Stress and Texture

Strain
Two types of stresses:

microstresses vary from one

grain to another on a microscopic
scale.
macrostresses stress is uniform
over large distances.

Usually:

macrostrain is uniform
produces peak shift
microstrain is nonuniform
produces peak broadening

b 2 2

d
tan
d

Applied and Residual Stress

Plastic flow can also set up residual stress.

Loaded below elastic limit

Loaded beyond elastic limit

Unloaded
Shaded areas show regions plastically strained

Methods to Measure Residual Stress

X-ray diffraction.

Nondestructive for the measurements near the surface: t < 2 m.

Neutron diffraction.

Can be used to make measurements deeper in the material, but the

minimum volume that can be examined is quite large (several mm3) due
to the low intensity of most neutron beams.

Dissection (mechanical relaxation).

Destructive.

General Principles
Consider a rod of a cross-sectional area A
stressed in tension by a force F.
Stress:

F
, x , z 0
A

x-rays

Stress y produces strain ey:

L L f L0
ey

L
L0
L0 and Lf are the original and final lengths of the bar.
The strain is related to stress as:

y Ee y
L increases D decreases so:

D D f D0
ex ez

D
D0

e x e z e y

for isotropic
material

Poissons ratio
usually 0.25 < < 0.45

General Principles
This provides measurement of the
strain in the z direction since:

ez

dn d0
d0

Then the required stress will be:

E d n d0

d0

Diffraction techniques do not measure stresses

in materials directly
Changes in d-spacing are measured to give strain
Changes in line width are measured to give
microstrain
The lattice planes of the individual grains in the
material act as strain gauges

General Principles

E d n d0

y
d0

we do not know d0 !

Elasticity
In general there are stress components in two or three directions at right
angles to one another, forming biaxial or triaxial stress systems.

Stresses in a material can be related to the set of three principal stresses 1,

2 and 3.

To properly describe the results of a diffraction stress measurement we

introduce a coordinate systems for the instrument and the sample. These
two coordinate systems are related by two rotation angles and f.
Li laboratory coordinate system
Si sample coordinate system

By convention the
diffracting planes are
normal to L3

Elasticity
In an anisotropic elastic material stress tensor ij is related to the strain
tensor ekl as:

ij Cijkl e kl
where Cijkl is elastic constants matrix.
Similarly:

e ij Sijkl kl

where Sijkl is elastic compliance matrix.

For isotropic compound:

e ij

ij ij kk
E
E

where ij is Kroeneckers delta, kk indicates the summation 11 + 22 + 33

Elasticity
Or we can write it as:

1
11 22 33 ,
E
1
e 22 22 11 33 ,
E
1
e 33 33 11 22 ,
E
1
e 23
23 ,
2
1
e 31
31,
2
1
e 12
12
2

e 11

where

21
shear modulus

Elasticity
Lets relate emn in one coordinate system to that in another system
through transformation matrix:
L
e mn
M miSL M njSLe ijS

The transformation matrix is:

M SL

so that we find

cos f cos
sin f cos
sin

L
33 f

sin f
cos f
0

cos f sin
sin f sin
cos

M 3SLi M 3SLje ijS

e 11S cos 2 f sin 2 e 12S sin 2f sin 2
e 22S sin 2 f sin 2 e 33S cos 2
e 13S cos f sin 2 e 23S sin f sin 2

Elasticity
In terms of stresses:

L
33 f

1 S
1 S
11 cos 2 f 12S sin 2f 22S sin 2 f 33S sin 2
33
E
E

1 S
11S 22S 33S
13 cos f 23S sin f sin 2
E
E
d d0
f
d0

Biaxial and Triaxial Stress Analysis

Biaxial stress tensor is in the form:

11 0 0
0

0
22

0
0 0
since stress normal to a free surface must be zero:

ij n j 0

For our tensor lets define:

fS 11S cos 2 f 22S sin 2 f

Then the equation for strain becomes:

ef
L

df d 0
d0

1 S

f sin 2 11S 22S

E
E

The sin2 Method

Stress 33 is zero, but strain e33 is not zero. It has finite value given by the
Poisson contractions due to 11 and 22:

e e e
S
33

S
11

S
22

S
11

22S

Then strain equation can be written as:

e f e
L

S
33

L
e f
e 33S

1 fS
E

df d 0
d0
df d n
d0

sin 2

dn d0
d0

1 fS
E

sin 2

The sin2 Method

We make ingenious approximation (by Glocker et al. in 1936):

dn, di and d0 are very nearly equal to one another,

(di dn) is small compared to d0,
unknown d0 is replaced by di or dn with negligible error.

