Max-Planck-Institut für Eisenforschung GmbH

Investigation of the texture and microstructure evolution around

a nanoindent close to an individual grain boundary.
David Mercier1 (d.mercier@mpie.de),
C. Zambaldi1, P. Eisenlohr2
M. A. Crimp2, T. R. Bieler2
1
Max-Planck-Institut für Eisenforschung, 40237 Düsseldorf, Germany
2
Michigan State University, East Lansing, MI 48824, USA

17th International Conference on Textures of Materials

August 24-29, 2014 | Dresden, Germany

Gr. A

Gr. B
Motivation of this work
Plasticity of Single Crystal is well understood.
 Indentation experiments are often used to characterize
plasticity of single crystal…

Inverse pole figure of pile-up topographies of cp-Ti 1

Misorientation maps underneath the indentation at different
1. Zambaldi C. “Orientation informed nanoindentation of a- cross sections, comparison between experimental and
titanium: Indentation pileup in hexagonal metals simulation results2
deforming by prismatic slip.”, J. Mater. Res., 2012,
27(1), pp. 356-367.
2. Zaafarani N. “On the origin of deformation-induced But, missing element to predict
rotation patterns below nanoindents.”, Acta Mater.,
2008, 56, pp. 31-42. polycrystal mechanics…
2014-08-25 MERCIER David 2
Motivation of this work (2/2)

Micromechanical behavior of grain boundaries.

 EBSD and indentations close to grain boundaries
are performed in alpha-Ti  quasi bi-crystal deformation.

Gr. A
Comparison of experimental
results (residual topography,
texture around indent…) to
simulated indentations as
predicted by
3D CPFE modeling.

Gr. B

Start to model the slip AFM topography of residual indent in

transmission and GB Ti-5Al-2.5Sn, close to a grain boundary.
mechanic…
2014-08-25 MERCIER David 3
Strategy  Creation of a toolbox

GB and
Bicrystal Crystal
definition Plasticity

Slip
transmission
model

MATLAB Toolbox and

Graphical User Interfaces (GUIs)
2014-08-25 MERCIER David 4
Bicrystal definition  5 DOF

Trace of the grain

boundary (GB)
Geometrical description1,2
1. GB inclination (b) (by serial
a polishing or by FIB) and GB
trace (a) (by EBSD )
b nGB Or
GB normal (nGB)
Crystal 1 GB
2. Step between grains after
( 𝛗𝟏 𝛟 𝛗𝟐 )𝟏 Crystal 2 polishing / Rougness (by AFM)

( 𝛗𝟏 𝛟 𝛗𝟐 )𝟐
[ 𝒖𝒗𝒘 ] / 𝝎 Crystallographic description3

1. Randle V. “Five-parameter’ analysis of grain boundary networks

1. Euler angles of grains
by electron backscatter diffraction.”, J. Microscopy, 2005, 222,
pp. 69-75.
(12 3) (by EBSD)
2. Randle V. “A methodology for grain boundary plane assessment Or
by single-section trace analysis.”, Scripta Mater., 2001, 44, pp.
2789-2794
2. Misorientation axis / angle
3. Morawiec A., “Orientations and Rotations: Computations in
Crystallographic Textures.”, Springer, 2004. [uvw] / w (by EBSD or TEM)

2014-08-25 MERCIER David 5

Crystal Plasticity of alpha-Titanium (hcp)

 Slip systems

Basal <a> Prism. 1st ord. <a> Prism. 2nd ord. <a> Pyr. 1st ord. <a> Pyr. 1st ord. <c+a> Pyr. 2nd ord. <c+a>
{} <> {} < > {} <> {} < > {} <> {} <>

 Twin systems

Large number of
dislocation slip and
twinning systems.

Tensile twinning Tensile twinning Compr. twinning Compr. twinning

{} < > {} < > {} < > {} < >

2014-08-25 MERCIER David 6

Criteria to predict the slip transmission

N factor (from Livingston & Chalmers)1

N  nin  nout * d in  d out   nin  d out * nout  d in 

1. Livingston J.D . & Chalmers B., “Multiple slip in

m’ factor (from Luster & Morris) 2 bicrystal deformation”, Acta Met. 1957,5, pp.
322-327.

m'  cos  cos  2. Luster J. & Morris M.A., “Compatibility of

deformation in two-phase Ti-Al alloys:
Dependence on microstructure and orientation
relationships.”, Metallurgical and Materials
Transactions A, 1995, 26(7), pp. 1745-1756.

