Bergeon, N.

Ji, K.

Karma, A.

Mota, F. L.

Pereda, J.

Song, Y.

Strutzenberg, L. L.

Tourret, D.

Trivedi, R.

NASA Technical Reports Server

UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
1 3D pattern adjustment during directional 
solidification of a transparent alloy 
conducted on DECLIC-DSI 
F.L.Mota, J.Pereda, N.Bergeon 
IM2NP, CNRS 
Aix-Marseille Université 
Marseille, France 
K.Ji, Y.Song, A.Karma 
Physics Department  
Northeastern University, Boston, USA 
R.Trivedi 
Dpt of Materials Science & Engineering  
Iowa State University, Ames, USA 
L.L.Strutzenberg 
Marshall Space Flight Center,  
Huntsville, USA 
D. Tourret 
IMDEA Materials Institute,  
Madrid, Spain 
https://ntrs.nasa.gov/search.jsp?R=20190027445 2019-09-26T19:19:30+00:00Z
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
2 Introduction 
  DECLIC-DSI instrument 
  Experiments in the DECLIC-DSI 
 
Effect of sub-boundaries on Primary spacing 
 Experimental results 
 Phase field simulations 
 
Conclusion and perspectives 
 
 
 
 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
3 DECLIC-DSI Device 
To study the microstructure formation 
during directional solidification Location of DSI 
Kibo module 
DSI 
(Directional  
 Solidification 
 Insert) 
DECLIC 
ISS 
Transparent systems   
In situ and real time observation 
of interfacial microstructure 
Large cylindrical crucible  
extended patterns 
Onboard the ISS from 2009 to 2011  
microgravity experiments 
dedicated to cellular regime 
Experiments on ground  
understand the effect of 
convection 
Onboard the ISS from 2017 to 2018  
microgravity experiments 
dedicated to dendritic regime 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
4 Experiments in the DECLIC-DSI  
Axial 
view 
1 cm 
13 cm 
Cylindrical crucible      
Diameter: 1 cm 
Solidification length: 10 cm 
SCN – 0.24 wt% camphor 
V: 0.1 – 30 µm/s 
G: 12 and 19 K/cm 
Solid seed: single crystal of 
selected orientation; kept during 
the whole flight campaign 
Vp = 0 µm/s 
Vp = 4 µm/s 
Vp = 15 µm/s 
Side view 
Vp = 0 µm/s Vp = 6 µm/s 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
5 Pattern analysis 
Reference experiment  
7.37 x 7.37 mm²  Real duration: 9h   
 Vp = 2  µm/s     G = 19 K/cm 
In-house software to follow each cell in time: 
 Primary spacing 
 Number of 1st neighbors 
 Trajectories (V, direction) 
 Pattern sliding 
 Very few tip-splittings 
 Areas of high elimination  
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
6 Evidence of Sub-boundaries 
 Motion associated to numerous phenomena  
dynamical reorganization 
500 µm 
V = 1 µm/s G = 19 K/cm 
 All boundaries are moving due to non-negligible 
surface tension anisotropy  
• Confirms the sub-boundary nature 
• Even at rest, some SB are moving at very low velocity – SB coarsening 
 All the Sub-grain boundaries are fixed 
when morphological instability triggers 
Elimination of SG   
Nucleation of a new SG  
(on pre-existing junctions) 
S. Bottin-Rousseau et al. PRB 66 (2012) 4102 
G. Faivre et al. CR Phys 14 (2013) 149 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
7 Effect of sub-grain on the dynamics of primary spacing 
 3 areas of  Vg and     3 sub-grains 
 Divergent and convergent GB 
Primary spacing evolution  
by sub-grain 
Cell trajectories analysis 
 Noticeable differences of  evolution 
depending on sub-grain 
 Cannot be attributed to differences 
of misorientation (1.4° < (Vg) < 1.9°) 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
8 Boundaries configuration 
 Initially: large distribution of , 
 homogeneously distributed  
 With time: global decrease of    
 except around the divergent GB 
 The evolution of primary 
spacing strongly depends 
on the distance to the 
divergent GB                
(effect  20 cells) 
 The effect of convergent 
GB is of shorter distance  
( 5 cells)  
Critical role of 
boundaries 
Primary spacing map  
Duration: 6.5 h 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
9 
 Target condition: Vp = 2  µm/s, G = 19 K/cm  
 Regular hexagonal array (λ = 220 μm) 
 Simulation box: 3960.74 × 760.14 μm² 
SB 
y 
z 
1 3 
Φ1 = -12° 
θ1 = 2.33° 
 
