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Preparation method of single-phase MgSiN2 powder

A powder, single-phase technology, applied in the field of preparation of single-phase magnesium silicon nitride ceramic powder, can solve the problems of ethanol volatilization loss of additives, high combustion reaction temperature, evaporation loss of magnesium powder, etc., to reduce evaporation and reaction speed. The effect of reducing and reducing evaporation loss

Active Publication Date: 2022-05-13
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the combustion reaction temperature is high (>2000°C), which easily leads to the evaporation loss of magnesium powder in the reactant, and it is difficult to prepare single-phase MgSiN. 2 powder
Although it has been reported (CN109775674A), MgSiN was prepared by combustion synthesis by adding urea and ethanol 2 Ceramic powder, but the additive ethanol is easy to volatilize and lose during operation, and there are silicon nitride impurity phases in the product

Method used

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  • Preparation method of single-phase MgSiN2 powder
  • Preparation method of single-phase MgSiN2 powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A single-phase MgSiN 2 The preparation of powder comprises the following steps:

[0016] 1) Take by weighing 17 grams of magnesium powder with a particle size of 1 micron, 33 grams of silicon nitride powder with a particle size of 0.5 micron and α phase content of 90 wt%, and 50 grams of silicon nitride magnesium powder with a particle size of 10 microns, and use roller milling The method mixes evenly to obtain the mixed powder;

[0017] 2) Put the above-mentioned mixed powder in the porous graphite crucible of the combustion synthesis device, and feed the nitrogen-argon mixed gas after vacuuming, the pressure is 10MPa, the volume percentage of nitrogen in the mixed gas is 30%, and the ignition induces self-propagating combustion reaction;

[0018] 4) After the reaction is completed and the temperature is lowered, the product is taken out to obtain the prepared single-phase MgSiN 2 Powder.

[0019] Carry out XRD phase test to the product, such as figure 1 As shown,...

Embodiment 2

[0021] A single-phase MgSiN 2 The preparation of powder comprises the following steps:

[0022] 1) Take by weighing 33 grams of magnesium powder with a particle size of 75 microns, 62 grams of silicon nitride powder with a particle size of 15 microns and α-phase content of 95 wt%, and 5 grams of silicon nitride magnesium powder with a particle size of 0.5 microns, and use roller milling The method mixes evenly to obtain the mixed powder;

[0023] 2) Put the above-mentioned mixed powder in the porous graphite crucible of the combustion synthesis device, and feed the nitrogen-argon mixed gas after vacuuming, the pressure is 1MPa, the volume percentage of nitrogen in the mixed gas is 50%, and the ignition induces self-propagating combustion reaction;

[0024] 4) After the reaction is completed and the temperature is lowered, the product is taken out to obtain the prepared single-phase MgSiN 2 Powder.

[0025] The XRD phase test was carried out on the product, and the analysis...

Embodiment 3

[0027] A single-phase MgSiN 2 The preparation of powder comprises the following steps:

[0028] 1) Take by weighing 25 grams of magnesium powder with a particle size of 45 microns, 48 ​​grams of silicon nitride powder with a particle size of 5 microns and α-phase content of 92 wt%, and 27 grams of silicon nitride magnesium powder with a particle size of 5 microns, and use roller milling The method mixes evenly to obtain the mixed powder;

[0029] 2) Put the above-mentioned mixed powder in the porous graphite crucible of the combustion synthesis device, and feed the nitrogen-argon mixed gas after vacuuming, the pressure is 5MPa, the volume percentage of nitrogen in the mixed gas is 10%, and the ignition induces self-propagating combustion reaction;

[0030] 4) After the reaction is completed and the temperature is lowered, the product is taken out to obtain the prepared single-phase MgSiN 2 Powder.

[0031] The XRD phase test was carried out on the product, and the analysis...

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Abstract

The invention discloses a preparation method of single-phase MgSiN2 powder, which comprises the following steps: uniformly mixing magnesium powder, silicon nitride powder and silicon magnesium nitride powder according to a certain proportion to obtain mixed powder, and inducing the mixed powder to generate self-propagating combustion reaction in a nitrogen-argon mixed atmosphere to obtain the single-phase MgSiN2 ceramic powder. By adopting the silicon magnesium nitride powder and the nitrogen-argon mixed gas, the combustion reaction temperature is reduced, the evaporation loss of magnesium in the reaction process is inhibited, and the single-phase MgSiN2 powder is obtained. The prepared MgSiN2 powder is high in purity, and the preparation method has the technical advantages of being low in energy consumption, short in period, low in cost and the like.

Description

technical field [0001] The invention relates to the technical field of nitride ceramic powder preparation. More specifically, it relates to a method for preparing single-phase magnesium silicon nitride ceramic powder. Background technique [0002] Magnesium silicon nitride (MgSiN 2 ) powder is an ideal sintering aid material for preparing silicon nitride ceramic substrates with high thermal conductivity. Currently, MgSiN 2 There are two methods for preparing ceramic powder, one is high-temperature nitriding method, and the other is combustion synthesis method. The preparation of silicon magnesium nitride by high temperature nitriding method has problems such as long production cycle, high energy consumption, and residual silicon in the product. Combustion synthesis is a low-cost preparation method with short cycle time and low energy consumption. However, the combustion reaction temperature is high (>2000°C), which easily leads to the evaporation loss of magnesium po...

Claims

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Application Information

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IPC IPC(8): C04B35/584C04B35/626C04B35/65
CPCC04B35/591C04B35/62605C04B35/65C04B2235/401
Inventor 贺刚杨增朝王良李江涛
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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