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Silicon nitride powder based on catalytic nitridation and preparation method thereof

A technology of silicon nitride powder and silicon powder, which is applied in the field of silicon nitride powder based on catalytic nitriding and its preparation, can solve the problem of restricting the application and industrial production of silicon nitride powder, and the powder is not in the form of whiskers , complex process and other issues, to achieve the effect of easy control, high production cost, and simple synthesis process

Active Publication Date: 2015-01-07
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In short, the existing silicon nitride powder preparation technology has some disadvantages: high cost, high reaction temperature, long nitriding cycle, low purity, complicated process, difficult to control, powder not in whisker shape, etc. Limits the application and industrial production of silicon nitride powder

Method used

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  • Silicon nitride powder based on catalytic nitridation and preparation method thereof
  • Silicon nitride powder based on catalytic nitridation and preparation method thereof

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Experimental program
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Embodiment 1

[0032] A silicon nitride powder based on catalytic nitriding and a preparation method thereof. The steps of the preparation method are:

[0033] Step 1. According to the mass ratio of polyvinyl alcohol: silicon powder: distilled water is 1: 200: (10000 ~ 12000), mix polyvinyl alcohol, silicon powder and distilled water, stir for 20 ~ 30 minutes, and then ultrasonically disperse for 20 ~ 30 minutes to prepare to obtain a suspension.

[0034] Step 2, adding concentration to the suspension is the chromium nitrate of 0.88mol / L, makes mixed solution; Wherein, the addition of chromium nitrate is Si: Cr 2 o 3 The mass ratio of is 1: (0.005~0.020).

[0035] Step 3: Add urea to the mixed liquid under stirring condition until the pH value is 7.5-8.5, continue stirring for 0.5-1 h; filter with suction, and dry in vacuum for 10-12 h to obtain a mixed powder.

[0036] Step 4: Put the mixed powder in a tube-type atmosphere furnace, raise the temperature to 1250-1300°C under the conditio...

Embodiment 2

[0038] A silicon nitride powder based on catalytic nitriding and a preparation method thereof. The steps of the preparation method are:

[0039] Step 1. According to the mass ratio of sodium dodecylbenzenesulfonate: silicon powder: distilled water is 1: 200: (14000~16000), mix sodium dodecylbenzenesulfonate, silicon powder and distilled water, and stir for 20~ 30min, and then ultrasonically dispersed for 20~30min to obtain a suspension.

[0040] Step 2, adding concentration to the suspension is chromium chloride of 0.88mol / L to obtain a mixed liquor; wherein, the addition of chromium chloride is Si:Cr 2 o 3 The mass ratio of is 1: (0.025~0.040).

[0041] Step 3: Add ammonia water to the mixed liquid under stirring condition until the pH value is 7.5-8.5, continue stirring for 0.5-1 h; filter with suction, and dry in vacuum for 10-12 h to obtain a mixed powder.

[0042] Step 4: Put the mixed powder in a tube-type atmosphere furnace, raise the temperature to 1350-1400°C unde...

Embodiment 3

[0044] A silicon nitride powder based on catalytic nitriding and a preparation method thereof. The steps of the preparation method are:

[0045] Step 1. According to the mass ratio of polyvinyl alcohol: silicon powder: distilled water is 1: 200: (10000 ~ 12000), mix polyvinyl alcohol, silicon powder and distilled water, stir for 20 ~ 30 minutes, and then ultrasonically disperse for 20 ~ 30 minutes to prepare to obtain a suspension.

[0046] Step 2, adding concentration to the suspension is chromium chloride of 0.88mol / L to obtain a mixed liquor; wherein, the addition of chromium chloride is Si:Cr 2 o 3 The mass ratio of is 1: (0.010~0.025).

[0047] Step 3: Add hydrazine hydrate to the mixed liquid under stirring conditions until the pH value is 7.5-8.5, and continue stirring for 0.5-1 h; filter with suction and dry in vacuum for 10-12 h to obtain a mixed powder.

[0048] Step 4: Put the mixed powder in a tubular atmosphere furnace, raise the temperature to 1300~1350°C under...

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Abstract

The invention relates to a silicon nitride powder based on catalytic nitridation and a preparation method thereof. The technical scheme is as follows: the method comprises the following steps: mixing a dispersing agent, silicon powder and distilled water in a mass ratio of 1:200:(10000-16000), stirring, and carrying out ultrasonic dispersion to obtain a suspension; adding 0.88 mol / L water-soluble chromium salt into the suspension according to the Si:Cr2O3 mass ratio of 1:(0.005-0.050) to obtain a mixed solution; adding a precipitant into the mixed solution until the pH value is 7.5-8.5, and stirring for 0.5-1 hour; carrying out vacuum filtration and vacuum drying to obtain a powder mixture; and putting the powder mixture into a tubular atmosphere furnace, heating to 1250-1400 DEG C in a nitrogen atmosphere, and keeping the temperature for 2-8 hours to obtain the silicon nitride powder based on catalytic nitridation. The method has the characteristics of low synthesis temperature, short period, simple technique and high yield, and is easy to control. The silicon nitride powder based on catalytic nitridation has the advantages of high purity and small particle size, and is partially crystal whiskers.

Description

technical field [0001] The invention belongs to the field of nitride powder technology. Specifically relates to a silicon nitride powder based on catalytic nitriding and a preparation method thereof. Background technique [0002] As a high-temperature structural ceramic, silicon nitride ceramics have excellent characteristics such as high strength, high hardness, small high-temperature creep, good thermal shock resistance, wear resistance, corrosion resistance, and good chemical stability. They are widely used in machinery, Chemical, thermal and aerospace fields. Silicon nitride powder is the basis for preparing high-performance silicon nitride ceramics. The preparation and properties of silicon nitride powder play a decisive role in the preparation of silicon nitride ceramics. [0003] At present, the preparation methods of silicon nitride powder mainly include: carbothermal reduction of silicon dioxide method, self-propagating method, thermal decomposition method, gas ph...

Claims

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Application Information

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IPC IPC(8): C01B21/068
Inventor 张海军邓先功张少伟李发亮鲁礼林
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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