Temperature-controlling activated self-spreading combustion process of synthesizing alpha-phase SiN powder

A self-propagating combustion, phase silicon nitride powder technology, used in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of complex induced reaction methods, long production cycles, and many processes, and meet the requirements of reducing equipment. , the effect of saving energy and improving the safety factor of production

Inactive Publication Date: 2007-03-28
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the disadvantages of the prior art, such as numerous procedures, long production cycle, complex induced reaction mode, large energy consumption and high cost, and provide a temperature-controlled activated automatic Method for Synthesizing α-phase Silicon Nitride Powder by Spreading Combustion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Si powder with an average particle size of 0.1 μm, Si with an average particle size of 0.5 μm 3 N 4 Powder (alpha phase content about 90wt%) and NH 4 F, take samples according to the weight ratio of 50:28:22, put them into the ball milling tank of the vibrating ball mill and mill them for 9 hours to fully mix and activate them; place the mixed and activated materials in a porous graphite crucible to make loose Packing density is about 1.0~2.4g / cm 3 , place a spiral tungsten wire on the upper layer of the material, the diameter of the tungsten wire is 0.5mm, and put them together into the combustion synthesis reactor; after vacuuming, fill high-purity nitrogen from the bottom of the reactor until the nitrogen pressure reaches 8MPa ;Through the spiral tungsten wire with a pulse current to make it generate heat and induce the combustion of the raw material powder. After the combustion reaction lasts for 15 minutes, it is cooled to room temperature, and then the high-pres...

Embodiment 2

[0037] Si powder with an average particle size of 5 μm, Si with an average particle size of 20 nm 3 N 4 Powder (alpha phase content about 90wt%), NH 4 F and NH 4 Cl, sampled by weight ratio 45:36:8:11, first weigh the Si powder and Si 3 N 4 After mixing, put it in an oven, dry it at 100°C for 1.5 hours, take it out and add the weighed NH 4 F and NH 4 Cl, put together in the ball mill jar of planetary ball mill and ball mill for 5 hours to make it fully mixed and activated, the amorphous phase content is not less than 5wt%; the mixed material is placed in a porous graphite crucible so that the bulk density is about 1.0~2.4g / cm 3 , put a spiral tungsten wire on the upper layer of the material, and put them together into the combustion synthesis reactor; after vacuuming, fill the ammonia gas from the bottom to 0.1MPa, and then fill it with high-purity nitrogen until the pressure in the reactor reaches 7.5MPa ;Through the spiral tungsten wire with a pulse current of 12A to ...

Embodiment 3

[0039] Si powder with an average particle size of 0.5 μm, Si with an average particle size of 78 μm 3 N 4 Powder (alpha phase content about 90wt%) and NH 4 Cl, sampled according to the weight ratio of 89:6:5, put into the ball milling tank of the planetary ball mill, ball mill for 4.5 hours, make it fully mixed and activated, the amorphous phase content is not less than 5wt%; put the mixed and activated material In a porous graphite crucible, the bulk density is about 1.0-2.4g / cm 3 , place a helical tungsten wire on the upper layer of the material, the diameter of the tungsten wire is 0.5mm, and put them together into the combustion synthesis reactor; after vacuuming, first fill with ammonia to 0.5MPa, and then fill with high-purity nitrogen , until the pressure in the reactor reaches 3MPa; pass the spiral tungsten wire with a pulse current of 12A to make it generate heat and induce the combustion of the raw material powder. After the combustion reaction lasts for 28 minutes...

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Abstract

The present invention belongs to the field of inorganic non-metal material, and is one kind temperature-controlling activated self-spreading combustion process of synthesizing alpha-SiN powder. Silicon powder in 40-94 weight portions, SiN diluent in 6-60 weight portions and catalyst in 0.5-30 weight portions are first mixed and grinding activated, and then filled into reactor, where the reactant system is induced to produce self-spreading combustion reaction in 3-9 Mpa nitrogen atmosphere to obtain alpha-SiN powder. The method of the present invention has the advantages of no need of material pre-treatment, simple process, short production period, simple reaction initiation, low power consumption, low cost, high alpha phase content in the product, etc.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and relates to a method for synthesizing α-phase silicon nitride powder through temperature-controlled activation and self-propagating combustion. Background technique [0002] Silicon nitride ceramics have unique physical and mechanical properties, such as high hardness, high strength, wear resistance, excellent thermal stability (especially low thermal expansion coefficient), good chemical stability, low friction coefficient, low density and High thermal conductivity, etc., so silicon nitride ceramic materials and devices are widely used in many fields such as engine manufacturing, chemical industry, and semiconductor industry. However, the high cost of raw materials has restricted the large-scale application of silicon nitride ceramic parts in various fields. Therefore, the international material community has been committed to developing new low-cost method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/068C04B35/622C04B35/584
Inventor 林志明贾楠杨筠方侃宋广智封凌萍李江涛景满德祁太元王生渊
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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