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Method of preparing alpha Si3N4 nano-powder

A nano-powder, -si3n4 technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., to achieve the effect of simple reaction and purification methods, low reaction temperature, and pure product phase

Inactive Publication Date: 2006-06-28
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, no single-phase α-Si has been directly prepared at a lower temperature. 3 N 4 Report on nanopowder

Method used

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  • Method of preparing alpha Si3N4 nano-powder
  • Method of preparing alpha Si3N4 nano-powder
  • Method of preparing alpha Si3N4 nano-powder

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Embodiment 1

[0017] Example 1: Mg 2 Si and NH 4 Preparation of α-Si by Cl reaction 3 N 4 Nano powder

[0018] Mg used in the reaction in this embodiment 2 The Si raw material can be magnesium silicide prepared by heating stoichiometric silicon powder and metal magnesium powder at 700-1000° C. for 24-48 hours in a closed manner, or magnesium silicide using reagents or industrial products. Take 26.08 mmol of Mg 2 Si and 106.9-117.4 mmol of NH 4 Cl(Mg 2 Si and NH 4 The molar ratio of Cl is 1 to 4.1-4.5) after mixing, put it into a stainless steel reaction kettle with a glass tube lining, use argon to remove the air in the kettle, seal it and place it in a resistance crucible boiler. Respectively react at a reaction temperature of 450, 500, 550, 600 or 650°C (furnace temperature control ±5°C) for 2-12 hours; after stopping heating, the reaction kettle is naturally cooled to room temperature in the air. Open the kettle to take out the reaction product and wash with distilled water and ...

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Abstract

A process for preparing alpha-Si3N4 nanoparticles size 15-95 nanometer includes such steps as proportionally mixing magnesium silicide with ammonium chloride, reaction at 450-650 deg.C for 2-12 hr in sealed condition, water washing, separation and drying.

Description

Technical field: [0001] The invention belongs to the technical field of nanometer material preparation, in particular to a method for preparing single-phase α-silicon nitride nanopowder through solid phase displacement reaction. Background technique: [0002] "Journal of American Ceramic Society" (J.Am.Ceram.Soc.1991, 74, 31-37) has reported that SiO can be reduced by high temperature carbothermal at 1500-1550°C 2 To prepare silicon nitride powder method, the journal (2001, 84, 1669-1674) also reported the use of N at 1200-1400 ° C 2 Gas and silicon powder react to prepare silicon nitride powder. But these traditional high-temperature reaction methods cannot prepare silicon nitride nanomaterials. This journal (1998,81,2294-2300) reported thermal decomposition of complex organic precursors to obtain amorphous silicon nitride powder, and then annealed and crystallized at 1450-1550°C; this journal (1991,74,2759- 2768) also reported that SiH 2 Cl 2 with NH 3 The reaction p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/068
Inventor 谷云乐钱逸泰陈庐阳
Owner UNIV OF SCI & TECH OF CHINA