Φ3 = 165° 
θ3 = 3.07° 
Divergent SB: comparison experiment and PF 
-6 -4 -2 0 2 4
180
200
220
240
260
280
300
P
ri
m
a
ry
 S
p
a
c
in
g
 (
µ
m
)
Distance from the SG1-SG3 border (mm)
 t = 0.76 h
 t = 0.96 h
 t = 2.07 h
 t = 3.39 h
 t = 4.75 h
 t = 6.05 h
 t = 7.40 h
 t = 8.08 h
EXPERIMENT 
-2 0 2
160
180
200
220
240
260
280
P
ri
m
a
ry
 S
p
a
c
in
g
 (
µ
m
)
Distance from the SG1-SG2 border (mm)
 t = 0.36 h
 t = 0.94 h
 t = 1.95 h
 t = 2.82 h
 t = 3.26 h
 t = 3.84 h
3D SIMULATION 
 The plateau λ on the left is 
decreasing in experiment, while 
increasing in the 3D PF simulation 
• Exp: the source produces cells with 
smaller λ 
• PF: the source produces cells with 
larger λ 
 The shape of the λ peak extends 
in simulation while becomes 
narrower in experiment 
Long distance 
effect of sources? 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
10 
SB 
Φ1 = -37° 
θ1 = 2.33° 
 
Φ2 = 62° 
θ2 = 2.67° 
y 
z 
1 2 
Convergent SB: comparison experiment and PF 
 Target condition: Vp = 2  µm/s, G = 19 K/cm  
 Regular hexagonal array (λ = 220 μm) 
 Simulation box: 3960.74 × 760.14 μm² 
-6 -4 -2 0 2
180
200
220
240
260
280
300
P
ri
m
a
ry
 S
p
a
c
in
g
 (
µ
m
)
Distance from the SG1-SG2 border (mm)
 t = 0.76 h
 t = 0.96 h
 t = 2.07 h
 t = 3.39 h
 t = 4.75 h
 t = 6.05 h
 t = 7.40 h
 t = 8.08 h
-2 0 2
160
180
200
220
240
260
280
P
ri
m
a
ry
 S
p
a
c
in
g
 (
µ
m
)
Distance from the SG1-SG2 border (mm)
 t = 0.36 h
 t = 0.94 h
 t = 1.95 h
 t = 2.82 h
 t = 3.26 h
 t = 3.84 h
EXPERIMENT 3D SIMULATION 
 The plateau λ on the right side of 
SB is decreasing in experiment, 
while increasing in the 3D PF 
simulation 
• Exp: the source produces cells with 
smaller λ 
• PF: the source produces cells with 
larger λ 
 The λ at the SB keeps decreasing 
until reaches the lowest point 
 Mechanisms along SB 
• Exp:  SB  stable, numerous eliminations 
• PF: incursions 
Long distance 
effect of sources? 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
11 
Conclusion 
 
 
 
 
 Success of µg experiments: extended 2D patterns of cells   
  Benchmark data in diffusive transport mode 
 Critical role of sub-boundaries configuration on primary spacing evolution
  3D phase simulations in progress… 
 1st observation of solitary cells: 3D phase field simulations   
  Behavior maps  = f(orientation angles) 
6
3
3
 μ
m
 
Vp = 1.5  µm/s 
G = 19 K/cm 
Orientation defect 
1
8
6
5
 μ
m
 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
12 DSI-R: dedicated to the dendritic regime 
 Increase of concentration  Dendrites at lower  pulling rates  
 Study of the formation of well-developed dendritic array structures 
V1 = 1.5 V2 = 12 µm/s, G = 12 K/cm, 6h15min V1 = 12 V2 = 3 µm/s, G = 12 K/cm, 3h28min 
UMR 7334, CNRS, Universités d’Aix-Marseille (AMU) et de Toulon (UTLN) 
13 
DECLIC 
onboard 
ISS 
Deepest thanks to 
 
CNES and NASA 
Thank you for 
your attention 
Image CADMOS-CNES/Sébastien Rouquette 
Image IM2NP 


3D Pattern Adjustment During Directional 1 Solidification of a Transparent Alloy Conducted on DECLIC-DSI

3D Pattern Adjustment During Directional 1 Solidification of a Transparent Alloy Conducted on DECLIC-DSI

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