First tensile tests on SiC fiber under ion beam
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1 First tensile tests on SiC fiber under ion beam CEA/DEN/DANS/DMN/SRMA: A. Jankowiak, C. Colin, K. Shimoda, JM. Costantini, S. Paradowski, T. Vandenberghe, S. Doriot CEA/DEN/DANS/DMN/SRMP: Y. Serruys, E. Bordas (JANNUS Saclay) CEA/DSM/IRAMIS/CIRIL: I. Monnet, T. Madi (GANIL Caen) CEA/DSM/IRAMIS/CIMAP: C. Grygiel (GANIL Caen) Commissariat à l'énergie Atomique de Saclay (CEA-Saclay) Gif-sur-Yvette Cedex, France 1
2 Background: SiC/SiC composites in nuclear fields Interesting intrinsic safety features: low activation level, high radiation damage tolerance Higher operating temperature with higher efficiency SiC/SiC composites are considered as advanced structural materials for fission and fusion nuclear energy systems 2
3 Current status of SiC/SiC for nuclear applications Su Irrad. /Su Unirrad. Use possible Recent developments lead to: - Near-stoichiometry (C/Si =1) - Highly crystalline matrerial Hi-Nicalon Type-S/PyC/FCVI-SiC Hi-Nicalon/PyC/FCVI-SiC Nicalon/PyC/FCVI-SiC Tyranno-SA/PyC/FCVI-SiC Monolithic CVD-SiC Kyoto/ORNL/PNNL/Tohoku Neutron Dose [dpa-sic] Selected composite for nuclear application composed: Tyranno TM -SA 3rd, Hi-Nicalon type-s fibers CVI matrix Pyrocarbon interface TySA/HNL-S HNL [1, 2] L.L. Snead, et al., JNM (2000) [5] R.H. Jones, et al., 1st IEA-SiC/SiC (1996) [6, 7] L.L. Snead, et al., JMR, submitted. 5 [8] T. Nozawa, et al., JNM (2002) [10] R.J. Price, et al., JNM (1982) [11] R.J. Price, et al., JNM 33 (1969) CG-NL irradiated composites does not exhibit degradation of mechanical strength up to 10 dpa (3 rd generation fiber) 1: 500C, HFIR 2: 400C, HFIR 3: C, HFIR 4: C, JMTR 5: C, EBR-II 6: 300C, HFIR 7: 800C, HFIR 8: 800C, JMTR 9: C, JOYO 10: 740C, HFIR 11: 630, 1020C, ETR 1 st and 2 nd generation: large strength loss > 1 dpa 3
4 Position of this study High-temperature No-irradiation Test of asreceived fibers at high temperatures (2006 ~ ) Test of asreceived fibers at roomtemperature (2006 ~ ) Test of ionirradiated fibers at high temperatures ( ) In-situ test at hightemperatures during ionirradiation using Mini MecaSiC (2012~) 1 st stage 2 nd stage 3 rd stage Test of ionirradiated fibers at roomtemperature ( ) In-situ test at room-temperature during ionirradiation using Mini MecaSiC (2011~) Irradiation Prospect under neutron irradiation Room-temperature 4
5 Position of this study High-temperature No-irradiation Test of asreceived fibers at high temperatures (2006 ~ ) Test of asreceived fibers at roomtemperature (2006 ~ ) Test of ionirradiated fibers at high temperatures ( ) In-situ test at hightemperatures during ionirradiation using Mini MecaSiC (2012~) 1 st stage 2 nd stage 3 rd stage Test of ionirradiated fibers at roomtemperature ( ) In-situ test at room-temperature during ionirradiation using Mini MecaSiC (2011~) Irradiation Prospect under neutron irradiation Room-temperature 5
6 Experimental procedures SiC Fibers Tyranno-SA grade 3 (Ube Industry Ltd) with a mean diameter of 7.5µm (30 irradiated fibers ) 6
7 Experimental procedures SiC Fibers Tyranno-SA grade 3 (Ube Industry Ltd) with a mean diameter of 7.5µm (30 irradiated fibers ) Irradiation conditions in GANIL - 92MeV Xe beam and two flux ( 3.3 x 10 9 ions/cm 2 /s x 10 9 ions/cm 2 /s) - Room-temperature, runs divided in two periods (irradiation of both sides) - Fluence: 2.46 x ions/cm x ions/cm 2: damage level 0.05dpa 9.89 x ions/cm x ions/cm 2 (more damage): 0.2dpa First side Fiber Opposite side Ion-irradiation direction Fibers 35mm 7.5µm 7
