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Method for solvent thermal reaction preparation of alpha-Si3N4 monocrystal nano wire

A solvothermal reaction, single crystal nanotechnology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of product impurity and high reaction temperature, achieve low reaction temperature, simple and easy to control reaction, Achieve the effect of industrialized production with large output

Inactive Publication Date: 2008-06-04
UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

[0003] The present invention proposes a method for the preparation of single-phase α-Si by uniform reaction at a relatively low temperature using solvothermal reaction 3 N 4 The method of nano wire powder, to overcome the defects of high reaction temperature and impure product obtained in the prior art

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  • Method for solvent thermal reaction preparation of alpha-Si3N4 monocrystal nano wire
  • Method for solvent thermal reaction preparation of alpha-Si3N4 monocrystal nano wire
  • Method for solvent thermal reaction preparation of alpha-Si3N4 monocrystal nano wire

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Embodiment 1

[0015] Example 1: Preparation of α-Si by reaction of magnesium nitride and silicon tetrachloride 3 N 4 Nanowires

[0016] Take 2 millimoles of magnesium nitride and 5 millimoles of silicon tetrachloride, put them into a stainless steel reaction kettle lined with a hafnium alloy, use nitrogen to remove the air in the kettle, seal them and place them in a resistance crucible boiler, respectively, at 550 ° C , 600°C and 700°C (furnace temperature controlled at ±5°C) for 5-24 hours; after stopping heating, cool the reaction kettle to room temperature naturally; open the kettle and remove unreacted SiCl 4 , the resulting product was washed with acid and water, centrifuged and dried to obtain α-Si 3 N 4 product. Vacuum-dried at 50°C for 6 hours to obtain an off-white powder product.

[0017] Adopt Japan Rikagu DmaxγA X-ray powder diffractometer to take Cu Kα ray (wavelength λ=1.54178 ) is a diffraction light source for X-ray diffraction analysis of the product.

[0018] fig...

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Abstract

The present invention relates to a solvent hot reaction preparation method of alpha -Si3N4 single crystal nanometer wire. The procedure is: mixing SiCl4 and Mg3N2 at mol ratio of 1:1.5-15, sealing in a vessel at 500 -700 degree C, reacting for more than 5 hours, acid washing and water washing the product, followed by centrifugal separating and drying, and then alpha-Si3N4 nanometer wire powders are obtained. The nanometer wire prepared in accordance with the present invention is about 35 nanometers in diameter, several micrometers in length. The reaction temperature of the invention is comparatively low and product phase is single, suitable for mass production.

Description

Technical field: [0001] The invention belongs to the technical field of silicon nitride nanomaterial preparation, in particular to α-Si 3 N 4 Solvothermal reaction preparation method of single crystal nanowires. Background technique: [0002] JOURNAL OF THE AMERICAN CERAMIC SOCIETY 88(3):566-569 MAR2005 reported the preparation of silicon nitride nanowires by annealing amorphous silicon nitride nanoparticles in a nitrogen flow at 1450-1550°C . The Bulletin of the Polish Academy of Chemical Sciences (BULLETIN OF THE POLISH ACADEMY OF SCIENCES-CHEMISTRY 50(2): 165-174 JUN 2002) reported the preparation of α-silicon nitride nanowires by reacting silica gel and ammonia at 1360°C. However, these preparation reactions all require a high reaction temperature, and the reactions all need to be carried out in an airflow, which requires high cost, which is not conducive to the large-scale preparation of silicon nitride nanowires. Netherlands "Chemical Physics Letters" (CHEMICAL PHY...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/38C30B29/62C30B7/14C01B21/068
Inventor 钱逸泰邹贵付谷云乐
Owner UNIV OF SCI & TECH OF CHINA
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