Controllable hydrothermal constant pressure synthesis method for preparation of boron-carbon-nitrogen material

A synthetic method, 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, difficulties in the dissolution and transportation of inorganic substances, and poor solvency , to achieve the effect of good phase purity, inhibition of phase reversal and high solubility

Inactive Publication Date: 2008-11-05
SHANDONG UNIV
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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 synthesis method for preparation of boron-carbon-nitrogen material
  • Controllable hydrothermal constant pressure synthesis method for preparation of boron-carbon-nitrogen material
  • Controllable hydrothermal constant pressure synthesis method for preparation of boron-carbon-nitrogen material

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Experimental program
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Embodiment 1

[0042] Example 1: Firstly, nitrogen gas is bubbled into the deionized water to eliminate dissolved oxygen therein, and then the deionized water is redistilled. Then under the protection of nitrogen, weigh the stoichiometric ratio of sodium azide (NaN 3 ) and carbon tetrabromide (CBr 4 , 1.06 mol / liter) into the autoclave, add 5ml of deionized water after oxygen removal treatment and seal. Apply a pressure of 164.0 MPa on the autoclave, then control the temperature of the autoclave to rise to 300 °C at a rate of 0.93 °C / min, react at constant temperature and pressure for 6 hours and then naturally cool to room temperature.

[0043] After the reaction, filter the deionized water clean, then wash the product successively with acetone and dilute hydrochloric acid to remove organic by-products and other impurities therein, and then repeatedly wash the product with deionized water until the filtrate is neutral. Slowly heat the product in vacuum to 60°C for drying, and carbon nitri...

Embodiment 2

[0044] Embodiment 2: As described in Embodiment 1, the difference is that the protective gas is argon, the carbon source is carbon tetrachloride (content 0.005 mol / liter), 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

[0045] Embodiment 3: As described in Embodiment 1, the difference is that the protective gas is neon, the carbon source is bromoform (content 0.05 mol / liter), the nitrogen source is barium azide, and the reaction temperature is 350 ℃, 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 controllable hydrothermal constant-pressure synthesis method for boron carbonitride material comprises: treating the deionized water, preparing liquids for boron resource, carbon source and nitrogen source respectively; putting into the kettle; forcing 20~2000MPa pressure then heating the kettle to 240~1000Deg with 0.01~60Deg / min speed for reaction 6~480h. Wherein, it can adjust and control the system temperature and pressure independently as well as the reaction speed and direction. All the product of diamond, cubic boron nitride and carbonitride crystal block have wide application.

Description

technical field [0001] The invention relates to a hydrothermal constant-pressure synthesis method for controllably preparing boron, carbon and nitrogen materials, which belongs to the fields of chemical industry and new materials. Background technique [0002] In boron-carbon-nitrogen series compounds, the atoms are separated by sp 3 Cubic boron nitride, diamond and carbon nitride combined by hybridization are not only excellent superhard materials, but also wide-bandgap high-temperature semiconductors with excellent performance. 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. [0003] Due to the existence of natural diamond in nature, its use value has been recognized by people for a long time, and it has been widely used. In contrast, since there is no natural cubic boron nitride, it was not until the succ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/06C01B21/064C01B21/082
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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