Outgoing slip Incoming slip

Residual Burgers vector3

3. Marcinkowski M. J. & Tseng W. F., “Dislocation
behavior at tilt boundaries of infinite extent.”,

b r  b in  b out
Metallurgical Transactions, 1970, 1(12), pp.
3397-3401.

Outgoing slip Incoming slip

4. Bieler T. R. et al., “The role of heterogeneous
deformation on damage nucleation at grain

Schmid Factor, resolved shear stress…4 boundaries in single phase metals.”, International
Journal of Plasticity, 2009, 25(9), pp. 1655-1683.

2014-08-25 MERCIER David 7

Strain Transfer parameters implemented in the toolbox

2014-08-25 MERCIER David 8

 Outline
Acquisition of EBSD map of the sample

Selection of interesting GB
Experiments

using the MATLAB Toolbox/GUI

EBSD map
Spherical indentation close to the chosen GBs

Measurement of the topography

by AFM and of the lattice rotation by EBSD AFM topography of a
residual indent

Inclination of GB measured by FIB or serial polishing

1st slip transmission analysis via

the MATLAB Toolbox/GUI
Modeling

Cross sectional view of GB

Creation of output files for CPFEM

using the MATLAB Toolbox/GUI

3D CPFE modeling

CPFEM displacement
 Slip transmission model using CPFEM results result after bicrystal
indentation
and the MATLAB Toolbox/GUI
2014-08-25 MERCIER David 9
EBSD onand
Loading Ti–5Al–2.5Sn (wt%)
Plot of EBSD sample
data

Outputs from OIM™ Data Analysis

• Grains number;
• Average orientation of each grains
 Euler angles (phi1, PHI, phi2);
• Phase of material;
• Average positions and diameters of grains;
• GB numbers;
• GB trace coordinates ;
• Trace length and trace angle.

 Loading of EBSD
Grain file type 2
EBSD orientation map with IPF coloring scheme
files. of Ti–5Al–2.5Sn (wt.%) sample. and
Reconstructed Boundaries file
TheSetting
sample ofexhibited
the a near- (HCP)
coordinate system.
microstructure with the body centered
cubic (BCC)  phase located primarily at
α phase
Plot grain
of the GBs 1.
boundaries
segments. MATLAB
 Mean grain diameter : (34 ± 16)µm
1. Seal J. R. et al., Mater. Sci. and Eng. A 552, 2012, pp. 61-68.
Toolbox/GUI
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Introduction to the MATLAB toolbox

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Selection
Indentation
of experiments
a specific grain boundary…

Gr. A

Gr. B
GB

Gr. B Gr. A

 Isolate a specific GB.

 Data transfer from EBSD map into a

new window in order to analyze in AFM topography of residual indent in Ti-5Al-2.5Sn, close to a grain
detail the given bicrystal… boundary with profiles of pile-up surrounding the indent.

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CPFE model generation from the GUI

 Possibility to tune the indenter geometry (tip radius,

apex
angle…), sample geometry (GB inclination, sample size…),
the mesh parameters (bias, number of elements…)…

 Generation of mesh procedure file and material config.

2014-08-25
file using Python scripts.
MERCIER David 13
Few details about CPFE model
Generation of a CPFE model with the MATLAB Toolbox/GUI

• Flow rule given by Kalidindi’s

constitutive model1,2,3
• Only Prismatic 1st order <a>,
Gr. B Basal <a> and Pyramidal 1st
order <c+a>

Gr. A

• The CPFE model used is purely local formulation, and includes only the
changes in slip system alignment across the boundary, but no
strengthening effect from grain boundaries.

• DAMASK  http://damask.mpie.de/
References
1. S.R. Kalidindi and L. Anand, “An approximate procedure for predicting the evolution of crystallographic texture in bulk deformtion processing of FFC metals.”, Int. J. Mech. Sci. 34(4)
(1992) pp. 309-329.
2. A.A. Salem et al., “Strain hardening due to deformation twinning in alpha-titanium: Constitutive relations and crystal-plasticity modeling.”, Acta Materialia 53(12) (2005) pp. 3495-3502.
3. X. Wu et al., “Prediction of crystallographic texture evolution and anisotropic stress-strain curves during large plastic strains in high purity alpha-titanium using a taylor-type crystal
plasticity model.”, Acta Materialia, 55(2) (2007) pp. 423-432J.
4. Zambaldi C. et al. “Orientation informed nanoindentation of α-titanium: Indentation pileup in hexagonal metals deforming by prismatic slip.”, J. of Mater. Res., 2012, 27(01), pp. 356-367

2014-08-25 MERCIER David 14

CPFEM results (1/3)

Gr. A

Gr. A

Gr. B
Gr. B
AFM topography of residual indent in Ti-5Al-2.5Sn,
close to a grain boundary.