8 Fiber cross-sectional damage profile using original-code (accumulation ) 1 named as irr-0.05 (mean) dpa named as irr-0.2 (mean) dpa Y (µm) 0-2 Y (µm) 0-2 X (µm) dpa X (µm) dpa - Irradiation damages in the fiber affected the entire volume - Maximum damage peak located at both edges near surface of the fiber against the ion-irradiated direction 8
9 Effect of the ion-irradiation on the structure In this study (~40 o C) -TySA3 irr0.05 =>No amorphization expected at low dpa -TySA3 irr0.2 => Potential amorphization in limited areas (edges of fiber) amorphization: 0.3 dpa *Ref. L.L. Senad et al, Nucl. Instrum. Meth. B 116 (1996) L.L. Senad et al, J. Nucl. Mater. 273 (1999) W.J. Weber et al, Mater. Sci. Eng. A 253 (1998)
10 Effect Edge of part the ion-irradiation on the structure (TySA3 irr0.2) Damage profile of TySA3 irr0.2 TEM image No amorphization detected at 0.2 dpa by TEM High magnification Ref: A. Audren, et al., NIMPR B 266 (2008) µm 10
11 MecaSiC to determine fiber properties Tensile tests from RT to 1800 C Vacuum: 10-6 bar (He atmosphere under development) Single SiC fiber Gauge length: 25 mm Measurement of diameter by laser diffractometry Zoom Graphite-grip method: cold grips and uniform temperature Heating by Joule effect up to 1800 C Post irradiation tests Monotonic tensile tests, thermal stability, thermal expansion, creep tests, electrical resistivity determination 11
12 Effect of ion-irradiation on thermo-elastic modulus RT C 450 Unirradiated fibers slight decrease with temperature (reversibility) Irradiated fibers decrease in elastic modulus at RT mechanical recovering starting at 700 o C gradual recovering during cooling similar behaviors for both irradiated fibers irr0.05 completely recovered at 1500 o C irr0.2 not recovered at 1500 o C Elastic modulus, GPa Normarized Elastic modulus ,3 1,25 1,2 1,15 1,1 1,05 1 0,95 0,9 0,85 0, Temperature, C Temperature, C 12
13 Effect of the ion-irradiation on the thermal expansion up to 1800 C Unirradiated fibers gradual increase with temperature no difference between heating and cooling (reversibility) =>material stability Irradiated fibers Three stages Test conditions: - T=RT<=>1800 o C - Heating/cooling=50 o C/min - Constant stress=20mpa gradual increase below 200 o C slight increase in the range o C significant increase above 1400 o C =>gradual decrease during cooling (similarly to unirradiated) =>shrinkage (material instability) =>larger shrinkage in irr0.2 13
14 Annealing treatments on TySA3 irr0.05 Test conditions: - T=RT<=>1800 o C - Heating/cooling=50 o C/min - Constant stress=20mpa Irradiated fibers shrinkage (recovering) begins at 200 o C linear decrease at 800 o C saturation at 1400 o C for 0.45% 14
15 Position of this study High-temperature No-irradiation Test of asreceived fibers at high temperatures (2006 ~ ) Test of asreceived fibers at roomtemperature (2006 ~ ) Test of ionirradiated fibers at high temperatures ( ) In-situ test at hightemperatures during ionirradiation using Mini MecaSiC (2012~) 1 st stage 2 nd stage 3 rd stage Test of ionirradiated fibers at roomtemperature ( ) In-situ test at room-temperature during ionirradiation using Mini MecaSiC (2011~) Irradiation Prospect under neutron irradiation Room-temperature 15
16 Position of this study High-temperature No-irradiation Test of asreceived fibers at high temperatures (2006 ~ ) Test of asreceived fibers at roomtemperature (2006 ~ ) Test of ionirradiated fibers at high temperatures ( ) In-situ test at hightemperatures during ionirradiation using Mini MecaSiC (2012~) 1 st stage 2 nd stage 3 rd stage Test of ionirradiated fibers at roomtemperature ( ) In-situ test at room-temperature during ionirradiation using Mini MecaSiC (2011~) Irradiation Prospect under neutron irradiation Room-temperature 16
