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Controllable hydrothermal constant pressure synthesizing method for producing BCN material

A synthetic method and hydrothermal technology, applied in the direction of nitrogen compounds, chemical instruments and methods, nitrogen and non-metallic compounds, etc., can solve the problems of unsatisfactory uniformity of the reaction system, difficulty in dissolving and transporting inorganic substances, and poor solvency , to achieve the effect of good phase purity, inhibition of phase reversal and high solubility

Inactive Publication Date: 2008-07-16
SHANDONG UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these methods also have many disadvantages: the synthesis process is carried out in a closed high-pressure container, once the reaction raw materials and their proportions are determined, the temperature and pressure of the system are related to each other according to a fixed relationship
However, this method has caused the following difficulties due to the use of an organic solvent as a medium: the one is that the organic solvent has poor dissolving power to inorganic substances, so that the uniformity of the reaction system is not ideal enough, which affects the uniformity of the final product. There are certain side effects
The second is that organic solvents are easy to carbonize when the temperature is high, causing certain pollution to the product
The third is that under solvothermal conditions, the dissolution and transportation of inorganic substances are difficult, and it is difficult to grow boron carbon nitrogen bulk crystals with higher application value in this environment

Method used

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  • Controllable hydrothermal constant pressure synthesizing method for producing BCN material
  • Controllable hydrothermal constant pressure synthesizing method for producing BCN material
  • Controllable hydrothermal constant pressure synthesizing method for producing BCN material

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Example 1: Nitrogen gas was first introduced into deionized water for bubbling to eliminate the dissolved oxygen therein, and then the deionized water was redistilled. Then under the protection of nitrogen, weigh out the stoichiometric ratio of sodium azide (NaN 3 ) And carbon tetrabromide (CBr 4 , 1.06 mol / L) was put into the autoclave, and 5ml of deionized water after deoxygenation treatment was added and sealed. A pressure of 164.0 MPa was applied to the autoclave, and then the temperature of the autoclave was controlled to rise to 300°C at a rate of 0.93°C / min. After 6 hours of constant temperature and pressure reaction, it was naturally cooled to room temperature.

[0044] After the reaction, the deionized water is suction filtered, and then the product is washed with acetone and dilute hydrochloric acid successively to remove the organic by-products and other impurities, and then the product is washed with deionized water repeatedly until the filtrate is neutral. Slow...

Embodiment 2

[0045] Example 2: As described in Example 1, the difference is that the protective gas is argon, the carbon source is carbon tetrachloride (content 0.005 mol / l), the nitrogen source is potassium azide, and the reaction temperature is 240°C. The pressure is 20 MPa, the heating rate is 1° C. / min, and the reaction time is 12 hours.

Embodiment 3

[0046] Example 3: As described in Example 1, the difference is that the protective gas is neon, the carbon source is bromoform (content 0.05 mol / l), the nitrogen source is barium azide, the reaction temperature is 350°C, and the pressure is 60MPa, the heating rate is 1.5°C / min, and the reaction time is 15 hours.

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Abstract

The invention relates to a controllable hydrothermal synthetic method of constant pressure for preparing boron carbon nitride material, belonging to a chemical technical field of new material. The method comprises the following processes of treatment of deionized water, preparation of boron source liquid, carbon source liquid and nitride source liquid, and loading a kettle; before an autoclave is heated up, pressure of 20 to 2,000 MPa is added; then the temperature is adjusted and the autoclave is heated up to 240 to 1,000 DEG C at a speed of 0.01 to 60 DEG C / minute, and the reaction is lasted for 6 to 480 hours. When the method is used for synthesizing boron carbon nitride material, the temperature and pressure of the system can be separately modulated, and the reaction speed and direction of the synthesized boron carbon nitride material can be controlled. Diamond, cube boron nitride and carbon nitride crystal can be obtained from the hydrothermal environment of constant pressure. The material has wide application prospect in fields of fine machinery processing, defense industry, drilling and exploitation of petroleum, photoelectronic elements of high temperature, large power and short wavelength.

Description

[0001] This application is a divisional application with the same name of 200610042088.9, and the filing date is January 20, 2006. Technical field [0002] The invention relates to a hydrothermal constant-pressure synthesis method for the controllable preparation of boron carbon nitrogen materials, and belongs to the field of chemicals and new materials. Background technique [0003] In the boron carbon nitrogen series compounds, the atoms are separated by sp 3 The cubic boron nitride, diamond, and carbon nitride formed by the hybrid method are not only excellent superhard materials, but also wide-bandgap high-temperature semiconductors with excellent performance. They are used in daily life, mechanical processing, oil exploration, high temperature and high power It has high application value in the development of short-wavelength semiconductor optoelectronic devices and the defense industry. It is a class of high-tech materials that will have a profound impact on our lives. [00...

Claims

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Application Information

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IPC IPC(8): C01B21/082C01B21/064C01B31/06
Inventor 崔得良赖泽锋陆希峰朱玲玲王琪珑蒋民华
Owner SHANDONG UNIV
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