Fluidized bed chemical vapor deposition preparation method of silicon carbide nanoparticle

A chemical vapor deposition, nanoparticle technology, applied in nanotechnology and other directions, can solve the problems of containing other elements, impurities, narrow particle size distribution, etc., to achieve the effect of rich application scope, convenient process operation and simple process flow

Inactive Publication Date: 2016-11-09
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using these methods to synthesize silicon carbide nanoparticles, on the one hand, it is relatively difficult to control the morphology and size of the reaction product, and it is even more challenging to prepare monodisperse silicon carbide nanoparticles with good sphericity, narrow particle size distribution, and adjustable size; On the one hand, the obtained SiC nanoparticles often contain other elemental impurities, and the stoichiometric ratio of SiC cannot be effectively controlled by design.
In addition, some methods require high energy input, which puts high demands on equipment, and cannot achieve mass continuous production of products

Method used

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  • Fluidized bed chemical vapor deposition preparation method of silicon carbide nanoparticle
  • Fluidized bed chemical vapor deposition preparation method of silicon carbide nanoparticle
  • Fluidized bed chemical vapor deposition preparation method of silicon carbide nanoparticle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The precursor, hexamethyldisilane, was heated to 80° C. by means of a water bath, and argon was used as the carrier gas, the flow rate of the carrier gas was 0.3 L / min, and the mixed gas of hydrogen and argon was used as the fluidizing gas, and H 2 The flow rate of Ar is 1.2L / min, and the flow rate of Ar is 1.5L / min. The fluidized bed reactor was heated to 900°C, zirconia fluidized particles were added and the carrier gas was introduced, and the powder was collected by the powder collection system at the top of the reactor. The obtained powder was heat-treated in an argon atmosphere at 1300°C for 1 hour.

[0034] The transmission electron microscope photo of the obtained product is as figure 1 It can be seen that the obtained product is monodisperse spherical particles, the particle size distribution is very narrow, the average particle size of the product is 120 nm, and the XRD spectrum of the product is as follows figure 2 As shown, by comparing the standard card, ...

Embodiment 2

[0036] The precursor, hexamethyldisilane, was heated to 80°C by means of a water bath, and argon was used as the carrier gas. 2 The flow rate of Ar is 1.5L / min, and the flow rate of Ar is 0.9L / min. The fluidized bed reactor was heated to 900°C, zirconia fluidized particles were added and the carrier gas was introduced, and the powder was collected by the powder collection system at the top of the reactor. The obtained powder was heat-treated in an argon atmosphere at 1300°C for 1 hour.

[0037] The transmission electron microscope photo of the obtained product is as image 3 As shown, it can be seen that the obtained product is monodisperse spherical particles, and the average particle size of the product is 15 nanometers. The XRD test of the product shows that the standard card product is cubic phase silicon carbide, and there is no other impurity phase.

Embodiment 3

[0039] The precursor, hexamethyldisilane, was heated to 100°C by means of electric heating, using hydrogen as the carrier gas, the flow rate of the carrier gas was 2.0L / min, and the mixed gas of hydrogen and argon was used as the fluidizing gas, H 2 The flow rate of Ar is 1.0L / min, and the flow rate of Ar is 1.5L / min. The fluidized bed reactor was heated to 800°C, the metal cobalt fluidized particles were added and the carrier gas was introduced, and the powder was collected by the powder collection system at the top of the reactor. The obtained powder was heat-treated in an argon atmosphere at 1400°C for 2 hours.

[0040] The obtained product is a monodisperse spherical particle with a narrow particle size distribution. The average particle size of the product is 280 nanometers. The product is tested by XRD. By comparing with the standard card product, the product is cubic phase silicon carbide, and there is no other impurity phase.

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Abstract

The invention relates to a fluidized bed chemical vapor deposition preparation method of silicon carbide nanoparticles. The fluidized bed chemical vapor deposition preparation method comprises the following steps: by using a fluidized bed chemical vapor deposition method, heating a precursor material hexamethyl disilane to generate vapor, and feeding the vapor into a fluidized bed reactor in a gas carrying manner; implementing pyrolytic reaction on the precursor vapor in a high-temperature zone so as to form silicon carbide nanoparticles; conveying the nanoparticles to the upper part of the fluidized bed reactor under the action of a fluidization gas, sucking out by using a negative-pressure device, and collecting so as to obtain silicon carbide nano powder; in the presence of an inert atmosphere, implementing high-temperature thermal treatment, thereby obtaining well-crystallized silicon carbide nanoparticles. The silicon carbide nanoparticles are cubic-phase silicon carbide, are sphere-shaped and are narrow in particle size distribution, and the sizes of the particles are 5-300 nanometers and are adjustable. By adjusting the reaction atmosphere, particles of pure silicon carbide and silicon-enriched or carbon-enriched silicon carbide can be prepared. The fluidized bed chemical vapor deposition preparation method is simple in process procedure, convenient and rapid in process operation, low in cost and beneficial to industrial production.

Description

technical field [0001] The invention relates to the technical field of silicon carbide material preparation, in particular to a method for preparing silicon carbide nanoparticles by fluidized bed chemical vapor deposition. Background technique [0002] Silicon carbide is widely used as high-temperature structural components and new sub-components due to its wide electronic band gap, excellent high-temperature mechanical properties, low thermal expansion coefficient, high thermal conductivity, and radiation resistance, corrosion resistance, and oxidation resistance. In aerospace, chemical, energy, electronics and other fields. By reducing the particle size of SiC nanomaterials to the nanoscale, due to the size effect, SiC materials will exhibit many novel properties different from those of bulk materials, further broadening their application fields. Silicon carbide particles with nano-size also show excellent high-temperature sintering performance, overcome the difficulty of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/36B82Y40/00
CPCC01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/62C01P2004/64
Inventor 刘荣正刘马林邵友林常家兴刘兵唐亚平
Owner TSINGHUA UNIV
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