17 Development of a in-situ tensile test device Same characterstics than Mecasic but more compact Implemented on every type of beam line To be used for other type of materials Gauge length: 25 mm Measurement of diameter by laser diffractometry (in-situ measurement possible) Vacuum: 10-6 bar (He atmosphere under development) Tensile tests at high temperature Graphite-grip method: cold grips and uniform temperature Heating by Joule effect up to 1800 C In-situ tests Swelling rate under irradiation, annealing study (in-situ, ex situ), irradiation creep. 17
18 Implementation in JANNUS Saclay E3 Épiméthée line 18
19 Tensile tests under flux (1) Irradiation conditions for Minimecasic experiment Irradiation End Strain % Residual strain 1 => Pre-stressing at 300MPa (! Strain depends on initial position of the motorised linear stage!) 2 => Fiber thermal expansion (irradiation) 3 => Strain variation (fiber and the graphite grips) : thermal expansion and swelling 4 => Fluctuation due to flux variation 5 => Fiber cooling (end of the irradiation) 6 => Graphite grip cooling 7 => Residual strain Time 10 3 s Difficulties to identify swelling due to irradiation from thermal expansion Graphite grips partially exposed (device improved) - Residual strain (0.20%) after the 3 runs of irradiation (0.40%) 19
20 Implementation in GANIL Caen IRRSUD line 20
21 Tensile tests under flux (2) Irradiation conditions for Minimécasic experiment Fiber SiC Tyranno SA3 Fiber diameter (µm) 7,44 Ion Xe23+ Energy (MeV) 92 Flux (ion/cm²/s) 3,29E+09 Dose(ions/cm²) 5,00E+14 dpa 0,1 (max 0,3) Fiber temperature max ( C) 44,6 C 1 => Pre-stressing at 300MPa 2 => Fiber expansion (only irradiation swelling) (2) Irradiation (3) Residual strain (4) 3 => Fluctuation due to flux beam shut down (themal expansion can be neglected) (1) 4 => Residual strain (0.45%) - Swelling rate of SiC for determined irradiation conditions - Residual strain after irradiation (0.45%) - After annealing at 1800 C this residual strain disappears almost completely 21
22 Annealing treatments Test conditions: - T= C(RT<=>200, 400, 600, C, 3min) - Detected from (σ, ε) curvature after cooling 1 => shrinkage starts at 200 o C 2 => gradual shrinkage when increasing temperature 3 => saturation at 1400 o C (recovering = 0.45%) Total recovering (1) (2) Good agreements with previous PI tests using similar irradiation conditions (3) Annealing temperature C 22
23 Position of this study High-temperature No-irradiation Test of asreceived fibers at high temperatures (2006 ~ ) Test of asreceived fibers at roomtemperature (2006 ~ ) Test of ionirradiated fibers at high temperatures ( ) In-situ test at hightemperatures during ionirradiation using Mini MecaSiC (2012~) 1 st stage 2 nd stage 3 rd stage Test of ionirradiated fibers at roomtemperature ( ) In-situ test at room-temperature during ionirradiation using Mini MecaSiC (2011~) Irradiation Prospect under neutron irradiation Room-temperature 23
24 Position of this study High-temperature No-irradiation Test of asreceived fibers at high temperatures (2006 ~ ) Test of asreceived fibers at roomtemperature (2006 ~ ) Test of ionirradiated fibers at high temperatures ( ) In-situ test at hightemperatures during ionirradiation using Mini MecaSiC (2012~) 1 st stage 2 nd stage 3 rd stage Test of ionirradiated fibers at roomtemperature ( ) In-situ test at room-temperature during ionirradiation using Mini MecaSiC (2011~) Irradiation Prospect under neutron irradiation Room-temperature
25 Thank you for your attention
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