Dissolvent hot liquid state phase-change method for synthesizing superhard micro nano material

A micro-nano, solvothermal technology, applied in the process of applying ultra-high pressure, polycrystalline material growth, chemical instruments and methods, etc., can solve the problem that the product is easy to be polluted, the consistency of product performance is deteriorated, and the input-output ratio is high. problems, achieving uniformity and improved isotropy, simplified post-processing, and reduced temperature and pressure

Inactive Publication Date: 2007-02-28
SHANDONG UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

The direct consequence of this phenomenon is that the input-output ratio is too high, and the product price has been high, which limits the application of these superhard materials.
[0004] In addition to the disadvantages of high input and low output caused by the use of extreme conditions, there are also the following disadvantages when using high temperature and high pressure methods to synthesize superhard materials: first, the uniformity of the reaction system is poor, resulting in poor particle size uniformity of the product; second, It is difficult to regulate the average particle size of the product in a wide range, so that the product variety is single, and it is difficult to adapt to the needs of different occasions, especially it is difficult to prepare the urgently needed superhard nanomaterials; thirdly, it is difficult to monitor the parameters of the phase transition process in real time. It leads to poor consistency of product performance; Fourth, excessive temperature and pressure accelerate the diffusion of impurity atoms, and the product is easy to be polluted

Method used

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  • Dissolvent hot liquid state phase-change method for synthesizing superhard micro nano material
  • Dissolvent hot liquid state phase-change method for synthesizing superhard micro nano material
  • Dissolvent hot liquid state phase-change method for synthesizing superhard micro nano material

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Experimental program
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Effect test

Embodiment 1

[0043] Embodiment 1: Firstly add metal sodium flakes in the solvent benzene, and distill after standing for 24 hours to remove the water and oxygen contained in the benzene. Under the protection of high-purity nitrogen, weigh an appropriate amount of hexagonal boron nitride nanopowder (average particle size is 8 nanometers) and grind for 15 to 30 minutes, then disperse it in redistilled benzene to obtain a hexagonal boron nitride content of 19.0 grams / L of suspension. After ultrasonic dispersion, the suspension was put into an autoclave, and the autoclave was sealed. Apply a pressure of 80 MPa on the autoclave, and then control the temperature of the autoclave to rise to 280 °C at a rate of 0.87 °C / min. After 4 hours of constant temperature and pressure, the autoclave is naturally cooled to room temperature.

[0044] After the above-mentioned hot pressing process is completed, the solvent is first filtered off, and then the obtained solid product is redispersed in acetone an...

Embodiment 2

[0045] Example 2: As described in Example 1, the difference is that the hot pressing temperature is 300° C., the heating rate is 0.93° C. / minute, and the hot pressing time is 6 hours. The infrared absorption spectrum of the cubic boron nitride nanocrystal obtained in this way is shown in Figure 1, the selected area electron diffraction diagram is shown in Figure 3, and the transmission electron microscope photo is shown in Figure 5.

Embodiment 3

[0046] Embodiment 3: As described in Embodiment 1, the difference is that the hot pressing temperature is 300° C., the heating rate is 0.93° C. / minute, and the hot pressing pressure is 160 MPa. The selected area electron diffraction pattern of the obtained cubic boron nitride nanocrystal sample is shown in Figure 4, and the microscopic morphology of a single cubic boron nitride grain is shown in Figure 6. The microscopic appearance of the sample is shown in Figure 8.

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Abstract

The invention discloses a solvent hot-liquid phase transforming method to synthesize superhard micro-nanometer material in the chemical and new material domain, which comprises the following steps: dispersing hexagonal boron nitride, graphite mold carbon nitride or graphite powder solid particle in the liquid dielectric organic solvent, proceeding ultrasonic dispersing disposal for suspension liquid, adding fitful addictive to reduce phase-transforming needed temperature and pressure, changing boundary energy condition between solid particle and liquid dielectric, accelerating the solid particle to change to needed material.

Description

technical field [0001] The invention relates to a solvothermal liquid phase transition method for controllably synthesizing superhard micro-nano materials under mild conditions, belonging to the technical fields of chemical industry and new materials. Background technique [0002] Cubic boron nitride and diamond not only have high hardness, but also have excellent thermal conductivity and good stability. In addition, they are also ideal wide-bandgap high-temperature semiconductor materials. It has been widely used in the development of power and short-wavelength semiconductor devices and in the defense industry. On the other hand, theoretical calculations show that: carbon atoms in sp 3 C that is hybridized and bonded to a nitrogen atom 3 N 4 It has a hardness very similar to that of diamond, and has the characteristics of high resistivity, high thermal conductivity and wide energy gap. As with diamond and cubic boron nitride, it is expected that C 3 N 4 The material h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J3/06C01B21/064C01B31/06C30B29/04C30B29/38
Inventor 崔得良赖泽锋朱玲玲赵显王琪珑蒋民华
Owner SHANDONG UNIV
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