df d n
dn

1 f

E
1 sin 2

sin 2

df d n

dn

The stress in a surface can be determined by measuring the d-spacing as a function

of the angle between the surface normal and the diffracting plane normal
Measurements are made in the back-reflection regime (2 180) to obtain
maximum accuracy

The sin2 Method

df d n
dn

1 f
E

sin 2

The sin2 Method

Lets assume that stresses in zx plane are equal. This is referred to as
an equal-biaxial stress state. We can write sample frame stress as:

0
0

0 0

0
0
0

No stress dependence on f

d d n
dn

1 sin 2
E

>0
<0
sin2
Biaxial or uniaxial stress

sin2

sin2

Triaxial stresses present

Texture present

The sin2 Method

d
E

2
sin
dn
n

Slope of the plot is:

d
sin 2

d
E

Generally and E are well-known

constants

Diffractometer Method

D sin

R sin

Diffractometer Method
The effect of sample or -axis displacement can be minimized if a
parallel beam geometry is used instead of focused beam geometry.

Measurement of Line Position

Sample must remain on the diffractometer axis as is changed (even if the
sample is large)
Radial motion of the detector to achieve focussing must not change the
measured 2
L-P factor may vary significantly
1 cos 2 2
LPA
across a (broad) peak
sin 2 1 tan cot

Absorption will vary when 0

Measurement of peak position
often requires fitting the peak
with a parabola:

2
2 0 21
2
a I 2 I1

3a b

b I 2 I3
2 2 2 21 2 3 2 2

Measurements of Stress in Thin Films

Thin films are usually textured. No difficulty with moderate degree
of preferred orientation.
Sharp texture has the following effects:
Diffraction line strong at = 0 and absent at = 45o.
If material anisotropic E will depend on direction in the specimen.
Oscillations of d vs sin2.

Measurements of Stress in Thin Films

In thin films we have a biaxial stress, so:

df d n
dn

1 f
E

sin 2

If we have equal-biaxial stress then it is even simpler:

a an
an

n
1 sin 2
d hkl d hkl

n
d hkl
E

We can calculate for any unit cell and any orientation. For cubic:

a cos

h 2 k 2 l 2

h h k k ll
k2 l2

Symbols h, k and l define (hkl) - oriented film

Texture Analysis
The determination of the lattice preferred orientation of the crystallites
in a polycrystalline aggregate is referred to as texture analysis.
The term texture is used as a broad synonym for preferred
crystallographic orientation in a polycrystalline material, normally a
single phase.
The preferred orientation is usually described in terms of pole figures.

{100} poles of a
cubic crystal

The Pole Figures

Let us consider the plane (h k l) in
a given crystallite in a sample. The
direction of the plane normal is
projected onto the sphere around
the crystallite.
The point where the plane normal
intersects the sphere is defined by
two angles: pole distance a and an
azimuth b.
The azimuth angle is measured
counter clock wise from the point
X.

The Pole Figures

Let us now assume that we project the plane normals for the plane (h k l)
from all the crystallites irradiated in the sample onto the sphere.
Each plane normal intercepting the sphere represents a point on the
sphere. These points in return represent the Poles for the planes (h k l) in
the crystallites. The number of points per unit area of the sphere
represents the pole density.

Random orientation

Preferred orientation

The Pole Figures

The Stereographic Projection

(a)
(b)

As we look down to the earth

The stereographic projection

The Stereographic Projection

The Pole Figures

The Pole Figures

The Pole Figures

We now project the sphere with its pole density onto a plane. This
projection is called a pole figure.

A pole figure is scanned by measuring the diffraction intensity of a given

reflection with constant 2 at a large number of different angular orientations
of a sample.
A contour map of the intensity is then plotted as a function of the angular
orientation of the specimen.
The intensity of a given reflection is proportional to the number of hkl planes
in reflecting condition.
Hence, the pole figure gives the probability of finding a given (h k l) plane
normal as a function of the specimen orientation.
If the crystallites in the sample have random orientation the contour map will
have uniform intensity contours.

