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Method for preparing silicon nitride nanometer rod by using sulfur auxiliary reaction under low temperature

A technology of silicon nitride and nanorods, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of high reaction temperature and inability to obtain crystalline Si, achieve low reaction temperature, strengthen toughness, and realize industrial production Effect

Inactive Publication Date: 2010-06-02
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the deficiencies of the prior art, the present invention proposes a method for preparing silicon nitride nanorods at a relatively low temperature (250-300° C., 23-40 MPa) using sulfur-assisted reactions to overcome the reaction temperature of the prior art. Crystalline Si cannot be obtained at high and low temperatures 3 N 4 Defects of one-dimensional nanomaterials

Method used

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  • Method for preparing silicon nitride nanometer rod by using sulfur auxiliary reaction under low temperature
  • Method for preparing silicon nitride nanometer rod by using sulfur auxiliary reaction under low temperature
  • Method for preparing silicon nitride nanometer rod by using sulfur auxiliary reaction under low temperature

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Embodiment 1

[0027] Example 1: Preparation of α-Si by reaction of silicon powder, sublimed sulfur and sodium azide 3 N 4 nanorod

[0028] Take 1 mmol of silicon powder, 2 mmol of sublimed sulfur and 4 mmol of sodium azide, put them into a stainless steel 20mL reaction kettle, remove the air in the kettle with nitrogen, seal it and place it in a resistance crucible boiler, and heat it at 250°C ( The furnace temperature is controlled at ±5°C) and 23.2MPa for 4-15 hours; 300°C and 25.4MPa for 1-5 hours; 400°C and 30MPa for 0.5-5 hours; after heating is stopped, the reaction The kettle was naturally cooled to room temperature; the kettle was opened, and the resulting product was washed 5 times with 10% hydrochloric acid, then washed with water until the pH was neutral, conventionally centrifuged, and dried to obtain α-Si 3 N 4 Nanorod-based silicon nitride powder products. Vacuum-dried at 60°C for 6 hours to obtain an off-white powder product.

[0029] Cu Kα rays (wavelength λ=1.5418 The ...

Embodiment 2

[0038] Mix silicon powder, sublimed sulfur and sodium azide in a molar ratio of 1:3:6, seal in an autoclave, and react at 250°C and 36MPa for 12 hours; the product is washed 3 times with 5% sulfuric acid, and then washed with water until Neutral pH, routine centrifugation and drying to obtain α-Si 3 N 4 Nanorod-based silicon nitride one-dimensional nanomaterials.

Embodiment 3

[0040] Mix silicon powder, sublimed sulfur and sodium azide in a molar ratio of 1:2.5:5, seal it in an autoclave, and react for 4 hours at 300°C and 32.6MPa; the product is washed 3 times with 5% nitric acid, and then washed with water to neutral pH, conventional centrifugation and drying to obtain α-Si 3 N 4 Nanorod-based silicon nitride one-dimensional nanomaterials.

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Abstract

This invention discloses a method for producing silicon nitride nanometer rod by utilizing sulfur auxiliary reaction at low temperature. In this invention, silicon powder, sublimate sulfur and sodiumazide in molar ration of 1:(2-3):(4-6) are mixed, and sealed in autoclave, under temperature of 250-300 deg.C and 23-40 MPa, reacting for 2-20hrs. The product is proceeded by acid-washing for 3-5 times to neutral pH value, then proceeded are: normal centrifugal separation and drying to obtain the one-D nanometer silicon material containing mainly alpha-Si3N4 nanometer rod. The diameter of thus produced Si3N4 nanometer rod is 70-400 Mu and its length is 300-4000 Mu. The advantages of this invention method are: low cost of raw material silicon powder, lower reaction temperature, excellent shapeof products, suitable for commercial production.

Description

technical field [0001] The invention belongs to the technical field of preparing silicon nitride nanometer materials, and in particular relates to a method for preparing silicon nitride nanorods at low temperature by using high-pressure sulfur-assisted reaction. Background technique [0002] American Journal of Materials Science (JOURNAL OF MATERIALS RESEARCH 15(2): 1048-1051 MAY 2000) reported that silicon nitride nanomaterials have better elasticity and bending strength than ordinary silicon nitride materials. Among many raw materials for silicon nitride production, silicon powder has become one of the most potential raw materials because of its cheapness and environmental protection. Therefore, the use of silicon powder to prepare silicon nitride nanomaterials is of great practical value. [0003] Netherlands "Crystal Growth" (JOURNAL OF CRYSTAL GROWTH 233(4): 803-808 DEC 2001) reported the preparation of amorphous silicon nitride nanocrystals at 1200°C using silicon powd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/068C04B35/584
Inventor 钱逸泰杨立山郭春丽马小健徐立强
Owner SHANDONG UNIV
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