Stress and Texture by XRD

Bob He, Bruker AXS

Conventional X-ray Diffractometer

Bragg-Brentano
Geometry.
Antiscatter
slit

Divergence slit

Monochromator

Scanning over 2 range

to collect XRD pattern.

Detectorslit 20000

Tube

Corundum Powder Diffraction

18000
16000
14000

Intensity

Sample

12000
10000
8000
6000
4000
2000
0

20

25

30

35

Two Theta

40

45

50

Diffraction Patterns vs. Atomic Arrangement

XRD2: Two-dimensional X-ray Diffraction

XRD2 : Innovation and Development

The most dramatic development in XRD2 happens
in detector and data evaluation algorithms:
Detector: collect 2D pattern with correct
intensity, position and angular coverage.

Data evaluation algorithm: data collection

strategy and data evaluation. (Diffraction Vector
Approach)

VNTEC-500 Outperform all previous

gaseous detectors.
High sensitivity: 80%
DQE for Cu
High spatial resolution:
FWHM of PSF is 200m
High maximum count
rate:
1.5Mcps global;
250kcps/reflection -local
Low background noise:
<5 cps/global
Maintenance-free:
no re-gassing

VNTEC-500 Outperforms all

previous gaseous detectors
Detector geometry:
Be-window opening 140 mm in dia.
Frame size:
2048 x 2048 pixels
1024 x 1024 pixels
512 x 512 pixels

Pixel size:

Detector working distance:

2 range in a single frame:

68 m x 68 m
136 m x 136 m
272 m x 272 m
5~30 cm in D8 DISCOVER enclosure
5
10
15
20
25
30

cm
cm
cm
cm
cm
cm

83
56
42
33
27
23

Stress/Texture/Microdiffraction
Horizontal th-2th, CEC

No barrier between 0D/1D/2D

Vertical theta-theta, CEC for microdiffraction/stress/texture

XRD2: Diffraction vector approach

Applications

Vector approaches

Phase Identification:

Polarization and absorption correction

Texture Analysis:

Orientation mapping angles;

Data collection strategy (scheme)

Stress Analysis:

Fundamental equation derived by

second order tensor transformation;
Data collection strategy (scheme)

Crystal Size Analysis:

Equations for the effective volume

calculation at both reflection and
transmission modes.

15.12.2011

Bruker Confidential

10

Single Crystals

S0

Laue equation

a ( s s0 ) h
b ( s s0 ) k
c ( s s0 ) l

XRD2: Debye cones from powders

Bragg law

n 2d sin

XRD2: Diffraction pattern with both g and 2 information

Debye Cone

Incident Beam
Sampl
e

Diffraction vector with g

cos 2 1
s s0 1
H

sin 2 sin g

sin 2 cos g
15.12.2011

Bruker Confidential

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XRD2:

Sample Space & Eulerian Geometry

The angular relationships

between XLYLZL and
S1S2S3 are:
XL

YL

ZL

S1

a11

a12

a13

S2

a21

a22

a23

S3

a31

a32

a33

The transformation matrix sin sin sin

from the diffraction space cos cos
a a a
to the sample
a a a sin sin cos

space is:
cos sin
a
a
a

11

12

13

21

22

23

31

32

33

sin cos

cos sin sin

sin cos
cos sin cos
sin sin
cos cos

cos sin

cos cos

sin

XRD2:

Sample Space & Unit Diffraction Vector

The components of the unit

vector hS in the sample
coordinates S1S2S3 is then
given by
h1 a11 a12 a13 hx
h a a a h
2 21 22 23 y
h3 a31 a32 a33 hz Or in expanded form:
In which each
h1 sin (sin sin sin cos cos ) cos cos g sin cos
component is a
cos sin g (sin sin cos cos sin )
h2 sin (cos sin sin sin cos ) cos cos g cos cos
function of
sample orientation
cos sin g (cos sin cos sin sin )
and g.
h sin cos sin cos sin g cos cos cos cosg sin
3

XRD:

Sample Space & Unit Diffraction Vector

The components of the unit vector

hS in the sample coordinates S1S2S3
is then given by

h1 cos sin

h2 sin sin

h cos
3

which is a single value at each

sample orientation.

