A high-pressure rapid preparation method of high thermal conductivity and high density silicon nitride material

A technology with high thermal conductivity and compactness, which is applied in the field of bulk structure ceramic materials and device manufacturing, can solve the problems of long time heating, uncontrolled precision, and difficulty in reaching 99%, etc., and can shorten the synthesis time, Simple operation, high thermal conductivity effect

Active Publication Date: 2020-09-18
哈尔滨海毅达超硬材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The manufacturing cost of this method is relatively high, it requires ultra-high temperature conditions, the precision cannot be controlled, and the thermal conductivity is not high, which is 19.4 and 19.8W / (m K); , completed under the condition of 4h, there are too many types of binders, and too many metal impurities and oxygen elements are introduced; the equipment for spark plasma sintering is expensive, and the cost of each sintering is extremely high
In summary, it can be concluded that the process is complicated, and a-Si is mostly used 3 N 4 High temperature phase change or doped β-Si 3 N 4 The seeds are sintered, and then high-temperature nitriding treatment is carried out after sintering; ultra-high temperature is required, 1650-2000°C; it takes a long time to heat up, and the sintering time usually takes several hours to make a bulk material; at the same time, the compactness is not high. High (95-98%), it is difficult to reach more than 99%, the thermal conductivity is usually around 17.59–35W / (m K), and the cost of sintered materials in individual methods is relatively high

Method used

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  • A high-pressure rapid preparation method of high thermal conductivity and high density silicon nitride material
  • A high-pressure rapid preparation method of high thermal conductivity and high density silicon nitride material

Examples

Experimental program
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Effect test

Embodiment 1

[0019] as attached figure 1 Shown: Select diamond powder with a particle size of 2-4μm, 0.5-1μmβ-Si 3 N 4 Powder is used as raw and auxiliary materials, and the mass parts are: 5 parts and 95 parts respectively. Mix the powder for 1 hour until it is uniform, put 1.6g of mixed powder 1 into a four-column press, put it into a graphite chamber, heat it in a vacuum at 500°C for 1 hour, put it into a heated graphite tube 2, and finally assemble parts 3-6 Put them into the pyrophyllite synthesis block 7 in order, the size of the pyrophyllite synthesis block is 32.5mm×32.5mm×32.5 mm, the diameter of the synthesis cavity is 18mm, and the inner diameter of the graphite tube is 16mm. Carry out high-pressure high-temperature synthesis on a six-sided top press (CS-IV, 6×14000KN), the condition is 4.5GPa, 1400°C, the sintering holding time is 10min, and then slowly cool down to room temperature, and obtain about Φ14mm×3.5mm Si after pressure relief 3 N 4 The material has a thermal cond...

Embodiment 2

[0021] as attached figure 1 Shown: Select MgO and Y with a particle size of 0.5-1 μm 2 o 3 Powder, 0.5-1μm β-Si 3 N 4 Powder is used as raw and auxiliary materials, and the mass parts are: 2 parts, 5 parts and 93 parts respectively. Mix the powder for 1 hour until it is uniform, put 1.6g of mixed powder 1 into a four-column press, put it into a graphite chamber, heat it in vacuum at 500°C for 0.5 hour, put it into a heated graphite tube 2, and finally put the assembled parts 3- 6 put into the pyrophyllite synthesis block 7 in order, the size of the pyrophyllite synthesis block is 32.5mm×32.5mm×32.5mm, the diameter of the synthesis cavity is 18mm, and the inner diameter of the graphite tube is 16mm. Carry out high-pressure high-temperature synthesis on a six-sided top press (CS-IV, 6×14000KN), the condition is 5.5GPa, 1500°C, the sintering holding time is 20min, then slowly cool down to room temperature, and obtain about Φ14mm×3.5mm Si after pressure relief 3 N 4 The mate...

Embodiment 3

[0023] as attached figure 1 Shown: select AlN powder with a particle size of 1 μm, 0.5-1 μm β-Si 3 N 4 Powder is used as raw and auxiliary materials, and the mass parts are: 5 parts and 95 parts respectively. Mix the powder for 1 hour until it is uniform, put 1.6g of mixed powder 1 into a four-column press, put it into a graphite chamber, heat it in vacuum at 500°C for 0.5 hour, put it into a heated graphite tube 2, and finally put the assembled parts 3- 6 put into the pyrophyllite synthesis block 7 in order, the size of the pyrophyllite synthesis block is 32.5mm×32.5mm×32.5 mm, the diameter of the synthesis cavity is 18mm, and the inner diameter of the graphite tube is 16mm. High-pressure high-temperature synthesis was carried out on a six-sided top press (CS-IV, 6×14000KN), the condition was 5GPa, 1480°C, the sintering holding time was 20min, and then the temperature was slowly lowered to room temperature, and Si of about Φ14mm×3.5mm was obtained after pressure relief. 3 ...

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Abstract

The invention relates to a high-pressure fast preparation method of a high-heat-conduction rate and high-compactness silicon nitride material. The method uses a high-temperature high-pressure sintering technology, and comprises the following concrete steps that under the high-pressure and high-temperature conditions (HPHT, 4.5 to 5.5 GPa, 1400 to 1500 DEG C), diamond, graphene, TiN, AlN, MgO, Y2O3powder and the like with the average particle diameter being 0.5 mu m are used as sintering auxiliary agents; silicon nitride (beta-Si3N4) powder with different mass ratios is used as framework materials for preparing high-heat-conduction rate and high-compactness silicon nitride block body materials. According to the method for preparing the high-performance structure material, sintering phasesof beta-Si3N4, diamond, ceramic hard phases and the like are formed through the mixed powder sintering technology of beta-Si3N4 and the auxiliary agents; the sintering body has high heat conduction rate and high compactness (low porosity). The method has the advantages that the operability is high; the process is simple; the ultrahigh temperature is not needed; the structure material synthesis time can be greatly shortened. The material is a novel ceramic material applicable to the fields of aerospace, war industry, electronics and the like.

Description

technical field [0001] The invention belongs to the field of block structure ceramic materials and device manufacturing, in particular to a method for preparing high-quality silicon nitride block ceramic materials with high compactness (low porosity) and high thermal conductivity. Background technique [0002] With the rapid development of my country's aerospace, military, electronics and other fields, the demand for high-power power electronic devices will also increase in the future. In order to adapt to more complex and harsh application conditions, high-power power electronic devices are developing in the direction of high temperature, high frequency, low power consumption, intelligence, modularization, and systematization, which puts more demands on the thermal shock resistance of the entire electronic device. Due to strict requirements, the preparation of high thermal conductivity ceramic substrate materials has become the key to the development of high-power module el...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/596C04B35/593
CPCC04B35/587C04B35/593C04B2235/3206C04B2235/3225C04B2235/3865C04B2235/3886C04B2235/425C04B2235/427C04B2235/5436C04B2235/5445C04B2235/656C04B2235/96C04B2235/9607
Inventor 贾洪声鄂元龙李海波贺雪莲李加琦牛瑞赵兴
Owner 哈尔滨海毅达超硬材料有限公司
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