International Conference on Mechanics of Nano, Micro and Macro Composite Structures International Conference on Mechanics of Nano, Micro and Macro Composite Structures International Conference on Mechanics of Nano, Micro and Macro Composite Structures International Conference on Mechanics of Nano, Micro and Macro Composite Structures Preparation, microstructure and properties of C sf /SiC multilayer composites by tape casting and pressureless sintering Wenshu Wenshu Yang Yang, , Elisa Elisa Padovano, Padovano, Laura Laura Fuso, Fuso, Matteo Matteo Wenshu Wenshu Yang Yang , , Elisa Elisa Padovano, Padovano, Laura Laura Fuso, Fuso, Matteo Matteo Pavese, Pavese, Silvia Pavese, Pavese, Silvia Silvia Silvia Marchisio, Marchisio, Dreidy Marchisio, Marchisio, Dreidy Dreidy Dreidy Vasquez, Vasquez, Vasquez, Vasquez, Claudia Claudia Claudia Claudia Vega Vega bolivar, Paolo Fino, Claudio Badini Vega Vega bolivar, Paolo Fino, Claudio Badini bolivar, Paolo Fino, Claudio Badini bolivar, Paolo Fino, Claudio Badini HTMAT group, HTMAT HTMAT HTMAT group, group, group, Department Department Department Department of Applied Science and of Applied Science and of Applied Science and of Applied Science and Technology Technology Technology Technology, Politecnico di Torino, Italy Politecnico di Torino, Italy Politecnico di Torino, Italy Politecnico di Torino, Italy Email: wenshu.yang@polito.it Email: wenshu.yang@polito.it Email: wenshu.yang@polito.it Email: wenshu.yang@polito.it
ICNMMCS ICNMMCS ICNMMCS ICNMMCS Outline � Introduction � Materials and Experimental � Results and Discussion � Conclusions � Acknowledgments
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 1. Introduction Properties Properties Properties Properties α- α α α - - -SiC SiC SiC SiC β β β β- -SiC - - SiC SiC SiC Crystal structure cubic hexagonal >1800 Melting Point ( ℃ ) 2730 (Transform into α-SiC) Density (g/cm 3 ) 3.21 3.21 Bulk modulus (GPa) 220 250 Elastic modulus (GPa) 450 400 Hardness RT (GPa) 36 32 CTE ( 10 −6 ℃ −1 ) 4.7 — SiC ( ) 2 O ( ) SiO ( ) CO ( ) + = + s g s g (1) 2 2 2 Passive oxidation 3 SiC ( ) O ( ) SiO ( ) CO ( ) + = + s g s g (2) 2 2 2 Low fracture toughness at room temperature
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 1. Introduction Toughing strategies • Introduction of second phase (composite) I. Particulates II. Whiskers III. Continuous fibres IV. Short fibres • Multilayers • Multilayer composite Crack deflection, pull-out and bridging of fibre or whicker, and interface delamination
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 1. Introduction Toho Tenax HTA40 fibre with epoxy coating Cut fibre Residual C 1. L. Fuso, D. Manfredi, S. Biamino, M. Pavese, P. Fino, C. Badini. SiC-based multilayered composites containing short carbon fibres obtained by tape casting. Composites Science and Technology. 2009, 69: 1772–1776.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 1. Introduction Purporses of This Study • To obtain C sf /SiC multilayer composites by tape casting and pressureless sintering. • To investigate the effect of short C fibre on microstructure, mechanical and thermal conductivity properties of C sf /SiC multilayer composites
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 2. Experimental Polyvinyl butyral as Polyethylene glycol as binder Toho HTC 124 (Water soluble sizing) plasticizer Fish oil as dispersant Dispersant B and C as sintering aids Ultrasonic α -SiC Ethanol and butanol as solvent Mechanical stirring Stacking Pressureless Tape and sintering Casting debinding SiC multilayer C sf /SiC multilayer composites 2. Matteo Pavese, Paolo Fino, Alberto Ortona, Claudio Badini. Potential of SiC multilayer ceramics for high temperature applications in oxidising environment. Ceramics International. 2008, 34: 197–203.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion (b) (a) (c) (g) + BYK 410 Without dispersant + BYK 163 (d) (f) (e) + Triton X100 + BYK 2150 + BYK 9077 + BYK 9076 Effect of dispersant (1 wt.%) on fibre dispersion (0.075 vol%) in mixture of ethanol and butanol: (a) BYK-163, (b) BYK-410, (c) BYK-2150, (d) BYK-9077, (e)BYK-9076, (f) Triton X-100. 3. W.S Yang, L. Fuso, S. Biamino, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Fabrication of short carbon fibre reinforced SiC multilayer composites by tape casting. Ceramic International. 2012, 38(2): 1011–1018.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion Observation Tape casting direction Tape casting direction
