
[ 9]
[to]
Maucherauch 1966
Prevey 1977
Ranganathan 1976
Wooden et al. 1960
Schlosberg 1979
Errors are not generally given in these references; they are useful in comparative studies, but for
highest accuracy they should be measured.
271
Material
Radiation
hkl
Incoloy 800
Inconel6oo
Inconel6oo
Inconel 718
Inconel 718
Inconel 718
Inconel X750
Monel K500
Nickel
Nickel
Ti-6A1-4V
Ti-6A1-4V
Ti-6A1-2Sn-4Zr-2Mo
Ti-SAI -1Mo-1V
Cr
Cr
Cu
Cu
Cu
Cr
Cr
Cu
Cu
Cu
Cu
Cu
Cu
Cu
420
220
420
331
331
220
220
420
420
331
213
213
213
213
4.65
4.73
4.33
4.35
5.00
3.21
2.71
4.76
4.36
4.83
8.20
7.51
6.76
6.99
[7]
[7]
[7]
[8]
[7]
[7]
[7]
[7]
[6]
[6]
[7J
[1]
[7]
[1]
ex-Brass
~-Brass
Co
Co
400
310
10.62
13.92
[6]
[6]
Zircoloy-2
Cr
104
8.48
[9]
Copper
Co
400
9.35
[6]
Tungsten
Co
222
2.15
[6]
Uranium
Cu
116
2.56
[9]
(1+v)/E
x 10- 8 psi
Ref.
References
Baucum, W.E., and Ammons, A.M. (1973) Adv. in X-Ray Analysis 17, 371-382
Braski, D.N., and Royster, D.M. (1967) Adv. in X-Ray Analysis 10, 295-310
Cohen, J.B. (1964) Report on Tungsten Lattice Parameter Round Robin, X-Ray Subcommittee
of SAE Iron and Steel Technical Committee, Div. 4
Dolle, H., and Hauk, V. (1978) Z. Metallkunde 69, 410-417
Esquivel, A.L. (1969) Adv. in X-Ray Analysis 12, 269-298
Faninger G. (1970) J. Soc. Mat. Sci. 19,42-57
French, "tl.N. (1969) J. Amer. Cer. Soc. 52, 271- 275
Hanabusa, T., Fukura, J., and Fujiwara, H. (1969) Bull. of J.S.M.E. 12, 931 -939
Hilley, M.E., Wert, J.J., and Goodrich, R.S. (1967) Adv. in X-Ray Analysis 10,204-294
Hilley, M.E., Larson, J.A., Jatczak, C.F., and Ricklefs, R.E. (eds.) "Residual Stress Measurements by X-Ray Diffraction," SAE Information Report J784a. (1971) SAE, Pennsylvania
James, M.R. (1977) Ph.D. Thesis. Northwestern University, Evanston, Illinois
James, M.R., and Cohen, J.B. (1977) Adv. in X-Ray Analysis 20,291-308
Kelly, C.J., and Eichen, E. (1973 Adv. in X-Ray Analysis 16, 344-353
Kelly, C.J., and Short, M.A. (1970) Adv. in X-Ray Analysis 114, 377-387
Kirk, D. (1971) Strain 7, 7 - 14
Koistinen, D.P., and Marburger, R.E. (1959) Trans. ASM. 51,537-555
272
Subject Index
69
35
274
Subject Index
equivalent directions 31
equivalent inclusion method 58
equivalent slip systems 42
errors, beam optics 190
omega goniometer 190-199
psi goniometer 200-203
Eshelby's tensor 56, 57
Fatigue crack, associated residual stresses
fatigue response 1, 8
filters 84
fixed count method 182
fixed time method 182
flow curves 39
fluorescent radiation 83
focal point 191
force balance 23, 38
force vector 15
Fourier analysis 238,259
Fourier series 234-238
fractional coordipates 29
free suffix 22 .
Indexing, tensors 15
incoherent scattering 85
inhomogeneous distribution 13
inhomogeneous materials 44
inhomogeneous plastic flow 43, 44
instrumental errors 190-205
intensity (diffracted) 88, 97
interference (constructive) 87
isotropic distribution 13
K absorption edge 84
kinematic theory 90
Kronecker's delta 26
Kroner average 72
Lame's constants 27
lattice plane spacings 31
lattice point 28
Laue camera 93, 94
205
Neerfeld average 68
neutrons, absorption of 114
diffracting volume 154
penetration depth of 115
scattering of 115
neutron flux 111
nuclear reactors 111
normal stresses 15
Machining stresses 8
macrostress 47
macrostress gradient-correction for
magic mirror 1
Marion-Cohen method 252
matrix notation 33
microstress 47, 53
Miller indices 30
Monochromators 90
mosaic structure 89,240, 241
Moseley's law 78
multiplicity 98
Subject Index
Poisson's ratio (selected materials) 27
polarization factor 85
for monochromators 91
polychromatic radiation 77
portable residual stress units 213, 214
position sensitive detector 105
potential well concept 32
principal strains 25
principal stresses 24
principal tensor components 22
proportional detector 104
proportional limit 44
pseudo-macro stress 54
psi-axis offset 199
psi-position missetting 202
psi-splitting 119
pulsed beam neutron source 114
pulse-height analyzer 105
Radial stresses 50
radiographic analysis 75
ratemeter 104
regular "d" vs. sin plots 118
residual stresses (definition) 47
analysis 47
.
macrostresses 47--49
microstresses 52-54
measurement methods 4--7
stress gradients 140
stress in a gear tooth 222
stress in bolted plate assembly 216
stress in crankshaft journals 220
stress in ring assemblies 215
stress in rolling 2
stress in solid circular cylinder 218
stress in shot-peened references 223
stress in welding 2
Reuss Average 65, 71
rigid body translation 17
Roentgen 75
rotating anodes 80
Safety precautions 212
scattering 84
from planes of atoms 86
from the unit cell 87
Schmid factor 43
Schmid's law 42.
scintillation counter 107
sealed tubes 80
self-consistent method for average
elastic moduli 67
shear modulus 26
shear stresses 15
short wavelength limit 77
shrink-fitting 50
275
276
tensor notation 20
Thomson equation 85
time of flight analysis 114
timer/scaler 104
top 15% rule 171
total diffracted intensity 109
total stress state in surface deformation 61
transformation of axes 20
transformation law (fourth rank tensors) 34
transformation law (second rank tensors) 22
transverse strains 25
triaxial stress analysis 125
true absorption 83
true elastic limit 44
true strain 40
true stress 41
twinning 44
two-tilt method 123
Undulators 81
unit cell 28
unstressed lattice spacing 126
Variance (in count rate) 182
vectors 15, 21
Vegard's law 157
vertical beam divergence 195
Voigt average 63, 70
von Laue 76
Subject Index
Warren-Averbach analysis of peak shape
238
white radiation 77
working origin 173
X-ray line broadening 230
x-ray peak shape 232
x-ray peak shape analysis 230
x-ray spectroscopy 89
x-ray strain equation 118
x-ray tubes 80
x-rays
absorption of 82
absorption coefficient of 82
Bremsstrahlung 77
characteristic radiation of 77
Compton scattering of 85
filters 84
generation of 80
inelastic scattering of 77
minimum wavelength 77
monochromator for 90
scattering factor of 86
structure factor for 87
white radiation 77
Yield strength 45
yielding (x-ray determination of) 159
Young's moduli (for selected materials) 27
Young's modulus, anisotropic materials 36