High-thermal-conductivity silicon nitride ceramic material and preparation method thereof
A technology of silicon nitride ceramics and raw materials, which is applied in the field of high thermal conductivity silicon nitride ceramic materials and its preparation, can solve the problems of high oxygen content, reduce energy consumption and cost, and be difficult to densify, and achieve low amorphous phase content , reduce lattice defects, and promote densification
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Embodiment 1
[0046] With 1wt% TiH 2 and 4wt% MgO as a sintering aid, and 95wt% α-Si 3 N 4 The powder is mixed by ball milling, dried and sieved to obtain a uniformly mixed powder; then it is dry-pressed under a pressure of 20MPa, and then subjected to cold isostatic pressing under a pressure of 250MPa; the green body obtained is put into a BN crucible , held at 510°C for 2 hours in an Ar atmosphere, then raised to 1000°C and held for 4 hours for pre-sintering; then the pre-sintered green body was sintered at 1780°C, the heating rate was 10°C / min, and the holding time was 4h; the sintering was completed Afterwards, cool to 1200°C at a cooling rate of 10°C / min, and then cool to room temperature with the furnace.
[0047] The density of the silicon nitride ceramic material prepared in Example 1 is 97.3%, the three-point bending strength is 449MPa, and the fracture toughness is 4.56MPa m 1 / 2 , the thermal conductivity is 55.6W / (m·K).
Embodiment 2
[0049] With 6wt% TiH 2 and 2wt% MgO as a sintering aid, and 92wt% α-Si 3 N 4 The powder is mixed by ball milling, dried and sieved to obtain a uniformly mixed powder; then dry-pressed under a pressure of 20MPa, and then subjected to cold isostatic pressing under a pressure of 300MPa; the green body obtained is put into a BN crucible , in an Ar atmosphere at 600°C for 2h, then heat up to 1200°C for 4h for pre-sintering; then sinter the pre-sintered green body at 1800°C for 1.5h, with a heating rate of 10°C / min; after sintering , cooled to 1550°C at a cooling rate of 2°C / min and held for 8 hours, and then cooled to room temperature with the furnace.
[0050] The density of the silicon nitride ceramic material prepared in Example 2 is 97.9%, the thermal conductivity is 62W / (m·K), the three-point bending strength is 508MPa, and the fracture toughness is 4.75MPa·m 1 / 2 .
Embodiment 3
[0052] With 5wt% TiH 2 and 7wt% MgO as a sintering aid, and 88wt% α-Si 3 N 4 The powder is mixed by ball milling, dried and sieved to obtain a uniformly mixed powder; then it is dry-pressed under a pressure of 30MPa, and then subjected to cold isostatic pressing under a pressure of 300MPa; the green body obtained is put into a BN crucible , after holding at 600°C for 2h under vacuum, the temperature was raised to 1300°C for 4h for pre-sintering; then the pre-sintered green body was sintered at 1780°C for 4h, and the heating rate was 5°C / min; then, at 1°C / min Cool down to 1580°C at a cooling rate of min and hold for 12 hours, then cool to room temperature with the furnace.
[0053] The density of the silicon nitride ceramic material prepared in Example 3 is 98.7%, the thermal conductivity is 78.90W / (m·K), the three-point bending strength is 510MPa, and the fracture toughness is 5.59MPa·m 1 / 2 . The cross-sectional microscopic topography figure of the silicon nitride ceramic ...
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