Calculated topography from CPFEM of spherical

indent close to a GB.

•Small discrepancy between experimental and simulated pile-up

topographies indicate strain transfer is mainly controlled by
geometrical consideration.

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CPFEM results (2/3)

CPFEM
EBSD

Gr. B Gr. A Gr. A

Gr. B
Local Misorientation from EBSD measurement vs CPFEM results.

•The CPFE model with no strengthening effect from grain boundaries

seems to predict almost correctly the plasticity transfer.

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CPFEM results (3/3)
Accumulated
prism. 1<a>
shear

r.A
G

Accumulated
.B
basal shear Gr
Isosurfaces of accumulated shear int the bicrystal
obtained by CPFEM.

Slip transfer is based on the

geometrical compatibility of the two
grains (high m’ value for prism. 1 <a>
and basal, low RBV, high LRB…).

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Advantages of the GUI
•Analysis of all GBs in a map (and color coded results), then
selection of interesting ones

•Fast transfer of experimental data into simulation input files :

 SX indentation
 BX indentation

•Reduction of possible sources of error in analysis by visualization,

standardized workflow and automated data I/O

•Readily extendible to other experiments :

 Polycrystal tensile test
 µ-cantilever bending test
 µ-pillar compression test
 Straining test and TEM Cu bi-crystal Straining test and TEM3.

1. Zhao Z. et al., “Investigation of three-dimensional

aspects of grain-scale plastic surface deformation of
an aluminum oligocrystal.”, International Journal of
Plasticity 24, 2008, pp. 2278-2297.

2. Dehm G. et al., “Plasticity and Fracture at Small

Tensile test of Aluminum
3.
oligocrystal “dogbone”1.
µ-pillar compression test and
µ-cantilever bending test 2.
2014-08-25 MERCIER David
Length Scales: from Single Crystals towards
Interfaces.”, Workshop on Mechanical Behaviour of
Systems – 4, 2013 (India).
Shen Z. et al., “Dislocation and grain boundary
interactions in metal.”, Acta Metal., 1988, 36(12), pp.
3231-3242.
18
Results from in situ straining test in TEM (Kacher et al. 2012)
 “In situ and tomographic analysis of dislocation/grain boundary interactions in a-
titanium.”, Phil. Mag., 2014, pp. 1-16.

Good agreement in term of residual Burgers vector

calculated with the MATLAB Toolbox and values given in
Kacher’s paper.

2014-08-25 MERCIER David 19

Results from polycrystal tensile test (Patriarca et al. 2014)
 “Slip transmission in bcc FeCr polycrystal.”, Materials Science and
Engineering: A, 2014, 588, pp. 308-317.

Good agreement in term of

residual Burgers vector
calculated with the MATLAB
Toolbox and values given in
Patriarca’s paper.

2014-08-25 MERCIER David 20

Conclusion and Outlook
•MATLAB Toolbox / GUI = “Bridge between EBSD and CPFEM”
 For bcc, fcc and hcp materials and for 1 or 2 phase materials
 Slip trace analysis
 Many functions implemented to analyze and to quantify the potential
for slip transmission at GBs
 Interfaced with Python code to rapidly generate CPFE simulation
input files for indentation experiments
 Possibility to implement new functions and new CPFE models for
other experiments (µ-cantilever, µ-pillar, straining test…)
 http://github.com/czambaldi/stabix
 Proceedings paper on ICOTOM17 conference

• Preliminary results : CPFE model with no strengthening effect from grain

boundaries seems to predict almost correctly the plasticity transfer.

•More indentation and 3D EBSD experiments to do…

2014-08-25 MERCIER David 21

Acknowledgments and Questions

Dr. P. Eisenlohr, Dr. M. Crimp and

Y. Su are acknowledged.

Materials World Network grant references NSF: DFG: ZA523/3-1

Thanks for your attention….

Questions ?

d.mercier@mpie.de

2014-08-25 MERCIER David 22