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Silicothermic reduction method for improving thermal conductivity and mechanical properties of silicon nitride ceramic substrate material

A technology of silicon nitride ceramics and thermal conductivity, applied in the field of inorganic non-metallic materials, can solve the problems of reducing the strength of silicon nitride, grain growth, etc., and achieve the reduction of liquid phase content, intergranular phase content reduction, and mechanical properties Reduced effect

Active Publication Date: 2020-12-29
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method will make the grain grow abnormally and reduce the strength of silicon nitride

Method used

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  • Silicothermic reduction method for improving thermal conductivity and mechanical properties of silicon nitride ceramic substrate material
  • Silicothermic reduction method for improving thermal conductivity and mechanical properties of silicon nitride ceramic substrate material
  • Silicothermic reduction method for improving thermal conductivity and mechanical properties of silicon nitride ceramic substrate material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] With 4mol% Y 2 o 3 and 8mol% MgO as a sintering aid, and 88mol% α-Si 3 N 4 Powder, add 0.1wt% Si, mix by ball milling, and sieve after drying to obtain a uniformly mixed powder; then dry press molding under 30MPa pressure, and then perform cold isostatic pressing under 300MPa pressure; the obtained The green body was put into a BN crucible, held at 1200 °C for 8 h under vacuum for deoxidation pretreatment; then sintered at 1900 °C under pressure, with a heating rate of 5 °C / min, N 2 The pressure is 1MPa, and the holding time is 4h; after sintering, cool to 1000°C at a cooling rate of 15°C / min, and then cool to room temperature with the furnace.

[0052] The thermal conductivity of the silicon nitride ceramic material prepared in Example 1 is 95.50W·m -1 ·K -1 , the three-point flexural strength is 834±24MPa, and the fracture toughness is 8.77±0.21MPa m 1 / 2 .

Embodiment 2

[0054] With 1mol% Y 2 o 3 and 4mol% MgSiN 2 As a sintering aid, with 95mol% α-Si 3 N 4 Powder, add 1wt% Si, mix by ball mill, sieve after drying to obtain uniformly mixed powder; then dry press molding under 30MPa pressure, and then carry out cold isostatic pressing treatment under 250MPa pressure; the obtained billet The body was put into a BN crucible, held at 1200 °C for 8 h under flowing Ar for deoxidation pretreatment; then sintered under pressure at 1900 °C, where the heating rate was 10 °C / min, N 2 The pressure is 2MPa, and the holding time is 12h; after sintering, cool to 1000°C at a cooling rate of 15°C / min, and then cool to room temperature with the furnace.

[0055] The thermal conductivity of the silicon nitride ceramic material prepared in Example 2 is 118.75W·m -1 ·K -1 , the three-point bending strength is 785±11MPa, and the fracture toughness is 9.98±0.27MPa m 1 / 2 .

Embodiment 3

[0057] With 2mol% Yb 2 o 3 and 8mol% MgO as a sintering aid, and 90mol% α-Si 3 N 4 Powder, add 4wt% Si, mix by ball mill, sieve after drying to obtain uniformly mixed powder; then dry press molding under 40MPa pressure, and then carry out cold isostatic pressing under 200MPa pressure; the obtained billet The body was placed in a BN crucible, and deoxidized pretreatment was carried out at 1400 °C for 6 h under flowing Ar; then it was sintered at 1900 °C under pressure, with a heating rate of 10 °C / min, N 2 The pressure is 2MPa, and the holding time is 2h; after sintering, cool to 1100°C at a cooling rate of 5°C / min, and then cool to room temperature with the furnace.

[0058] The thermal conductivity of the silicon nitride ceramic material prepared in Example 3 is 89.60W m -1 ·K -1 , the three-point flexural strength is 856±17MPa, and the fracture toughness is 7.91±0.17MPa m 1 / 2 .

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Abstract

The invention relates to a silicothermic reduction method for improving thermal conductivity and mechanical properties of a silicon nitride ceramic substrate material. The method comprises the following steps: (1) mixing silicon nitride powder, a sintering aid and silicon powder which is elemental Si and accounts for 0.1-5wt% of the mass of the silicon nitride powder to obtain mixed powder; (2) carrying out compression molding on the obtained mixed powder to obtain a silicon nitride ceramic biscuit; (3) placing the obtained silicon nitride ceramic biscuit in a vacuum atmosphere or an argon atmosphere, and carrying out presintering treatment at 1000-1400 DEG C to obtain a silicon nitride green body; and (4) sintering the obtained pre-sintered silicon nitride green body at the temperature of1800-2000 DEG C to obtain the silicon nitride ceramic substrate material.

Description

technical field [0001] The invention relates to a silicon thermal reduction method for improving the thermal conductivity and mechanical properties of a silicon nitride ceramic substrate material, in particular to a silicon nitride ceramic material with high thermal conductivity and high strength and a preparation method thereof, belonging to inorganic non-metallic materials field. Background technique [0002] Silicon nitride (Si 3 N 4 ) As a structural ceramic, it has excellent mechanical properties, wear resistance, corrosion resistance, thermal shock resistance, and good electrical insulation performance. It is widely used in aerospace, chemical industry, nuclear energy, machinery and other fields. In 1995, Haggerty et al. (J.Haggerty and A.Lightfoot Opportunities for enhancing the thermalconductivities of SiC and Si 3 N 4 β-Si 3 N 4 Theoretical thermal conductivity can reach 200~320W·m -1 ·K -1 , which shows that the application of silicon nitride ceramics to h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/584C04B35/622C04B35/64
CPCC04B35/584C04B35/622C04B35/64C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/658C04B2235/96C04B2235/9607
Inventor 曾宇平王为得左开慧夏咏锋姚冬旭尹金伟梁汉琴
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI