Viscosidad de Escorias Articulos

Introduction to Crystallographic
Texture
Nilesh Prakash Gurao

Assistant Professor
Materials Science and Engineering
Indian Institute of Technology Kanpur, Kanpur India
Microstructure
 Structure at micron scale
 Distribution of phases in 3D
 Size, shape, orientation
Cheong et al. Acta Mater. 55 (2007) 1757
Herbig et al Acta Mater. 59 (2011) 590
D Raabe 2011
3/3/2016 HRXRED-2016 IIT Kanpur 2

Rolling of Nickel at IISc
Initial 10%
5%
25%
50%
35%
N. P. Gurao, S. Suwas, Materials Letters 2013

Twinning in stainless steel at USASK
5000
A
4000
Load (N)
3000
B B C D
2000
1000
C 0 A E
0 2 4 6 8 10
Displacement (mm)
200 µm
S. Sinha, J. A. Szpunar, NAP Kiran Kumar, N. P. Gurao, MSEA 2015

Twinning in titanium at IITK
Tension 500 N Tension 750 N Tension 1000 N
Compression Reload Tension Annealing 500 C

990 N 1000 N 1 hour
S. Sinha, N. P. Gurao, manuscript under preparation

Definition
 Texture is derived from “textor” in Latin
 The way things are woven
 Fabrics, rocks and materials
 Morphological texture
 Crystallographic texture
 Preferred orientation of crystallites

Morphological texture
Kanjeevaram Saree Rock

Crystallographic texture
Single orientation
Random orientation
Preferred orientation

Electron Back Scatter Diffraction

Utility
 Texture in polycrystalline materials is ubiquitous
 Goss oriented Silicon steel
 Earing of aluminum cans
 Substrate for semiconductor tapes
 Fatigue properties of aluminum and titanium alloys
 Quality of epitaxial films: YBa2Cu3O7-δ Pmmm space group c┴

epitaxy
 Recoverable strain in SMA

desirable cup showing earing
www.alumatter.org.uk
PMN-PT templated with SrTiO3
Seabaugh et al. J. Intel. Mater. Struct. 15 (2004) Gall et al. Acta Mater. 47 (1999)
209. 1203.
Orientation and Texture
 Orientation is relative
 Need of reference frame
 Orientation is relationship between the object under

consideration and the reference
 For materials
• Sample constitutes the reference frame
• Crystal constitutes the object
 Texture is relationship between sample and crystal frame

of reference

Representing texture
 Texture Relative orientation
 Crystal and Sample frame of reference
 Both must be orthogonal
 Ortho-normalization of unit cell if α or β or γ ≠ 90◦

 Science of texture evolved for rolling
 Three important directions
 Rolling Direction (RD), Transverse Direction (TD), Normal

Direction (ND)
 Crystal directions [100], [010] and [001]
ND
001
RD
TD 010
100

Description of orientation
 {hkl}<uvw>
 Euler Angles
 Axis angle pair Rodrigues-Frank vector
 Quaternions

Texture description
 Simplest description of texture
 Relationship between crystallographic planes and

direction and sample planes and direction
 (hkl) ┴ ND and <uvw> ║ RD
 For HCP, plane normal and corresponding direction are

not necessarily parallel
 Ortho-normalization ensures that complete orientation is

described without any ambiguity

Texture description: Mathematical
Cc = g Cs
g orientation matrix

Euler angles
ND
R
TD D 001
100
010
 Rotate φ1 about ND so that RD is

perpendicular to plane containing ND and [001]
RD RD’ and TD TD’
 Rotate Φ about RD’ so that ND and [001] coincide
ND [001] and TD’ TD’’
 Rotate φ2 about ND so that crystal and sample frame coincide
RD’ [010] and TD’’ [100]

Additional parameters
 Axis-angle pair (Rodrigues-Frank vector)

A unique axis can be found out about which if rotated by a
unique angle, the sample and crystal frame of reference
coincide
θ 
R = tan   ⋅ r
2
 Quaternions
Mathematically elegant description of encoding axis-angle
information
Rotation of θ about [uvw] axis is represented as
  
1
θ ( ui + vj + wk ) 1    1
q( q0 , q1 , q2 , q3 ) = e 2
= cos θ + (ui + vj + wk ) sin θ
2 2

Representing texture
 Pole Figure: distribution of crystallographic direction/plane

w.r.t. sample frame of reference
 Orientation Distribution function: distribution of

orientation in terms of Euler angles
 Inverse Pole figure: distribution of sample direction w.r.t.

crystal frame of reference

Pole figures

Stereographic projection
ND
RD 001
TD 010
100

Cube {100}<001> orientation
1 01

{100}<001> in different pole figures
ND
RD 100
TD 001
010
100 pole figure 101 pole figure 111 pole figure
1 01 1 01 1 01

Type of projection
Angle true
Area true

Random texture

For a polycrystal
 Single orientation Multiple spots
 Deviation from exact orientation Scatter

Contour levels
 Density of poles
 Compared with that of random sample
 Smoothened contours
 Multiples of random distribution (mrd)

Inverse pole figure
FCC tension

 Easiest description of texture
 Most commonly used for processes where only one direction is

uniquely defined
 Uniaxial deformation , thin film deposition or solidification
 Multiple IPF needed to describe complicated textures like rolling.
ND IPF RD IPF TD IPF
FCC rolling
Euler angles and Orientation space
Roe Bunge Williams

φ ϕ2+π/2 α
θ Φ ρ
ψ ϕ1-π/2 β=ψ +tan-1(tanαcosρ)
Every (hkl)[uvw] orientation has a

unique
(φ1, Φ, φ2) location in Euler space

Volume of Orientation space
2π π 2π
VODF =
φ
∫ ∫
φ φ
∫ dφ sin φdφdφ
1 2
1 =0 =0 2 =0

Volume of Orientation space
Volume element
dV = dAdΦ 2 = sin Φ dΦ dΦ 1
dΦ 2
V = 8π2

Crystal and Sample
Symmetry
 Cubic 24 rotation matrices (432)

 Hexagonal 12 rotation matrices
(62)
g ′ = Oc gOs
 Tension/Compression (Axial
symmetry)
 Rolling (222)
Cubic-Orthotropic
a) b) c)
d) e) f)
111 pole figure of 90% rolled a) Ni b) Ni-10%Co c) Ni-20%Co d)

Ni-30%Co e) Ni-40% Co and f) Ni-60%Co
Cubic-axial
Initial
texture
Simulated
texture
Experimental
texture
Compression direction inverse pole figure of different FCC materials

a) b)
100 pole figure of FCC material showing a) 110 and b) 111 fibre

Reduced volume of orientation
space 8π 2 π2
Φ = 0-  For rolling V = =
π = 0-
Φ 24 * 4 12
2
φ1 = 0- 2π  Actually plotted volume V = π
2
2π 4
 For axial symmetry only one section
required as all φ2 sections are similar

Pole Figure to Orientation Distribution Function
 Pole figures 2D information
 Texture 3D Orientation Distribution Function (ODF)
An ODF describes the frequency of occurrence of

particular crystal orientations in an imaginary
three-dimensional orientation space defined by
Euler angles
 Developed for cubic crystals with orthotropic symmetry
Rolling
 Extended to all crystal structures and all processes

 Two methods to determine ODF
 Spherical Harmonics
 Discrete Methods
 Incomplete PF data is input
 Spherical Harmonics
 C co-efficient (co-efficient of spherical harmonic functions)
 Even and odd ODF
 Problems with truncation and ghost error

 Direct methods
 WIMV method (Williams-1968, Imhof-1977, Mathies and Vinel-1982)

 The Vector method (Ruer and Baro-1977; Vadon and Heizmann-1991)
 The component method (Helming and Eschner-1990)
 The ADC (Arbitrary Defined Cells) method (Pawlik-1986)

Experimental ODF

Texture quantification
 Maximum intensity in a pole figures/ ODF
strength of texture
 Texture index quantitative parameter to

compare similar texture 1
2
F = 2
8π 2
∑ [ f ( g )] ∆g
i
i
Normalized sum of squared density values

Δgi = ODF cell volume
 Applicable for similar texture

 Better quantitative estimate by plotting fibres and
volume fraction of texture components
 Fibres are obtained by plotting f(g) as a function of Euler

angle
 Volume fraction of a component {hkl}<uvw> is obtained

by determining fraction of orientations in the viscinity of
given orientation

Volume fraction of different texture
components in differently rolled
Copper
Beta fibre plot for Cu and Cu-Zn alloys

Evolution of texture during processing
Solidification only one direction important Fibre texture
Thin film deposition growth direction Fibre texture
Deformation two directions important {hkl}<uvw>

Complete Euler space required for complex deformation processes like
Equal Channel Angular Pressing, cross rolling
Recrystallization two direction important {hkl}<uvw>

Retain similar symmetry as corresponding deformation texture
Phase transformation two directions {hkl}<uvw>

Measuring texture
 Macro-texture Bulk sample
 Micro-texture Microstructure + Texture
 X-ray and neutron diffraction
 Electron diffraction
 Synchrotron can offer both

Diffraction and Texture
 X-ray diffraction is routinely used to study the crystalline

structure of materials
 Information about texture is embedded in this information
 Even optical microscopy shows some orientation dependent
contrast
 Additional diffraction techniques like neutron, synchrotron and
electron diffraction offer better statistics and spatial resolution
respectively

Polarized Light Micrograph
Nano-cellulose Magnesium

Micro-texture from Electron Back Scatter Diffraction
Misorientation Profile
50% rolled austenite sample
70
60
50
Misorientation [degrees]
40
30
20
10
0
0 10 20 30
Distance [microns]
Misorientation Angle
0.4
0.3
Number Fraction
0.2
0.1
0.0
10 20 30 40 50 60
Gurao and Suwas, unpublished work

Misorientation Angle [degrees]

Riot of colours in α+γ steels
Gurao and Suwas, unpublished work

X-ray Diffraction for bulk texture
Braggs Law
d d sinθ d sinθ
nλ = 2dsinθ
XRD Database
Name and formula
Reference code: 00-001-1260
PDF index name: Nickel
Empirical formula: Ni
Chemical formula: Ni
Crystallographic parameters
Crystal system: Cubic
Space group: Fm-3m
Space group number: 225
a (Å): 3.5175
Alpha (°): 90.0000
Measured density (g/cm^3): 8.90
Volume of cell (10^6 pm^3): 43.52
Z: 4.00
Status, subfiles and quality
Status: Marked as deleted by ICDD
Subfiles: Inorganic Quality: Blank (B)
References
Primary reference: Hanawalt et al., Anal. Chem ., 10, 475, (1938)
Optical data: Data on Chem . for Cer. Use, Natl. R es. Council Bull. 107
Unit cell: The Structure of Crystals, 1st Ed.

Powder diffraction
http://ww1.iucr.org/cww-top/crystal.index.html
XRD of bulk electrodeposited nano-Ni
Lattice parameter, phase diagrams

Texture, Strain (micro and residual)
Size, microstructure (twins and
dislocations)

Estimating Texture
I111
 Intensity ratio I 200
 XRD on different faces
 Extended concept for plotting inverse pole figure

sample powder
I111 I111
sample
vs powder
I 200 I 200

Diffraction in TEM

Diffraction in polycrystal in Bragg-Brentano geometry
Source
Detector

Diffraction in polycrystal in Schulz reflection geometry
Source β Detector
xy oscillation
Schulz reflection geometry
RD
TD

Pole figure measurement
 Fix Bragg-Brentano condition for one peak
 Parallel beam optics
 Polycapillary or Gobel mirror
 Sample oscillation to improve statistics
 Rotation about axis normal to plane of sample (β)
 Tilt along axis in the plane of the sample (α)

 Continuous and discrete scans

Limitation of Schulz method
 De-focusing error at higher tilt
 Incomplete pole figures α = 70-75◦
 Pole figures not measured at θ < 10◦

α path length of X-rays Irradiated volume
 Absorption is balanced for thicker sample
 Absorption correction for thinner samples

Corrections in pole figures
 Background correction
I corrected = I measured (α,β) - IBG(α)
 Defocusing correction
I corrected = (I measured (α, β) - IBG(α))/D(α)
 Normalization
Inormalised (α, β) = Icorrected (α, β) / R

Transmission method for pole figures
 Thin sample
 X-rays should penetrate through
 Good data at higher inclination
 No errors for higher α (>45)
 Use in combination with Schulz method to obtain

complete pole figures

State of the art
 High brightness source micro-focus tube, liquid

metal anode
 Excellent beam optics to ensure parallel beam with small

divergence and dimensions Gobel mirror, polycap
 Position Sensitive detector 2θ range fast PF

determination
 Area detector 2θ and α range very fast PF

determination
 Well suited for in-situ heating (and straining) studies

Synchrotron diffraction
 Brighter than X-rays
 Heterogeneity study (5µm width)
 In-situ studies phase transformation, recrystallization
 Excellent for weakly scattering materials like polymers and biological

materials

Neutron diffraction
 Only method to measure magnetic texture
 Thermal neutrons (λ = 1-2Å) with higher penetration ensure no

absorption and defocusing correction
 Complete pole figures
 Mono-chromator and Position Sensitive detector
 Pulsed neutron source provide better statistics
 Time of flight measurements

Other techniques
 Ultrasonic measurement
 Selected Area Diffraction
 Kossel Diffraction
 Electron Back Scatter Diffraction
 Transmission Electron Microscopy-Orientation Imaging

