Benrabah, Imed-Eddine

Bonnet, Frédéric

Deschamps, Alexis

Paul Van Landeghem, Hugo

English

Paul van Landeghem, Hugo

Hal - Université Grenoble Alpes

Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures

Archive Ouverte en Sciences de l'Information et de la Communication

  
1Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Development of compositional-gradient metallic alloys for 
combinatorial investigation of microstructures
1 SIMAP, INP Grenoble, CNRS, St. Martin d’Hères Cedex, 2 Research, ArcelorMittal, Maizieres-les-Metz, 
France
Imed-Eddine BENRABAH * 1 , Hugo Paul VAN LANDEGHEM 1 , Alexis DESCHAMPS 1 , Frédéric BONNET 2
ALEMI conference 13th-14th June, 2019, Vancouver, Canada
  
2
Introduction - motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Understanding and modeling of the influence of composition on ferrite growth kinetics 
during γ to γ + α transformation.
   
C.R. Hutchinson, H.S. Zurob, Y.J.M. Brechet, Metall. Mater. Trans. A 37A (2006) 1711–1720.
  
3
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Understanding and modeling of the kinetics of ferrite growth in multicomponent systems 
(Fe-C-X-Y-Z).
- Solute Drag based models for ternary systems 
   
Model
Exp. Model
Exp.
Fe-C-SiFe-C-Mn
C Qiu, HS Zurob, CR Hutchinson - Acta Materialia, 2015
  
4
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Understanding and modeling of the kinetics of ferrite growth in multicomponent systems 
(Fe-C-X-Y-Z).
- Solute Drag based models for Higher order systems 
   
Fe-C-Mn-SiFe-C-Mn-Mo
C Qiu, HS Zurob, CR Hutchinson - Acta Materialia, 2015WW Sun, HS Zurob, CR Hutchinson - Acta Materialia, 2017
775°C
Model
Exp.
Model
  
5
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Understanding and modeling of the kinetics of ferrite growth in multicomponent systems 
(Fe-C-X-Y-Z).
- Solute segregation at the migrating interface (coupled or anti-coupled solute drag effect)
  
6
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Understanding and modeling of the kinetics of ferrite growth in multicomponent systems 
(Fe-C-X-Y-Z).
- Solute segregation at the migrating interface (coupled or anti-coupled solute drag effect)
- Interaction between substitutional and interstitial atoms at the interface  
   
Van Landeghem, H. P., Langelier, B., Panahi, D., Purdy, G. R., Hutchinson, C. R., Botton, G. A., & Zurob, H. S. (2016). JOM, 68(5).
  
7
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
   
  
8
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Performing time- and space-resolved high energy X-ray diffraction experiments to gather 
phase transformation kinetics.
  
  
9
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Performing time- and space-resolved high energy X-ray diffraction experiments to gather 
phase transformation kinetics.
  
In one composition gradient
 
Growth kinetics of 20 points of different compositions every 30 seconds
During 300 seconds
200 measurements per gradient
Data for model calibration
  
10
Introduction-motivations
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Performing time- and space-resolved high energy X-ray diffraction experiments to gather 
phase transformation kinetics.
- APT (atom probe tomography) and TEM (transmission electron microscopy) techniques 
will be used on the treated samples to investigate the segregation at the migrating interface.   
  
11
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
   Solid joints 
Hot uniaxial compression
1
High temperature diffusion
2
Extending by cold/hot rolling3
  
12
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
   
Sample
Applied 
weight
Furnace
900°C 
22MPa
1hour
Ar/2%H2 
Fe-C-X1
Fe-C-X2
Fe-C-X3
Solid joints 
Hot uniaxial compression
1
  
13
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
   Solid joints 
Hot uniaxial compression
1
  
14
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
   Solid joints 
Hot uniaxial compression
1
  
15
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
   
High temperature diffusion
2
  
16
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
   Generate gradients of composition 
Perform diffusion in the single phase domain
DICTRA 1380°C for 72 hours        ~ 600-900 µm
High temperature diffusion2
Time
660°C – 6h 
Room Temperature
1380°C – 72h 
Te
m
pe
r a
t u
r e
Good control of diffusion atmosphere 
Avoid decarburization and oxidation 
Reduced pressure 2.5mbar
Argon flow (0.5l/min) < 5ppb O2
  
