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Extremely fast sintering of advanced ceramic materials
Tan, Hua ; Chlup,, Zdeněk (oponent) ; Sedláček,, Jaroslav (oponent) ; Salamon, David (vedoucí práce)
Rapid sintering techniques, such as Spark Plasma Sintering (SPS), Flash Sintering (FS), Selective Laser Sintering (SLS), Induction Sintering (IS), and Microwave Sintering (MS), are designed to effectively and predictably control ceramic microstructure during the sintering process. Spark Plasma Sintering as one of the most novel rapid sintering technique has been studied for decades. There are three main features in SPS: direct Joule heating, pulsed direct current, and mechanical pressure. However, the mechanisms of these features are not clearly and fully addressed. This thesis was inspired by the increasing attention towards rapid sintering techniques and open scientific questions. The present study has four parts, investigation of ‘Field effect’, pulse pattern effect, pressure effect, and direct Joule heating. The results showed the negligible impact of the electromagnetic field during SPS according to the simulation as well as no ‘field effect’ was found during the experiments. While the effect of pulse pattern was significant, the TiO2 powder was sintered by pulse patterns 12:2 and 10:9 with the constant power input. Titania grain size increased one order of magnitude and 8% in density after application of the pulse pattern 10:9, while the amount of consumed energy remained constant. The variation of the effective power and contact resistance induced by the mechanical pulse are two main reasons accounting for the varying energy efficiency heating with different pulse patterns. The pressure timing effect also significantly influenced the SPS. The results showed that applying the pressure at 900 brought high density and small grain size of the sintered alumina nanopowder, leading to the best Vickers hardness. The interaction between pressure and vapor, leading to the different vapor transfer rate of the first sintering stage, was considered as a reason for the differences in microstructure (micropores, grain size, etc.). The timing of the mechanical pressure can also promote the densifying diffusion mechanisms during the second sintering stage, such as grain boundary diffusion and lattice diffusion. The direct Joule heating of the electrically conductive samples by direct electrical current passing through the sample leads to high internal and low measured temperature when sintering boron carbide (B4C) and its composites. Adding titanium alloy and silicon in B4C significantly increased the densification, which was the main reason for the change of mechanical properties. The sample doped by 1 vol. % of Ti alloy (B4C+1.0Ti) reached the hardness 3628.5 ± 452.6 HV1 (16.2% higher than pure boron carbide) with a fracture toughness 2.11 ± 0.25 MPam0.5. The sample doped by 0.5 vol. % of Si (B4C+0.5Si) achieved the hardness 3524.6 ± 207.8 HV1 (13.0% higher than pure boron carbide), the sample B4C+1.0Si achieved the highest fracture toughness 2.97 ± 0.03 MPam0.5 (15.6% higher than pure boron carbide). The grains of titanium doped composites became a bit larger and inhomogeneous compared with the pure boron carbide. In contrast, the grain size of silicon doped samples did not change compared with that of pure boron carbide. The secondary phase silicon carbide was well connected with the boron carbide matrix and showed a great strengthen effect on both the hardness and fracture toughness. This work examined various features of the SPS technique and their effect on ceramic materials, leading to a better understanding of this novel technique.
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Extremely fast sintering of advanced ceramic materials
Tan, Hua ; Chlup,, Zdeněk (oponent) ; Sedláček,, Jaroslav (oponent) ; Salamon, David (vedoucí práce)
Rapid sintering techniques, such as Spark Plasma Sintering (SPS), Flash Sintering (FS), Selective Laser Sintering (SLS), Induction Sintering (IS), and Microwave Sintering (MS), are designed to effectively and predictably control ceramic microstructure during the sintering process. Spark Plasma Sintering as one of the most novel rapid sintering technique has been studied for decades. There are three main features in SPS: direct Joule heating, pulsed direct current, and mechanical pressure. However, the mechanisms of these features are not clearly and fully addressed. This thesis was inspired by the increasing attention towards rapid sintering techniques and open scientific questions. The present study has four parts, investigation of ‘Field effect’, pulse pattern effect, pressure effect, and direct Joule heating. The results showed the negligible impact of the electromagnetic field during SPS according to the simulation as well as no ‘field effect’ was found during the experiments. While the effect of pulse pattern was significant, the TiO2 powder was sintered by pulse patterns 12:2 and 10:9 with the constant power input. Titania grain size increased one order of magnitude and 8% in density after application of the pulse pattern 10:9, while the amount of consumed energy remained constant. The variation of the effective power and contact resistance induced by the mechanical pulse are two main reasons accounting for the varying energy efficiency heating with different pulse patterns. The pressure timing effect also significantly influenced the SPS. The results showed that applying the pressure at 900 brought high density and small grain size of the sintered alumina nanopowder, leading to the best Vickers hardness. The interaction between pressure and vapor, leading to the different vapor transfer rate of the first sintering stage, was considered as a reason for the differences in microstructure (micropores, grain size, etc.). The timing of the mechanical pressure can also promote the densifying diffusion mechanisms during the second sintering stage, such as grain boundary diffusion and lattice diffusion. The direct Joule heating of the electrically conductive samples by direct electrical current passing through the sample leads to high internal and low measured temperature when sintering boron carbide (B4C) and its composites. Adding titanium alloy and silicon in B4C significantly increased the densification, which was the main reason for the change of mechanical properties. The sample doped by 1 vol. % of Ti alloy (B4C+1.0Ti) reached the hardness 3628.5 ± 452.6 HV1 (16.2% higher than pure boron carbide) with a fracture toughness 2.11 ± 0.25 MPam0.5. The sample doped by 0.5 vol. % of Si (B4C+0.5Si) achieved the hardness 3524.6 ± 207.8 HV1 (13.0% higher than pure boron carbide), the sample B4C+1.0Si achieved the highest fracture toughness 2.97 ± 0.03 MPam0.5 (15.6% higher than pure boron carbide). The grains of titanium doped composites became a bit larger and inhomogeneous compared with the pure boron carbide. In contrast, the grain size of silicon doped samples did not change compared with that of pure boron carbide. The secondary phase silicon carbide was well connected with the boron carbide matrix and showed a great strengthen effect on both the hardness and fracture toughness. This work examined various features of the SPS technique and their effect on ceramic materials, leading to a better understanding of this novel technique.
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