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Method of manufacturing sub-micron trapezoid silicon nitride magnesium polycrystal ceramic powder

A silicon magnesium nitride, sub-micron-level technology, applied in the field of ceramic material preparation, can solve the problems of high temperature requirements, large resource consumption, etc., and achieve the effects of reduced energy consumption, lower preparation temperature, and irregular shape

Inactive Publication Date: 2011-03-23
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned existing processes have high requirements on temperature and consume a lot of resources

Method used

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  • Method of manufacturing sub-micron trapezoid silicon nitride magnesium polycrystal ceramic powder
  • Method of manufacturing sub-micron trapezoid silicon nitride magnesium polycrystal ceramic powder
  • Method of manufacturing sub-micron trapezoid silicon nitride magnesium polycrystal ceramic powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 2.65 grams [Mg 2 Si] and 4.50 g NaN 3 (Si:Mg:NaN 3 =1:2:1.98) into a stainless steel reaction kettle with a volume of 20ml, cover the reaction kettle and tighten it, seal it and put it into a well-type crucible boiler, react at a constant temperature of 600°C for 6 hours, and after natural cooling, the products are sequentially used without Water ethanol, dilute hydrochloric acid (0.1M) and distilled water were ultrasonically washed for 5-20 minutes to remove impurities such as alkali metals and their oxides and soluble by-products. After centrifugation, they were dried in a vacuum oven at 80°C for 24 hours to obtain 2.13 grams of off-white powder. After structure, microstructure, composition and morphology analysis, it is proved that the product is a relatively pure random orthorhombic silicon magnesium nitride polycrystalline powder, and its morphology and size are shown in the appendix figure 2 .

Embodiment 2

[0030] Take 2.82 grams of SiO 2 , 3.07 grams of Mg and 3.18 grams of NaN 3 (Si:Mg:NaN 3 =1:2.72:1.04) into a stainless steel reaction kettle with a volume of 20ml, cover the reaction kettle and tighten it, seal it and put it in a well-type crucible boiler, react at a constant temperature of 500°C for 12 hours, after natural cooling, the products are sequentially used with Wash with water ethanol, dilute hydrochloric acid (0.1M) and distilled water ultrasonically for 5-20 minutes to remove impurities such as alkali metals and their oxides and soluble by-products. After centrifugation, dry in a vacuum oven at 80°C for 24 hours to obtain 2.04 grams of off-white powder. After structure, microstructure, composition and morphology analysis, it is proved that the product is relatively pure random orthorhombic silicon magnesium nitride polycrystalline powder.

Embodiment 3

[0032] Take 0.90 g Si, 0.86 g Mg and 3.00 g NaN 3 (Si:Mg:NaN3=1:1.11:1.44) into a stainless steel reaction kettle with a volume of 20ml, cover and tighten the reaction kettle, seal it and put it in a well-type crucible boiler, react at a constant temperature of 600°C for 12 hours, and cool naturally Finally, the product was ultrasonically washed with absolute ethanol, dilute hydrochloric acid (0.1M) and distilled water for 5-20 minutes to remove impurities such as alkali metals and their oxides and soluble by-products. Drying for 24 hours yielded 2.43 g of off-white powder. After structure, microstructure, composition and morphology analysis, it is proved that the product is relatively pure random orthorhombic silicon magnesium nitride polycrystalline powder.

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Abstract

The invention relates to a preparation method of submicron-stage rhombic silicon nitride-magnesium polycrystal ceramic powder, and the difference lies in that Si-Mg precursor and sodium azide are carried out with heat sealed reaction; the ratio of reactive Si: Mg: NaN3 equals 1:1 to 2.75:1 to 3.23; the heating temperature is 450-600 DEG C, and the reactive time is 4-12 hours; and product is washed and dried and granular ruleless submicron-stage rhombic silicon nitride magnesium polycrystal ceramic powder is obtained. Compared with the prior art, the preparation method has the advantages as follows: 1) synthesis route of silicon nitride-magnesium is carried out with the growth of submicron polycrystal at the same time, mild reaction conditions are realized, the preparation process is relatively simple, the preparation temperature is especially reduced greatly, and then the energy consumption is reduced greatly; 2) the appearance of the product of MgSiN2 ceramic powder is ruleless, the granularity reaches submicron stage, the distribution is uniform, the degree of crystallization is good, the purity is high, and the size is uniform.

Description

technical field [0001] The invention relates to the field of preparation of ceramic materials, in particular to a preparation method of submicron orthorhombic silicon magnesium nitride polycrystalline ceramic powder. Background technique [0002] MgSiN 2 It has high thermal conductivity, high electrical resistance, relatively good fracture toughness and hardness, oxidation resistance up to 920°C, low dielectric constant, low dielectric loss, and good thermal shock resistance. It is used in various fields, especially in electronics, National defense and aerospace have good applications. Submicron orthorhombic magnesium silicon nitride polycrystalline powder, used in the preparation of high-density integrated circuit substrate materials, β-Si 3 N 4 Rod crystals and luminescent materials have great application prospects. [0003] It is known that there are three methods for synthesizing magnesium silicon nitride, including high-temperature direct nitriding method, carbother...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/58C04B35/626
Inventor 谷云乐王吉林
Owner WUHAN INSTITUTE OF TECHNOLOGY