Stress measurement with two-dimensional X-ray diffraction

Bob B. He*
Bruker AXS, 5465 E. Cheryl Parkway, Madison, Wisconsin 5371 1, USA
ABSTRACT
Two-dimensional diffraction systems, when used for residual stress measurement, have many advantages over the
conventional one-dimensional diffraction systems in dealing with highly textured materials, large grain size, small
sample area, and weak diffraction. The stress measurement is based on the fundamental relationship between the stress
tensor and the diffraction cone distortion. The benefit of the 2D method is that all the data points on diffraction rings are

used to calculate stresses so as to get better measurement result with less data collection time. The present paper
introduces the recent development in the theory and applications of stress measurement using 2D detectors.
Keywords: Residual stress, stress measurement, x-ray diffraction, two-dimensional detector, area detector, texture.

1. INTRODUCTION
The two-dimensional x-ray diffraction (XRD2) system is defined as a diffraction system with the capability of acquiring
diffraction pattern in 2D space simultaneously and analyzing 2D diffraction data accordingly. A 2D diffraction pattern
contains far more information than a one-dimensional profile collected with the conventional diffractometer. In order to

exploit the advantages of the 2D detector, new approaches are necessary to configure the XRD2 system and to
understand and analyze 2D diffraction data' . In addition, the new theory should also be consistent with the conventional
theory so that the 2D data can also be used for conventional applications. Stress measurement using 2D detectors is a
very good example of the different approaches used in XRD2 system.

Two-dimensional x-ray diffraction (XRD2) systems can measure residual stress with high speed and high accuracy,
especially when dealing with highly textured materials, large grain size, small sample area, and weak diffraction2. This
feature, along with many advantages in phase analysis, texture and other functions, makes XRD2systems more desirable
to users in semiconductor, electronics and auto industries. There are many other approaches to using 2D detectors for
stress measurement . The method suggested by the present authors has the advantage of direct relationship between
diffraction cone distortion and stress tensor, and the 2D theory is consistent with the conventional method. This paper is
an introduction to the method. More details in theoretical and practical aspects can be found in other publications 2,6

2. XRD2 GEOMETRY CONVENTION

Figure 1(a) shows the diffraction cones in the laboratory coordinates system, XLYLZL. Analogous to the conventional 3circle and 4-circle goniometer, the direct x-ray beam propagates along the XL axis, ZL is up, and YL makes up a right
handed rectangular coordinate system. The axis XL is also the rotation axis of the cones. The apex angles of the cones

are determined by the 20 values given by the Bragg equation. The apex angels are twice the 28 values for forward
reflection (2e9o) and twice the values of l8OO2O for backward reflection (20>900). The 'y angle is the azimuthal angle
from the origin at the 6 o'clock direction (-ZL direction) with right handed rotation axis along the opposite direction of
incident beam (-XL direction). The 'y angle actually defines a half plane with the XL axis as the edge, it will be referred
to as y-plane thereafter. The conventional diffractometer plane consists of two y-planes with one 'y=900 plane in the
negative YL side and 7=2700 plane in the positive YL side. and 20 angles forms a spherical coordinate system which
covers all the directions from the origin of sample (goniometer center). The y-20 system is fixed in the laboratory
systems XLYLZL, which is independent of the sample orientation in the goniometer. Figure 1(b) shows the relationship
'y

bhe@bruker-axs.com,

001-6082763086, Fax:OOl-6082763015

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127

i, )

and translation axes XYZ. w is the base rotation, all other rotations and translations
among all rotation axes (w, x,
are on top of this rotation. The next rotation above co is the x rotation. and g have the same axis but different starting
positions and rotation directions, and = 9O-i. The next rotation above co and X(W) is rotation. The sample
translation coordinates XYZ are so defined that, when co = = 4 =0, the relationship to the laboratory axes becomes X=
-XL, Y= ZL, and Z= YL. The rotation axis is always on the Z-axis at any sample orientation.
ZL

XL

(a)

(b)

Figure 1 The geometric definition of diffraction cones and sample orientations in an XRD2 system

3. FUNDAMENTAL EQUATION
The fundamental equation for strain measurement using 2D detector is given [3] as

f2e2

+ f22e22 + f13s13 + f2323 + f33i33 _

f13=2AC,

(sin 0
ln sin 0

with:

J2=2AB,

f23=2BC,

f33=c2

a=sinGcosw+sinycos0sinw
b = cosycos0

A = acosbbcosi'sin+csinit'sin
B = asinq5 +bcosi'cosb csiniticosb

c = sin0sincosincos0cosa

C = bsinii+ccosi

Wheref/s are the strain coefficients determined by the sample orientation and diffraction vector direction for each data
point on the diffraction ring. And ln(sin 6 Isin 0) represents the diffraction cone distortion at a particular (y, 20) position.
Equation ( 1) is the fundamental equation for strain and stress measurement by diffraction using 2D detectors, which
gives a direct relation between the diffraction cone distortion and strain tensor. Since it is a linear equation, the least
squares method can be used to solve the strain or stress tensor with very high accuracy and low statistics error. For
isotropic materials, there are only two independent elastic constants, Young's modulus E and Poisson's ratio v or the
macroscopic elastic constants S2 = (1+ v) I E and S1 = v I E . Then we have

puG_h +
where

p11_-

+ 3G_13 + p22a22 + p23cr23 + po33 = ml(sin Go

J()[(l + v)f - v] == +S2f1 + S1

1(Y)(l + v)f1

sin 0

}S2f,1

if i =

if

(3)

