Preparation method of silicon carbide nanometer crystal whiskers

A technology of nano-whiskers and silicon carbide, which is applied in the field of preparation of silicon carbide nano-whiskers, can solve the problems of harsh reaction conditions, high toxicity and corrosion, and limited applications, and achieve the effect of high purity

Inactive Publication Date: 2016-02-17
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, no matter which method is used to prepare silicon carbide whiskers, different types of catalysts are used, and the addition of these catalysts greatly affects the purity of silicon carbide whiskers, which limits its wider application.
Wen Guangwu et al. used silicon tetrachloride (SiC1 4 ), benzaldehyde (PhCHO), alkylamine (RNH 2 ) and boron trichloride (BCI 3 ) as raw materials, a large number of β-SiC nano whiskers with good crystallinity were prepared on the surface of the material by the gas pressure synthesis method without using a catalyst (Wen Guangwu et al. Growth of β-SiC nanowires from SiBONC ceramic powder. Rare metal Materials and Engineering, 2008, 37 (3): 561-564), the diameter of the prepared silicon carbide nano whiskers is 20~200nm, and the average length is about 1mm, but the raw materials used in the gas pressure synthesis method have great toxicity and corrosion nature, and the reaction conditions are relatively harsh, and the preparation cost of β-SiC nano whiskers is relatively high

Method used

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  • Preparation method of silicon carbide nanometer crystal whiskers
  • Preparation method of silicon carbide nanometer crystal whiskers
  • Preparation method of silicon carbide nanometer crystal whiskers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Step 1. Preparation of silicon-doped pitch

[0034] According to the solid-liquid mass ratio of 1: (1~3), dissolve the pulverized asphalt in an organic solvent, let it stand for 6~8 hours, filter, and distill the filtered filtrate at 120~150°C to obtain asphalt Organic solvent soluble components.

[0035] Mix 10~20wt% organic silicon with 80~90wt% asphalt organic solvent soluble components to obtain asphalt mixture, and then dissolve the asphalt mixture in organic solvent according to the solid-liquid mass ratio of 1:(1~3) , and stirred for 2-3 hours to obtain a mixture of asphalt organic solvent-soluble components.

[0036] Move the mixture of asphalt organic solvent-soluble components to the reaction kettle, and raise the temperature to 250-300°C at a rate of 2-10°C / min under an inert atmosphere and stirring conditions, and keep it warm for 2-3 hours; then stop Stir and cool naturally in an inert atmosphere to obtain silicon-doped pitch.

[0037] Step 2. Preparatio...

Embodiment 2

[0044] Step 1. Preparation of silicon-doped pitch

[0045] According to the solid-liquid mass ratio of 1: (1~3), dissolve the pulverized asphalt in an organic solvent, let it stand for 6~8 hours, filter, and distill the filtered filtrate at 120~150°C to obtain asphalt Organic solvent soluble components.

[0046] Mix 20~30wt% organic silicon with 70~80wt% asphalt organic solvent soluble components to obtain asphalt mixture, and then dissolve the asphalt mixture in organic solvent according to the solid-liquid mass ratio of 1:(1~3) , and stirred for 2-3 hours to obtain a mixture of asphalt organic solvent-soluble components.

[0047]Move the mixture of asphalt organic solvent soluble components into the reaction kettle, raise the temperature to 300~350℃ at a rate of 2~10℃ / min under inert atmosphere and stirring condition, keep it warm for 3~4h; then stop Stir and cool naturally in an inert atmosphere to obtain silicon-doped pitch.

[0048] Step 2. Preparation of silicon-doped...

Embodiment 3

[0055] Step 1, preparation of silicon-doped resin

[0056] According to the solid-liquid mass ratio of 1: (1~3), dissolve the pulverized resin in an organic solvent, let it stand for 6~8 hours, filter, and distill the filtered filtrate at 120~150°C to obtain the resin Organic solvent soluble components.

[0057] Mix 30~40wt% silicone with 60~70wt% resin organic solvent soluble components to obtain a resin mixture, and then dissolve the resin mixture in an organic solvent according to the solid-to-liquid mass ratio of 1:(1~3) , and stirred for 2 to 3 hours to obtain a mixed solution of resin organic solvent soluble components.

[0058] Move the mixed liquid of the organic solvent-soluble components of the resin to the reaction kettle, raise the temperature to 350-400°C at a rate of 2-10°C / min under an inert atmosphere and stirring conditions, and keep it warm for 4-5h; then stop Stirring and natural cooling in an inert atmosphere yields a silicon-doped resin.

[0059] Step 2...

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Abstract

The invention discloses a preparation method of silicon carbide nanometer crystal whiskers. According to the technical scheme, 10 wt%-40 wt% of organosilicone and 60 wt%-90 wt% of pitch organic solvent soluble components or resin organic solvent soluble components, co-cracking is conducted on an obtained solution for 2-6 h on the condition that the temperature ranges from 250 DEG C to 450 DEG C, and silicon-doped pitch or silicon-doped resin is obtained; carbonization is conducted on the silicon-doped pitch or the silicon-doped resin for 1-3 h on the conduction that the temperature ranges from 700 DEG C to 900 DEG C, and silicon-doped pitch-based carbon materials or silicon-doped resin-based carbon materials are obtained. The silicon-doped pitch-based carbon materials or the silicon-doped resin-based carbon materials are ground into fine powder and filled into a mold, mechanical pressing is conducted, and demoulding is conducted; a graphite crucible filled with a green body is put into a high-temperature carbonization furnace, heat treatment is conducted for 1-3 h at the temperature ranging from 1200 DEG C to 1800 DEG C in an inert atmosphere, natural cooling is conducted, and the silicon carbide nanometer crystal whiskers are obtained. According to the preparation method of the silicon carbide nanometer crystal whiskers, a catalyst does not need to participate, and the prepared silicon carbide nanometer crystal whiskers have the advantages of being high in purity, large in length-diameter radio and easy to collect.

Description

technical field [0001] The invention belongs to the technical field of silicon carbide nanomaterials. In particular, it relates to a preparation method of silicon carbide nano-whiskers. Background technique [0002] Silicon carbide whiskers (SiC w ) is a high-purity single-crystal material with diameters ranging from nanometers to micrometers, with high melting point (>2700°C), low density, excellent tensile strength (tensile strength is 2100MPa), and good specific strength and specific elastic modulus It is widely used as a reinforcing and toughening additive for various high-performance materials, and is used in aerospace, national defense and civil industries (Ning Shufan. Preparation method and application of SiC whiskers. Journal of Xi'an Shiyou University, 2004 , 19(1)). [0003] At present, all SiC whisker preparation processes mainly include two types: gas phase reaction method and solid material method, (Hao Bin. Research progress on SiC whisker preparation me...

Claims

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Application Information

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IPC IPC(8): C01B31/36
CPCC01P2002/72C01P2002/85C01P2004/03C01P2004/10
Inventor 董志军李轩科张旭袁观明丛野
Owner WUHAN UNIV OF SCI & TECH
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