Boron-carbon-nitrogen material phase regulated dissolvent heat constant pressure synthesis method

A synthesis method, boron-carbon-nitrogen technology, applied in the direction of nitrogen compounds, chemical instruments and methods, nitrogen and non-metallic compounds, etc., can solve problems such as difficult preparation conditions, lower product application value, and damage the selectivity of the reaction process, to achieve High application value, realization of low-cost mass synthesis, and the effect of enlarging the scale of preparation

Inactive Publication Date: 2006-07-19
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have their own limitations: for example, in addition to controlling the reaction temperature, it is almost impossible for us to control other influencing factors in the reactor, so it is difficult to quickly optimize the preparation conditions to achieve low yield of the two materials. cost mass s...

Method used

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  • Boron-carbon-nitrogen material phase regulated dissolvent heat constant pressure synthesis method
  • Boron-carbon-nitrogen material phase regulated dissolvent heat constant pressure synthesis method
  • Boron-carbon-nitrogen material phase regulated dissolvent heat constant pressure synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: firstly add metal sodium flakes into benzene, and distill after standing for 24 hours to remove water and oxygen therein. Then under the protection of nitrogen, weigh the stoichiometric ratio of sodium azide (NaN 3 ) and trichloroazine (C 3 N 3 Cl 3 ) into the autoclave, then add 8ml of dried benzene and then seal it. Apply a pressure of 40 MPa on the autoclave, then control the temperature of the autoclave to rise to 220 °C at a rate of 0.01 °C / min, react at constant temperature and pressure for 8 hours, and then naturally cool to room temperature.

[0041] After the reaction, the benzene was first filtered off with suction, and then the product was washed with acetone, ethanol, and dilute hydrochloric acid in sequence to remove organic by-products and other impurities, and then the product was repeatedly washed with deionized water until the filtrate was neutral. Heating the product in vacuum to 60°C for drying can obtain graphite carbon nitride (g-C 3...

Embodiment 2

[0042] Example 2: As described in Example 1, the difference is that the reaction temperature is increased to 260°C.

Embodiment 3

[0043] Embodiment 3: As described in Embodiment 1, the difference is that the reaction temperature of the autoclave is increased to 300° C., trichloroazine is replaced by trimethylamine, and sodium azide is replaced by nitrogen trichloride.

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Abstract

The solvent thermal constant-pressure synthesis method to adjust and control phase of boron carbonitride material comprises: preparing liquids for boron resource, carbon source and nitrogen source respectively; putting into the kettle; forcing 40~2000MPa constant pressure then heating the kettle to 220~1000Deg with 0.01~60Deg/min speed; after reaction, cooling to room temperature, and taking post-treatment to the product. Wherein, it can adjust and control the system temperature and pressure independently as well as the reaction speed and direction, and obtains large-size diamond, cubic boron nitride and carbonitride crystal block.

Description

1. Technical field [0001] The invention relates to a solvothermal constant-pressure synthesis method for regulating the phase of boron-carbon-nitrogen materials, which belongs to the field of new chemical materials. 2. Background technology [0002] As superhard materials with excellent performance, cubic boron nitride, diamond, and carbon nitride (collectively referred to as boron carbon nitride) have played and will soon play a pivotal role in daily life and industrial production. The artificial synthesis of these materials, especially Low-cost mass synthesis has always been the dream of human beings. In order to realize this ideal, various preparation methods have been developed and improved, among which the high temperature and high pressure method is the most mature. So far, using this method, the industrialization of cubic boron nitride and diamond has been realized. However, it is not difficult to see from a comprehensive analysis of this method that the preparation...

Claims

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Application Information

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IPC IPC(8): C01B31/06C01B21/064C01B21/082B01J3/06
Inventor 崔得良陆希峰赖泽锋朱玲玲王琪珑蒋民华
Owner SHANDONG UNIV
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