Process for preparing nitride ultromicro powder and nitride crystal wunder hydrothermal condition

A nitride, ultrafine powder technology, applied in chemical instruments and methods, nitrogen compounds, nitrogen-metal/silicon/boron binary compounds, etc. There are strict requirements and other problems to achieve the effect of easy monitoring and control, environmental protection, and good uniformity

Inactive Publication Date: 2002-08-21
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods are either highly corrosive and have strict requirements on equipment, or require high temperature and high pressure conditions, and use extremely expensive large precision equipment
On the one hand

Method used

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  • Process for preparing nitride ultromicro powder and nitride crystal wunder hydrothermal condition
  • Process for preparing nitride ultromicro powder and nitride crystal wunder hydrothermal condition
  • Process for preparing nitride ultromicro powder and nitride crystal wunder hydrothermal condition

Examples

Experimental program
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Effect test

Embodiment 2

[0032] First, 120ml of water is added into a conical flask with a capacity of 250ml, and then 3.7g of boric acid (H 3 BO 3 ) into water, stirring while dissolving, and continuously stirring for 10 to 30 minutes to obtain a solution with a concentration of 0.5 mol / liter. With continuous stirring, 2.7 g of ammonium chloride (NH 4 Cl) was added to the boric acid solution obtained above. Then after stirring for 30 minutes, add 1.6g of phosphorus, continue stirring for 2 hours, transfer the uniformly stirred mixed solution to the reactor, then add water to make the filling rate reach 75%, seal the kettle, and heat the reactor to 400°C Keep warm for 10 hours. After the reaction was completed, the product was suction filtered, then washed with deionized water, and suction filtered several times until the filtrate was neutral. The obtained powder is heated and dried at 60° C. in a vacuum to obtain boron nitride micropowder with a particle size of nanometer. Embodiment 3. The thir...

Embodiment 3

[0033] Add 100ml of water into a conical flask with a capacity of 250ml, then dissolve 9.8g of sodium azide into the water, stir while dissolving, and add 3.5g of boron trioxide to the solution obtained above while stirring continuously . Add 1.6g of phosphorus, continue to stir for 2 hours, transfer the uniformly stirred mixed solution to the reactor, add water to make the filling rate reach 60%, seal the reactor, and heat the reactor to 350°C for 10 hours. After the reaction was completed, the product was filtered with deionized water several times until the filtrate was neutral. The powder thus obtained can be heated and dried in a vacuum to obtain boron nitride nanometer powder. Embodiment 4. Preparation four of boron nitride nanometer powder

Embodiment 4

[0034] 150ml of water is added into a 250ml Erlenmeyer flask, then 27g of sodium ammonium hydrogen phosphate is dissolved in water, and stirred while dissolving, and under continuous stirring, 3.5g of boron trioxide is added to the previously obtained solution. Then stir for 10 to 30 minutes, then add 5g of metal zinc powder, continue to stir for 0.5 to 2 hours, then transfer the evenly stirred mixed solution to the reaction kettle, then add water to make the filling rate reach 75%, seal the kettle, and put the reaction The kettle was heated to 450°C for 16 hours. Filter the product with deionized water until the filtrate is neutral. The obtained powder is heated in vacuum at 50-60 DEG C and dried to obtain boron nitride nanometer powder with a particle size of tens of nanometers. Embodiment 5. The fifth of the preparation of boron nitride nanopowder

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Abstract

The present invention relates to the field of nano material and crystal growth technology. The present ivnention features that crystal and superfine powder of boron nitride, gallium nitride, aluminium nitride and indium nitride are prepared through dissolving boron, gallium, aluminium and indium in deionized water, adding metal nitride or ammonia while stirring; adding P, Zn and other reductant; heating at 100-800 deg.c for 10-120 hr and by means of reaction coupling. The present inventino has the advantages of no need of large and expensive instrument and equipment, no need of oxygen-free and water-free condition and capability of obtaining large crystal. The process is low in nitride preparing cost and suitable for large-scale production.

Description

(1) Technical field [0001] The invention relates to a new method for preparing nitride ultrafine powder and bulk crystals under low temperature and low pressure conditions by using a hydrothermal reaction method, and belongs to the technical field of nanometer materials and crystal growth. (2) Background technology [0002] Hexagonal boron nitride nanopowders have attracted widespread attention due to their high thermal conductivity, good chemical stability, excellent lubricating properties and sintering properties. After hexagonal boron nitride nano-powders are added to lubricating oil, they tend to deposit on the defects of the friction surface first, play a role in repairing defects, and can significantly improve the lubrication effect; as a heating container material, hexagonal boron nitride nano-powders can The firing temperature is greatly reduced (the maximum temperature drop can reach 1800°C), and the density and toughness of the container can be significantly improv...

Claims

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Application Information

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IPC IPC(8): C01B21/06C01B21/064C01B21/072
Inventor 郝霄鹏崔得良于美燕徐现刚蒋民华
Owner SHANDONG UNIV
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