The Pole Figures

out-of-plane
direction

Rotation Axis f
(1 0 0)

Rotation
Axis
(1-11)

(-1 -1 1)

{1 1 1}
(1 0 0)

(1 -1 1)

(1 1 1)

The Pole Figures

Rotation Axis f

(1 0 0)

out-of-plane
direction

Rotation
Axis

{1 0 0}
(1 1 1)
(1 1 1)

(0 0 1)

(0 1 0)

Schulz Reflection Method

This method requires special sample holder which allows rotation of
the specimen in its own plane about an axis normal to its surface, f,
and about a horizontal axis, c.

Reflection

Transmission

Schulz Reflection Method

In the Bragg-Brentano geometry a divergent x-ray beam is focused on
the detector.
This no longer applies when the sample is tilted about c.

Advantage: rotation in around

c in the range 40o < c < 90o
does not require absorption
correction.

Field and Merchant Reflection Method

The method is designed for a parallel incident beam.

Field and Merchant Reflection Method

Diffracted intensities must be corrected for change in absorption due to change
in a.

dI D

I 0 ab x 1 sin 1 sin b
e
dx
sin

a volume fraction of a specimen containing particles having

correct orientation for reflection of the incident beam.
b fraction of the incident energy which is diffracted by unit
volume

substitute

90o a , b a 90o
Integrate 0 < x <

ID

I 0 ab
1 cosa cosa

We interested in the intensity at angle a, relative to intensity at a = 90o:

I D a a
1 cot a cot
o
I D a 90

Pole Figure Measurement

Pole figure diffractometer consists of a four-axis single-crystal
diffractometer.
Rotation axes:
, w, c, and f

Example: Rolled Copper

Texture measurements were performed on Cu disk = 22 mm, t = 0.8 mm.

Four pole figures (111), (200), (220) and (311) were collected using Schulz reflection method.
Background intensities were measured next to diffraction peaks with offset 2 = 4o.
Defocusing effects were corrected using two methods:
measured texture free sample
calculated (FWHM of the peaks at = 0o is required obtained from -2 scan.
XPert Texture program was used for quantitative analysis.

Example: Rolled Copper

Measure -2 scan in order to determine the reflections used for the pole figure measurements.
Use FWHM of the peaks to calculate the defocusing curve.

Example: Rolled Copper

Pole Figure Measurements

Four pole figures have been measured.

Symmetry of rolling process is obtained
from the pole figures:
pole figure is symmetrical around
f = 0o and f = 90o.
The symmetry is called orthorhombic
sample symmetry.

Example: Rolled Copper

Background Correction
Pole figure intensities include background.
Correction for background radiation is performed by
measuring the intensity vs. -tilt next to the diffraction
peak.

Example: Rolled Copper

Defocusing Correction

Sample stage and /or sample is above or

below the diffraction plane: peaks are
displaced from original position.
Intensity can be corrected:
experimentally using a texture-free
sample
theoretically calculating geometrical
defocusing corrections

Example: Rolled Copper

Corrections
Experimental pole figures are corrected for background intensities.
Either experimental or theoretical defocusing correction curve is applied.

Measured and calculated defocusing corrections for Cu(220) pole figure

Example: Rolled Copper

Corrections
(a)

2D representation of Cu(220) pole figure as (a) measured and (b) corrected.

The most noticeable effect is at higher -tilt angles.

(b)

Example: Rolled Copper

Orientation Distribution Function Calculation
XPert Texture calculates ODF
When ODF is available XPert Texture can
calculate pole figures and inverse pole figures
for any set of (hkl).

Measured

Calculated

TaN Thin Film

TaN (001)

MgO (001)

200 TaN

104

6000

200 MgO

105

FWHM=0.72 deg

5000

Intensity (cps)

Intensity (cps)

4000

103

3000

2000

1000

102

101
41

42

43

2 (deg)

44

-1.0

-0.5

0.0

w (deg)

0.5

1.0

TaN Thin Film

f-scan of TaN (202) and MgO (202) reflections.

Intensity (cps)

TaN 220

MgO 220

50

100

150

200

f (deg)

250

300

350

TaN Thin Film

TEM reveals additional structure.

TaN Thin Film

XRD 002 pole
figure of TaN
film

TaN Thin Film

54

TaN Thin Film

Atomic Force Microscopy images of TaN films prepared under
different N2 partial pressure

pN=2 mTorr

pN=2.5 mTorr

pN=4 mTorr