Microscopy

Summary
 Crystallographic texture plays an important role in
determining physical and mechanical properties of
materials
 X-ray diffraction offers a robust tool to study texture in a

variety of materials
 Schulz reflection geometry is widely used in laboratory X-

ray diffractometers to determine texture
 Data analysis and interpretation is very important to

understand texture
 Microstructure and Texture- Processing-Performance of

materials can be appreciated
References
 M. Humphreys and W. B. Heatherly, An introduction to texture in
materials, Monograph No. 5, The Institution of Metallurgist London 1979.
 H. J. Bunge, European Journal of Mineralogy, 9 (1997) 735.
 R. W. Cahn, Materials Science and Technology, 15 1991.
 U. F. Kocks, C. N. Tome amd H.-R Wenk, Texture and Anisotropy, Cambridge
University Press, 1998.
 H. J. Bunge, Texture Analysis in Materials Science-Mathematical
Methods, Buttersworth London 1982.
 V. Randle and O. Engler, Introduction to Texture Analysis
Macrotexture, Microtexture and Orientation Mapping, Gordon and Breach
Science Publishers, 2000.
 S. Suwas and N. P. Gurao, Crystallographic texture in Materials, Journal of
the Indian Institute of Science 88 (2008) 151.
 S. Suwas and R. K. Ray, Crystallographic Texture of Materials, book under
preparation

3/3/2016 Thank you
SCM-2014 IIT Kanpur 79

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Introduction to Crystallographic

Nilesh Prakash Gurao

Herbig et al Acta Mater. 59 (2011) 590

3/3/2016 HRXRED-2016 IIT Kanpur 2

N. P. Gurao, S. Suwas, Materials Letters 2013

3/3/2016 HRXRED-2016 IIT Kanpur 3

3/3/2016 HRXRED-2016 IIT Kanpur 4

Compression Reload Tension Annealing 500 C

3/3/2016 HRXRED-2016 IIT Kanpur 5

 Texture is derived from “textor” in Latin

 The way things are woven

 Fabrics, rocks and materials

 Preferred orientation of crystallites

3/3/2016 HRXRED-2016 IIT Kanpur 6

Kanjeevaram Saree Rock

3/3/2016 HRXRED-2016 IIT Kanpur 7

3/3/2016 HRXRED-2016 IIT Kanpur 8

3/3/2016 HRXRED-2016 IIT Kanpur 9

 Texture in polycrystalline materials is ubiquitous

 Goss oriented Silicon steel

 Earing of aluminum cans

 Substrate for semiconductor tapes

 Fatigue properties of aluminum and titanium alloys

 Quality of epitaxial films: YBa2Cu3O7-δ Pmmm space group c┴

 Recoverable strain in SMA

3/3/2016 HRXRED-2016 IIT Kanpur 10

PMN-PT templated with SrTiO3

 Need of reference frame

 Orientation is relationship between the object under

 Texture is relationship between sample and crystal frame

3/3/2016 HRXRED-2016 IIT Kanpur 12

 Texture Relative orientation

 Crystal and Sample frame of reference

 Both must be orthogonal

 Ortho-normalization of unit cell if α or β or γ ≠ 90◦

3/3/2016 HRXRED-2016 IIT Kanpur 13

 Three important directions

 Rolling Direction (RD), Transverse Direction (TD), Normal

 Crystal directions [100], [010] and [001]

3/3/2016 HRXRED-2016 IIT Kanpur 14

 Axis angle pair Rodrigues-Frank vector

3/3/2016 HRXRED-2016 IIT Kanpur 15

 Simplest description of texture

 Relationship between crystallographic planes and

 (hkl) ┴ ND and <uvw> ║ RD

 For HCP, plane normal and corresponding direction are

 Ortho-normalization ensures that complete orientation is

3/3/2016 HRXRED-2016 IIT Kanpur 16

3/3/2016 HRXRED-2016 IIT Kanpur 17

 Rotate φ1 about ND so that RD is

3/3/2016 HRXRED-2016 IIT Kanpur 18

 Axis-angle pair (Rodrigues-Frank vector)

3/3/2016 HRXRED-2016 IIT Kanpur 20

 Pole Figure: distribution of crystallographic direction/plane

 Orientation Distribution function: distribution of

 Inverse Pole figure: distribution of sample direction w.r.t.

3/3/2016 HRXRED-2016 IIT Kanpur 21

3/3/2016 HRXRED-2016 IIT Kanpur 22

3/3/2016 HRXRED-2016 IIT Kanpur 23

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100 pole figure 101 pole figure 111 pole figure

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