17
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
   
EPMA measurements before and after diffusion treatment
Diffusion couple 
Fe-0.3%C-1%Mn || Fe-0.3%C-0.2%Mo
  
72 hours at 1380°C
2.5mbar – Argon (high purity)
Profile length after diffusion
 
950µm (Mn profile)
700µm (Mo profile)
High temperature diffusion2
  
18
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
   
Extending by cold/hot rolling3
  
19
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Extending by cold/hot rolling3
Low carbon 
steel 
Reduction ~85%
Thickness : 7mm – to – 1mm
Sample
Small multiple cold rolling passes
  
20
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
EPMA measurements before and after diffusion treatment
Diffusion couple 
Fe-0.3%C-1%Mn || Fe-0.3%C-0.2%Mo
  
Profile length after diffusion
 
950µm (Mn profile)
700µm (Mo profile)
Extending by cold/hot rolling3
  
21
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
EPMA measurements before and after diffusion treatment
Diffusion couple 
Fe-0.3%C-1%Mn || Fe-0.3%C-0.2%Mo
  
Profile length after diffusion
 
950µm (Mn profile)
700µm (Mo profile)
After cold rolling 
~7 mm (Mn profile)
~4.5mm (Mo profile)
Extending by cold/hot rolling3
  
22
Methodology of CGM fabrication
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
EPMA measurements after cold rolling
Extending by cold/hot rolling3
Diffusion couple 
Fe-0.3%C || Fe-0.3%C-1.0%Ni
  
After cold rolling 
~3 mm (Ni profile)
  
23
High energy X-ray diffraction experiments
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
  
24
High energy X-ray diffraction experiments
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Performing time- and space-resolved high energy X-ray diffraction experiments to gather 
phase transformation kinetics.
Synchrotron beam time : 12 shifts –  9th-12th November 2018
    ESRF ( beamline ID11, HEXRD 87keV, beam size 200-600µm)
  
25
High energy X-ray diffraction experiments
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Performing time- and space-resolved high energy X-ray diffraction experiments to gather 
phase transformation kinetics.
Synchrotron beam time : 12 shifts –  9th-12th November 2018
    ESRF ( beamline ID11, HEXRD 87keV, beam size 200-600µm)
Procedure : 910°C – 10 s 775°C 
762°C  – 20 min
750°C
730°C
80°C
/s
 
 γ + α
 γ 
Te
m
p e
r a
t u
r e
Time
80°C
/s
Room Temperature
  
26
High energy X-ray diffraction experiments
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Performing time- and space-resolved high energy X-ray diffraction experiments to gather 
phase transformation kinetics.
Synchrotron beam time : 12 shifts –  9th-12th November 2018
    ESRF ( beamline ID11, HEXRD 87keV, beam size 200-600µm)
Procedure : 
    
 
    
   
Sample translation
Fe-C-X1
Fe-C-X2
Resistive heating
C
om
po
si
tio
n 
gr
ad
ie
nt
  
27
High energy X-ray diffraction experiments
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
ETMT
Primary 
beam
CCD 
detector
- Resistive heating
- 2D detector
- 2 welded thermocouples 
- Controlled atmosphere : Argon
- Acquisition time : 0.15 s
- Scan over 3 to 8 mm
 -Scan speed : 1mm / 2.6 s
- Scan step : 75 µm
Thermocouple
Sample
Pri
ma
ry 
bea
m
Sa
m
pl
e 
tr
an
sl
at
io
n
  
28
High energy X-ray diffraction experiments
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Debye-Scherer diffraction rings Intensity – 2θ plot 
circular integration
  
29
Results
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Data analysis : Pos x
              
n1
              
t+1
Te
m
p e
r a
t u
r e
Time
t1
t0
t2 t3
 
 γ + α
 γ 
 α
  
30
Shouldered peaks
Results
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Data analysis : 
Shouldered peaks - introducing errors on calculated ferrite fraction -  
  
31
Results
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Coarse microstructure 
Saturated pixels 
No powder diffraction condition 
  
32
Results
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
1mm
Decarburization during HEXRD measurements
Gradient of composition
Beam
  
33
Results
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
1mm
Decarburization during HEXRD measurements
Fe-C
-M
n
Gradient of composition in the sample depth
Heterogeneous deformation during cold-rolling
  
