reactive sintering

SPARK PLASMA REACTIVE SINTERING:
A SOLUTION FOR PRODUCING
DENSE MATERIALS
Frédéric BERNARD
Laboratoire Interdisciplinaire Carnot de Bourgogne
UMR 5209 CNRS / Université de Bourgogne.
9, Av. A. Savary, BP 47 870 F21078 Dijon, France,
Location
Nanostructured Materials Team
200 nm
1 µm
200 nm
ICB – UMR 5209 CNRS / Université de Bourgogne
NanoSciences Department
MaNaPI Team
Main Scientific Topics:
Study of interface phenomena of nano-objets : interaction with their environments,
Thermodynamic properties, reactivity and transport
Study of consolidation and grain growth mechanisms during Flash Sintering.
Study of nanostructure influence on physico-chemical properties
Mots clefs :
Nanostructures and Interfaces (Colloïdes, Powders and massive) –
Reactivity - in situ experiment - Modeling –“Flash” sintering
SYNTHESIS
Powders : Chemical and
mechanical routes
Denses : « Flash » Sintering
CHARACTERISATIONS
Ex-situ et in_situ of the microstructure
Physico-chemical properties
Modeling
APPLICATIONS TO NANOSTRUCTURED MATERIALS
DEFENSE
Part: DGA, NEXTER,
CIME BOCUZE, STGOBAIN
ENERGY
Part: CEA Valduc, CEA
Grenoble, CEA Cadarache, CEA
Valrhô, SNPE, AREVA-NP
HEALTH
Part: PHARMIMAGE,
CHU, NVH Medicinal
PRODUCTION OF NANOPOWDERS (H2O supercritical)
ZrO2
ZnO
TiO2
Aimable, A.; Muhr, H.; Gentric, C.; Bernard, F.; Le Cras, F.; Aymes, D. Powder Technology (2009), 190(1-2), 99-106.
Aimable, A.; Xin, B.; Millot, N.; Aymes, D. Journal of Solid State Chemistry (2008), 181(1), 183-189.
SPS EQUIPEMENT
ICB Dijon (F. Bernard) FCT System HP D 125
Max. pressing Ø
Pressing force
Piston stroke
Piston velocity
Temperature
Gas pressure
150
20…1250
0…200
0…4
RT…2400
5∙10-2…1100
mm
kN
mm
mm/s
°C
mbar
Pulse voltage
Pulse current
Power max.
Pulse duration
Pause time
0...10
0...30000
300
1...1000
0...1000
V
A
kW
ms
ms
CHARACTERIZATION FACILITIES
Morphology, Size, Surface...
SEM, BET, XRD , Raman Spectroscopy, Granulometry…
5 nm
{111}
0.26 nm
[111]
{100}
Raman Reactional Chamber
Structure, Microstructure, Texture...
XRD, TEM, Raman Spectroscopy
Behavior, Reactivity, Dilatation...
XPS, TGA/DTG, Dilatometry
Raman Spectrometry
Curve detector
In-Situ Characterizations
very accurately device for controlling and monitoring
pO2 (1 to 10-31 bar) coupled to ATG, XRD, Raman,
Dilatometry…
Synchrotron and Neutron Facilities
LURE (TRXRD, EXAFS)
ESRF (anomalous diffraction)
LLB, ILL (neutron diffraction)
Reactional
Chamber
Goniometer 4 cercles
Infrared Camera
(40 frames/sec)
TRXRD Device on H10
Beamline at LURE
SPARK PLASMA SYNTHESIS
Flash Reactive Sintering
2 µm
REACTIVE SINTERING : PRINCIPLE
REACTANT POWDERS
Powder A
Powder B
REACTIVE SINTERING
OF M(A+B) FOR
PRODUCING DENSE AB
COMPOUND
MIXTURE OF
REACTANT POWDERS
M(A+B)
P=CHARGE
PUNCH
SAS
DIE
POWDER
SPS CHAMBER
1 µm
DC PULSED
COURANT
SPARK PLASMA SYNTHESIS
Flash Reactive Sintering
Solid State
Reaction
+
Densification
Combustion
Synthesis
+
Densification
CONTENTS : REACTIVE SINTERING
I.
II.
III.
IV.
V.
VI.
INTRODUCTION
PREPARATION OF REACTANT POWDER MIXTURES
DEVELOPPEMENT OF SPECIFIC TOOLS
EXAMPLE 1 : SHS REACTION IN Mo/2Si SYSTEM
EXAMPLE 2 : SOLID STATE REACTION IN IODOAPATITE
SOME APPLICATIONS