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion Typical fibre length distribution after 6 h mechanical mixture of SiC slurry and the fibre-predispersed solution. Statistical result of fibre length distribution after 6 h mechanical mixture of SiC slurry and the fibre-predispersed solution. 3 mm → 600 µ m 3 mm → 60 µ m 4. Zhang Y, Li S, Han J, Zhou Y. Fabrication and characterization of random chopped fiber reinforced reaction bonded silicon carbide composite. Ceramics International. 2012, 38: 1261-1266.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion 15 vol% 10 vol% 5 vol% Fracture surface of C sf /SiC multilayers with different fibre content after debinding. 5. W.S Yang, S. Biamino, E. Padovano, L. Fuso, M. Pavese, S. Marchisio, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Microstructures and mechanical properties of short carbon fibre/SiC multilayer composites prepared by tape casting. Composites Science and Technology. 2012, 72: 675–680.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion (a) (b) SiC 5 vol% 50 µ m 50 µ m (c) (d) 15 vol% 10 vol% XRD patterns of SiC multilayer and C sf /SiC multilayer composites. 50 µ m 50 µ m Representative morphology of sintered SiC multilayer and C sf /SiC multilayer composites. 5. W.S Yang, S. Biamino, E. Padovano, L. Fuso, M. Pavese, S. Marchisio, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Microstructures and mechanical properties of short carbon fibre/SiC multilayer composites prepared by tape casting. Composites Science and Technology. 2012, 72: 675–680.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion Relationships among fibre content, relative density and elastic modulus or bending strength of SiC multilayer and C sf /SiC multilayer composites. 5. W.S Yang, S. Biamino, E. Padovano, L. Fuso, M. Pavese, S. Marchisio, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Microstructures and mechanical properties of short carbon fibre/SiC multilayer composites prepared by tape casting. Composites Science and Technology. 2012, 72: 675–680.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion Fibre Relative Shrinkage (%) content density Materials (vol%) (%) Length Width Thickness SiC multilayer 0 88.8 19.1 20.7 21.4 5 83.1 5.1 19.0 31.7 C sf /SiC multilayer 10 81.3 3.9 15.1 26.4 composites 15 72.0 3.0 13.1 29.8 5. W.S Yang, S. Biamino, E. Padovano, L. Fuso, M. Pavese, S. Marchisio, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Microstructures and mechanical properties of short carbon fibre/SiC multilayer composites prepared by tape casting. Composites Science and Technology. 2012, 72: 675–680.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion SiC 5 vol% 15 vol% 10 vol% Fracture surface SiC multilayer and C sf /SiC multilayer composites. 5. W.S Yang, S. Biamino, E. Padovano, L. Fuso, M. Pavese, S. Marchisio, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Microstructures and mechanical properties of short carbon fibre/SiC multilayer composites prepared by tape casting. Composites Science and Technology. 2012, 72: 675–680.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion C fibre content Maximum Free carbon weight loss up in in Materials content to 1300 °C volume weight (wt.%) (wt.%) (vol%) (wt.%) SiC — — 4.5 0.2 multilayer 5 2.8 4.4 2.4 C sf /SiC multilayer 10 5.8 4.2 5.7 composites 15 8.9 4.1 11.2 Oxidation curves of SiC multilayer and C sf /SiC multilayer composites. 5. W.S Yang, S. Biamino, E. Padovano, L. Fuso, M. Pavese, S. Marchisio, D. Vasquez, C. Vega Bolivar, P. Fino, C. Badini. Microstructures and mechanical properties of short carbon fibre/SiC multilayer composites prepared by tape casting. Composites Science and Technology. 2012, 72: 675–680.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion (b) (a) (a) (b) (a) (b) Thermal diffusivity-Temperature relationship of pure SiC and C f /SiC in Z direction Thermal diffusivity-Temperature relationship of pure SiC and C f /SiC in Z direction Thermal conductivity of pure SiC and C f /SiC multilayers in Z direction at (a) before and (b) after 1500ºC/5h oxidation (a) before and (b) after 1500ºC/5h oxidation (a) 100 and (b) 1500ºC Effect of fibre amount on specific heat of multilayers R.G. Munro. Material properties of a sintered α -SiC. J. Phys. Chem. Ref. Data. 1997, 26(5): 1195-1203.
ICNMMCS ICNMMCS ICNMMCS ICNMMCS 3. Results and Discussion Heat flux SiC Multilayer C sf /SiC Multilayer Inner materials The outer dense SiC layers are expected to provide excellent oxidation resistance and good heat conductivity in the plane. The C sf /SiC layers in the middle of the multilayer architecture could grant acceptable thermal conductivity in plane and low conductivity through the TPS thickness.
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