34
Results : Effect of Mn on formed ferrite fraction 
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Diffusion couple :Fe-0.16C / Fe-0.16C-1Mn (%wt.)
Temperature of transformation : 760°C
 
Te
m
p e
r a
t u
r e
Time
910°C/ 10s
760°C / 20min
Zero partition γ + α 
LEP
PE/LEP
PE/LENP α 
Composition gradient
γ
Fe-C-Mn 760°C
- No vertical composition gradient
- Limited decarburization ‘First thermal cycle’ 
- Correct diffraction rings ‘limited shouldered peaks 
effect’
  
35
Results : Effect of Mn on formed ferrite fraction 
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Diffusion couple :  Fe-0.16C || Fe-0.16C-1Mn (%wt.)
Temperature of transformation : 760°C after 20min
Non-complete 
transformation when 
increasing Mn content
Is it solute drag effect ?
  
36
Results : Effect of Mn on formed ferrite fraction 
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Diffusion couple :Fe-0.16C / Fe-0.16C-1Mn (%wt.)
Temperature of transformation : 760°C after 20min
Non-complete 
transformation when 
increasing Mn content
Is it solute drag effect ?
H.S. Zurob, D. Panahi, C.R. Hutchinson, Y. Brechet, G.R.
Purdy, Metall. Mater. Trans. A 44 (2013) 3456–3471.
  
37
Effect of Mn and Mo on ferrite growth kinetics
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Diffusion couple 
Fe-0.3%C-1%Mn || Fe-0.3%C-0.2%Mo
  
Profile length After cold rolling 
~7 mm (Mn profile)
~4.5mm (Mo profile)
Te
m
p e
r a
t u
r e
Time
910°C/ 10s
730°C / 20min
  
38
Effect of Mn and Mo on ferrite growth kinetics
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Diffusion couple Fe-0.3%C-0.2%Mo || Fe-0.3%C-1%Mn
  
Temperature of transformation : 730°C after 20 min
Non-complete transformation
Increasing with Mn content
 
  
39
Effect of Mn and Mo on ferrite growth kinetics
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Ferrite growth kinetics measured in a Fe-C-Mn || Fe-C-Mo diffusion couple 
Hi
gh
er
 M
n 
Lo
we
r M
o
Access to phase transformation kinetics 
dependency on composition
Coupling HEXRD with compositionally 
graded materials
  
40
Effect of Mn and Mo on ferrite growth kinetics
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Measured kinetics are 
slower than both PE 
and LENP modes
Gibbs energy 
dissipation by Solute-
interface interaction…
Is it Solute Drag effect
- Measured ferrite growth kinetics Vs LENP-PE predicted kinetics
  
41
Effect of Mn and Mo on ferrite growth kinetics
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
Measured kinetics are 
slower than both PE 
and LENP modes
Gibbs energy 
dissipation by Solute-
interface interaction…
Is it Solute Drag effect
Retardation effect
In Mn rich side
- Measured ferrite growth kinetics Vs LENP-PE predicted kinetics
Fe-0.11C-1.5Mn (0.5Mo)
Fe-0.12C-1.49Mn-xMo
Xia et al. Acta Mater. 
(2015)
Xia et al. Metall. Mater. Trans. (2006) 
650°C
550°C
  
42
What’s next ?
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Fix the prior problems : 
- Furnace with a rotating sample holder
- And controlled atmosphere
- Larger reduction using hot rolling followed by cold-rolling
Grain size
Decarburization 
Vertical gradient
Guillaume Geandier 
Benoit Denand
Intsitut Jean Lamour Nancy, France
  
43
What’s next ?
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 
- Implementing a new methodology for the fabrication of compositionally-graded materials.
- Fix the prior problems : 
- Furnace with a rotating sample holder
- And a better control of the atmosphere
- Larger reduction using hot rolling followed by cold-rolling
Performing ‘AGAIN’ time- and space-resolved high energy X-ray diffraction experiments to 
gather phase transformation kinetics. 
Desy-Hambourg November 2019 12 shifts
- APT (atom probe tomography) and TEM (transmission electron microscopy) techniques 
will be used on the treated samples to investigate the segregation at the migrating interface. 
Grain size
Decarburization 
Vertical gradient
  
44
Thank You
Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures - ALEMI Vancouver Canada 


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Development of compositional-gradient metallic alloys for combinatorial investigation of microstructures

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Archive Ouverte en Sciences de l'Information et de la Communication