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Preparation method of high-crystallinity hexagonal boron nitride powder

A boron nitride powder, high crystallinity technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of low crystallinity of h-BN

Inactive Publication Date: 2017-02-22
河北正雍新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention mainly aims at the problem of low crystallinity of h-BN, and provides a preparation method of hexagonal boron nitride powder with high crystallinity

Method used

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  • Preparation method of high-crystallinity hexagonal boron nitride powder
  • Preparation method of high-crystallinity hexagonal boron nitride powder

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Experimental program
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Effect test

Embodiment 1

[0013] The industrial-grade urea is purified to analytical purity by recrystallization, ground to below 200 mesh, and dried before use. The urea after the above treatment is uniformly mixed according to the mass ratio of boric acid and urea at a ratio of 1:0.5, and put into a silicon nitride crucible for nitriding in a nitrogen atmosphere. The specific process parameters are to first raise the temperature to 850°C, hold it for 2 hours, and carry out nitriding, then raise the temperature to 1600°C, hold it for 2 hours, so as to improve the crystallinity. At the end of the final incubation period, two air changes were performed. After grinding the nitrided powder, XRD (X-ray Diffraction, X-ray diffraction) was used to measure the h-BN crystal phase content as 100% ( figure 1 ), so washing and purification are not required. The graphitization index of the sample was calculated to be 5.6. figure 2 Shown is the powder morphology obtained by SEM test, it can be seen that the lam...

Embodiment 2

[0015] The industrial-grade urea is purified to analytical purity by recrystallization, ground to below 200 mesh, and dried before use. The urea after the above treatment is weighed according to the ratio of boric acid to urea mass ratio of 1:4, and after adding 10% sodium azide of the total mass of urea and boric acid, mix evenly, put it into a boron nitride crucible, and in a nitrogen atmosphere Nitriding is carried out. The specific process parameters are to first raise the temperature to 900°C, hold it for 1 hour, and carry out nitriding, then raise the temperature to 2000°C, hold it for 2 hours, so as to improve the crystallinity. At the end of the final incubation period, two air changes were performed. Because there is borax in the raw material, there will be a certain amount of Na in the reaction product 2 O, therefore, after grinding the nitrided powder, wash it twice quickly with deionized water at 30°C, wash it with absolute ethanol, and dry it. The h-BN crystal ...

Embodiment 3

[0017] The industrial-grade urea is purified to analytical purity by recrystallization, ground to below 200 mesh, and dried before use. The urea after the above treatment is uniformly mixed according to the mass ratio of boric acid and urea at a ratio of 1:2, and put into a silicon nitride crucible for nitriding in a nitrogen atmosphere. The specific process parameters are to first raise the temperature to 950°C, hold it for 0.5h, and carry out nitriding, then raise the temperature to 1850°C, and hold it for 2h, so as to increase the crystallinity. At the end of the final incubation period, two air changes were performed. Because there is sodium azide in the raw material, there will be a certain amount of Na in the reaction product 2 O, therefore, after grinding the nitrided powder, wash it twice quickly with deionized water at 30°C, wash it with absolute ethanol, and dry it. The h-BN crystal phase content in the sample was determined to be 100% by XRD. The graphitization i...

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Abstract

The invention provides a preparation method of high-crystallinity hexagonal boron nitride powder. The method is low in cost, simple to operate and suitable for mass production. Certain quantities of boron sources, nitrogen sources and additives are weighed in proportion and evenly mixed through ball milling, the mixture is put into a crucible, heated to about 900 DEG C in a nitrogen atmosphere and kept at the temperature, boron nitride is prepared and heated to 1,600-2,000 DEG C for refinement after complete nitridation, and the crystallinity of boron nitride is increased.

Description

technical field [0001] The invention belongs to the field of powder preparation, in particular to a preparation method of high crystallinity hexagonal boron nitride powder. Background technique [0002] Hexagonal boron nitride is one of the many structural forms of boron nitride. It has a similar structure to graphite and has a white appearance. It has good lubricity, electrical insulation, thermal conductivity, and chemical corrosion resistance. The product is easy to machine. It is a kind of A new type of ceramic material with excellent performance and great development potential has broad application prospects in lubricants, thermal conductivity materials, hydrogen storage materials, ceramics, electrical engineering, catalysis, nuclear industry, electronics, and aerospace. In particular, the properties of h-BN with high crystallinity, such as heat conduction, insulation, lubrication, high temperature resistance and molten metal corrosion resistance, are superior to ordina...

Claims

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Application Information

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IPC IPC(8): C01B21/064
CPCC01B21/064C01P2002/72C01P2004/03C01P2006/80
Inventor 付亚杰张红冉吴诚
Owner 河北正雍新材料科技有限公司
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