XRD & XRD2:

Fundamental Equations for Strain

As a second order tensor, the relationship between the measured

strains and the strain tensor is given by:
0D/1D:
2D:

h h

ij hi h j

(g , , , )

ij

Both equations are in the same form except the difference in hs

11 cos2 sin2 12 sin 2 sin2 22 sin 2 sin2

13 cos sin 2 23 sin sin 2 33 cos2
Introducing g=90 or 270 (diffractometer plane),
the above equation can be derived from the bottom equation

({ghkl,}, , ) h1211 2h1h212 h22 22 2h1h313 2h2h3 23 h32 33

The sin2 - Method for Stress

Measurements

The sin2 - Method for Stress

Measurements

The sin2 - Method for Stress

Measurements

Basic Types of - sin2 Functions

XRD2: Fundamental Equation for

Stress Measurement
Introducing the
elasticity constants:
E & or
the macroscopic
elastic constants:

&

1
2

S2 (1 ) / E

S1 / E

the fundamental
equation for stress measurement in XRD2:
S1 ( 11 22 33) 12 S2 ( 11h12 22h22 33h32
sin 0
2 12h1h2 2 13h1h3 2 23h2h3 ) ln

sin

XRD2: Diffraction Rings Distortion

Due to Stress

The simulated diffraction ring distortion in radar chart:

(a) equibiaxial stress with scan;
(b) uniaxial stress with scan for Fe (211) with Cr
radiation.

Comparison of the sin2 and 2D

method for stress measurement
Sin2 method measures one data point
at each sample orientation. Data points
follow the longitudinal line (constant ).
2D method measures many data points
at each sample orientation and not
limited to constant .

Comparison of the sin2 and 2D

method for stress measurement

62

38

33 26

23

With increasing data points, the new 2D method can measure stress
with higher accuracy than the conventional sin2 method for the
same amount of data collection
25

Bruker Confidential

15/12/2011

The D8 DISCOVER with DAVINCI

VNTEC-500 for stress measurement
Almen strip (spring
steel)
(211) & (200) rings
Ring distortion when
sample rotates with
and

XRD2:

Stress Measurement Example

A standard reference
sample (SN# B024) from Prof.
Chuanhai Jiang distributed at
the 15th CCRS, Chongqing,
China, October 11-18, 2009.
The reference value of 1098 MPa measured with Cr
radiation by the Sin2 method.
Co tube, 40kV/30mA, a
slightly focusing polycapillary
lens and 1 mm pinhole
collimator produces a beam
size 0.3 mm on the sample.
Total data collection time: 5
minutes for 32 frames (5s
each+rotation). 1 or 2 minutes
are sufficient too.

XRD2:

Stress Measurement Example

cracks?

XRD2:

Stress Measurement Example

Parameter
setting

Results
reporting:
11= -1068
18 MPa
22= -1085
18 MPa

Evaluate
the data
quality

Principal
stress and
stress
ellipse
equibiaxial

Stress Measurement Using GADDS: A spring loaded

on the XYZ stage of GADDS Micro-diffractometer
A spring
mounted on the
XYZ stage.
Size:
coil diameter10mm wire
diameter-1mm
coil pitch-4mm
The inside
surface is
aligned to the
goniometer
center.
Both the
incident and
diffracted beams
can pass
through the gap
Residual Stress:
-864 (48) MPa

D8 DISCOVER with GADDS:

FSW Specimen Loaded on -Circle Cradle
Specimen is loaded on the

XYZ stage of the Eulerian

cradle

Each mapping spot is

aligned to the instrument

center with the laser/video
alignment system.

Stress data is collected with

and scans.

Cr-K radiation
Beam size: 0.8 mm
Aluminium (311) planes
Five frames, each 30

seconds, for each point.

D8 DISCOVER with GADDS:

Residual Stress Mapping on FSW:

22

Longitudinal Normal Stress

150

Residual Stress (MPa)

100
50

113
195

113
195

-50
-100
-150
-40

-30

-20

-10

10

20

30

Distance from Weld Center Line (m m )

Residual stress (22) distribution on top surface

40

XRD2:Diffraction Pattern Across FSW

Original material

Boundary

FSW weldment

XRD2:

Innovations to 2D method:
Stress Measurement from Multiple (hkl) Rings
Regression
Cu Film Stress vs. Loading
800

60
58

750
56
700

52

(331)

650
600
550

50

(331) only stress

48

(420) only stress

46

Linear

44

(331)+(420)
Std.err
(331) only std.err

500
450

Improve the accuracy and

reduce the effect of
anisotropy and texture

(331)+(420) Stress

(420) only std.err

400

42
40
38
36
34

350
32
300

30
0

3
4
5
Loading Strain (X 0.001)

Standard error (MPa)

Stress (MPa)

(420)

54

XRD2:

Innovations to 2D method:
Intensity Weighted Least Squares Regression

low intensity and poor

profile due to texture and
large grain tends to give
larger 2 shift error.
Ref: B. He, Two-dimensional X-ray Diffraction,
John Wiley & Sons, 2009, pp 299-303.

i 1

i 1

S wi ri2 wi ( yi y i )2

wi

Ii

i2

maximum (or integrated) intensity

the standard error of profile fitting
of the ith data point

XRD2:

Innovations to 2D method:
Pixel Direct Diffraction (PDD) Analysis

PDD analysis is based on diffraction vectors associated with each pixel in

diffraction frames collected with area detectors.
Conventionally, a 2D frame is treated as a continuous distribution of diffraction
intensity, and 2D diffraction patterns are integrated to diffraction profiles as
intensity distributions versus 2 or g angles.
In the DPP method, the diffraction meaning of each pixel is analyzed as an
independent event and the final diffraction results are generated by a collective
consideration of all pixel diffractions. (Each pixel is a point detector.)
The final crystallographic results are based on the statistical analysis of all pixels.
PDD results in a more accurate diffraction analysis with less human interference.
. stress analysis, the larger 2
For

shift error due to texture and

large grain can be eliminated.
No profile analysis is required.
Ref: B. He, Two-dimensional X-ray Diffraction, John
Wiley & Sons, 2009, pp 402-406.

i 1

i 1

S I i ri2 I i ( yi y i )2

Ii is the pixel intensity used as weighting

factors, n is the number of total pixels in the
selected region for all 2D frames

Texture:

Crystal Orientation and Pole Figure

The direction of
poles is defined by
and b angles in a
spherical
coordinates.
The pole densities
at all directions
are mapped on the
equatorial plane by
Stereographic
Projection.

The 2D map is
called pole figure

Texture: XRD2 vs. XRD(0D/1D)

d

XRD

XRD2

XRD2:

Sample Space & Unit Diffraction Vector

The components of the unit

vector hS in the sample
coordinates S1S2S3 is then
given by
h1 a11 a12 a13 hx
h a a a h
2 21 22 23 y
h3 a31 a32 a33 hz Or in expanded form:
In which each
h1 sin (sin sin sin cos cos ) cos cos g sin cos
component is a
cos sin g (sin sin cos cos sin )
h2 sin (cos sin sin sin cos ) cos cos g cos cos
function of
sample orientation
cos sin g (cos sin cos sin sin )
and g.
h sin cos sin cos sin g cos cos cos cosg sin
3

XRD2: Fundamental Equation for

Texture Analysis

The pole figure angles

(,b) can be calculated
from the unit vector
components by the pole
mapping equations:

sin h3 cos
1

b cos

h1
h12 h22

h h
2
1

2
2

b 0 if h2 0

b 0 if h2 0

The D8 DISCOVER with DAVINCI

VNTEC-500 for texture measurement
Steel can
(200) & (110) rings
Intensity variation during
scan

XRD2: Data Collection Strategy

(Scheme D=7cm)
2=40, =20, =35.26

2=40, =23, =30

The pole figure coverage can be simulated from the diffraction

2 angle, detector swing angle, detector distance, goniometer
angles, and scanning steps.

XRD2: Data Collection Strategy (Scheme)

Data collection strategy for Cu thin films with two scans.

XRD2: Data Collection Speed vs. 2D or 0D

2D: 108 exposures (frames); 0D: 973 exposures (points)

multiple pole-figures;
single pole-figures
2D detector is 1~2 orders of magnitude faster than 0D detector.

Texture Measurement Using VANTEC-500:

Magnetron sputter-deposited Cu films

Cu (311)

(220)

(200) (111)

3m Cu film on Si
substrate.

Four diffraction rings

are observed at 10 cm
detector distance.
Four pole figures can
be measured
simultaneously.

Si (311)

Diffraction spots from

Si wafer appear on
some frames.

Arts from XRD2: Pole-figure from Cu film and Si

Frames Collected from One Oriented Nylon

Sheet for Two Orientations
Machine
Direction
Phi-Axis

Sample provided by Prof. Brisson of University of Laval

Debye Rings from textured aluminum sheet

2D Data collected
in 1.5 s per frame
coverage from
2=-40 to 2
=+40
highly textured
Aluminum
good statistics
from fast
transmission
measurement

Percent Crystallinity with preferred orientation:

Stretching of a Rubber Band

unstretched
bright spots caused by
large grains of filler

stretched
200% elongation, 10 hours

Data Collection
Strategy with
Multex Area

Transparent
Texture
Evaluation

Texture:

g-TiAl alloys
(1): Comparison of 2D Patterns

Full, spotty Debye Ring visible

Partial, smooth Debye Ring visible

Large Grains

Fine Grains

Weak Texture

Sharp Texture

Note the strong Differences in the 2 dimensional Diffraction

Pattern

Texture:

g-TiAl alloys
(2): Comparison of Pole Figures
(110)

(111)

Fine Grains
Sharp Texture

Large Grains
Weak Texture

More About XRD2

1. Introduction.
2. Geometry Conventions.
3. X-Ray Source and Optics.
4. X-Ray Detectors.
5. Goniometer and Sample Stages.
6. Data Treatment.
7. Phase Identification.
8. Texture Analysis.
9. Stress Measurement.
10. Small-Angle X-Ray Scattering.
11. Combinatorial Screening.
12. Quantitative Analysis.
13. Innovation and Future Development.

December
15.
Copyright
Dezember
2011 Corporation. All rights reserved
8,Bruker
2010

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