Each diffraction frame corresponds to one set of sample orientation (co, y and ). The diffraction ring on each frame is
integrated and peak-fitted over a selected number of sections along the ring, so as to obtain a set of (y, 20) data points
representing the 20(y) function. The stress tensor can be determined by fitting the data points to equation (2) with the
least-squares method. For biaxial stress, the above equation becomes

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p11a11 + p1p12 + p2p22 + PhaPh =

where the coefficient Ph

ml

(4)

2d sin 6)

, Q 5 a pseudo hydrostatic stress component caused by the approximate d-spacing

d . For biaxial stress with shear, we have

p11a11 + p12a12 + p22a22 + p13a13 + p2323 + Phah ml

2d sin 9)

(5)

The anisotropy correction can also be included in the x-ray elastic constants 4-S2 (hkl) and S1 (hkl) to replace the
macroscopic elastic constants --S2 and S1 . The equations for calculating x-ray elastic constants are:
-- S2 (hkl) = - S2[1 + 3(0.2 ['(hkl)A] ;

IT(hkl) =

S1 (hkl) =

S1

S2[O.2

T(hkl)]ti\

5(A - 1)
3+2A

h2k2 + k212 + 12h2

(h2+k2+12)2

(6)

The factor of anisotropy (A<) is a measure for the elastic anisotropy of a material. Values of A for the most important
cubic materials can be found in the reference 6, additional values may be found from literature.

4. COMPARISON BETWEEN CONVENTIONAL METHOD AND 2D METHOD

The residual stresses on a hardened carbon steel roller were measured by the conventional method and the new 2D
method 2 The data points at 7=900 from 7 frames, a typical data set for -diffractometer, are used to calculate stress
with the conventional Sin2 i/i method. In order to compare the statistic error between different number of data points,
different number of data points (3, 5, 7 and 9) are used to calculate stress with the new 2D equation. The results from the
conventional method and the new 2D method are compared in Figure 2. The measured residual stress is compressive
and the stress values from different methods agree very well. With the data taken from the same measurement (7 frames),
the new 2D method gives lower statistical error and the error decreases with increasing number of data points from the
diffraction rin
-850

---1

;i

5 7 points

-800

-700

:Li

-600

-550

sin2i' 3pts 5pts 7pts 9pts

METHODS

(a)

(b)

Figure 2 Comparison of the conventional and 2D methods. (a) Data points taken from the diffraction ring;
(b) Measured stress and standard deviation for different methods and data points.

5. VIRTUAL OSCILLATION
In the case of materials with large grain size or microdiffraction with a small x-ray beam size, it is difficult to determine
the 20 position due to poor counting statistics. To solve this problem with conventional detectors, some kind of sample

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129

oscillations, either by translation or by rotation are necessary to bring more crystallites into diffraction condition. In
another words, the purpose of oscillations is to bring more crystallites into Bragg condition. For 2D detectors, when the
y-integration is used to generate the diffraction profile, it actually integrates the data collected in a range of various
diffraction vectors. The angle between two extreme diffraction vector is equivalent to an oscillation angle. We may call
this effect as "virtual oscillation". Fig. 3 shows the relation between the y-integration range, Ay and the virtual oscillation
angle, A'p. The 20 value of the y-integrated profile is an average over the Debye ring defined by the -y-range.

Figure 3 The relation between the y-range, L\y and the virtue oscillation angle
The virtual oscillation angle Aii can be calculated from the integration range &y and Bragg angle 0,

z\ ti = 2 arcsin[cos 8 sin(Ay I 2)]

(7)

For example, if we integrate from 7=800 to 1OO, Ay=20, 0 64, the virtual oscillation angle Aii = 8.7. In the
conventional oscillation, mechanical movement may results in some sample position error. Since there is no actual
physical movement of the sample stage during data collection, the virtual oscillation has no such a problem. When 2D
theory is used for stress measurement, the virtual oscillation effect is further enhanced due to the larger y range.

6. CONCLUSIONS
The 2D fundamental equation is the basis of stress measurement in an XRD2 system. Since the whole or a part of the
Debye ring can be used for stress analysis, a two-dimensional x-ray diffraction system can measure stress with high
sensitivity, high speed and high accuracy. The spotty, textured, or weak diffraction data, normally associated with large
grain sample or micro-area diffraction, can be treated by "virtual oscillation". . The conventional method and the 2D
method are consistent both in theory and experimental results.

REFERENCES
1.

B. B. He, Uwe Preckwinkel and Kingsley L. Smith, "Fundamentals of two-dimensional x-ray diffraction (XRD2)",

Advances in X-ray Analysis, Proceedings of the 48th Annual Denver X-ray Conference, Steamboat Springs,
Colorado, USA, 43, 1999.

2. B. B. He, Uwe Preckwinkel and Kingsley L. Smith, "Advantages of Using 2D Detectors for Residual Stress
Measurement", Advances in X-ray Analysis, Proceedings of the 47th Annual Denver X-ray Conference, Colorado
Springs, Colorado, USA, 42, 1998.
3.

Yasuo

Yoshioka and Shin'ich Ohya, "X-ray Analysis of Stress in a Localized Area by Use of Image Plate",

Proceedings ofICRS-4, Baltimore, USA, 1994

4. G. M. Borgonovi, "Determination of Residual Stress from Two-Dimensional Diffraction Pattern", Nondestructive
Methods for Material Property Determination, Plenum Publishing Corporation, 47, 1984.

5. T. Sasaki, et a!., "Influence of image processing conditions of debye scherrer ring images in x-ray stress
measurement using imaging plate", Advances in X-Ray Analysis, 40, 1996.

6. B. B. He, "Residual Stress Measurement with Two-dimensional Diffraction", in Proceedings of the 20thHeat
Treating Society Conference, St. Louis, Missouri, USA, October 9-12, 2000.

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