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Method for low-temperature preparation of cubic silicon carbide nano wire

A cubic silicon carbide and nanowire technology, applied in nanotechnology, nanotechnology, nanostructure manufacturing and other directions, can solve problems such as large-scale preparation that have not been realized, and achieve good product morphology, simple and easy-to-control operation, and low reaction temperature. Effect

Inactive Publication Date: 2008-05-14
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned preparation processes often need to be carried out at a high temperature above 1200°C or in an airflow. The prepared nanowires may be applied to high-tech fields, but their large-scale preparation has not yet been realized.

Method used

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  • Method for low-temperature preparation of cubic silicon carbide nano wire
  • Method for low-temperature preparation of cubic silicon carbide nano wire
  • Method for low-temperature preparation of cubic silicon carbide nano wire

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1: Low-temperature synthesis of cubic silicon carbide nanowires

[0033] Take 1.0g of silicon powder, 4.0g of sodium metal, 3mL of tetrachlorethylene and 1g of sulfur powder, and put them into a special stainless steel reaction kettle (the volume of the reaction kettle is 25ml). In a drying oven, react for 40 hours at 120°C (furnace temperature controlled at ±1°C) and 6.8MPa; after stopping heating, cool the reaction kettle to room temperature naturally; open the kettle, wash the obtained product with 95% ethanol, Wash with 1mol / L hydrochloric acid, then wash with 70% perchloric acid by weight percentage, wash with nitric acid:hydrofluoric acid=1:1 mixture, wash with carbon disulfide, wash with water until pH neutral, centrifuge and vacuum at 50°C After drying for 6 hours, an off-white powder product, namely cubic silicon carbide (3C-SiC) powder, was finally obtained.

[0034] The crop phase of the product was analyzed using a German Bruker D8 ADVANCE X-ray pow...

Embodiment 2

[0041] Example 2: Low-temperature synthesis of cubic silicon carbide nanowires

[0042] Take 1.0g of silicon powder, 4.0g of sodium metal and 3mL of tetrachlorethylene, put them into a special stainless steel reaction kettle (the volume of the reaction kettle is 25ml), use nitrogen to remove the air in the kettle, seal it and place it in an electric heating constant temperature blast drying box, React at 260°C (furnace temperature controlled at ±1°C) and 8.7MPa for 20 hours; after stopping heating, cool the reactor to room temperature naturally; Washing, then washing with 70% perchloric acid by weight percentage, washing with nitric acid: hydrofluoric acid = 1: 1 mixed solution, washing with water until the pH is neutral, centrifuging and vacuum drying at 50°C for 6 hours, finally obtaining off-white Powder products, namely 3C-SiC powder.

[0043] Fig. 8 is the X-ray powder diffraction spectrum of the purified product prepared by using silicon powder, sodium metal and tetrach...

Embodiment 3

[0046] Example 3: Low-temperature synthesis of cubic silicon carbide nanowires

[0047] Mix silicon powder, tetrachlorethylene, sodium metal and sublimed sulfur in a molar ratio of 0.5:1:2:0.5, seal in an autoclave, and react at 160°C and 10MPa for 35 hours; the product is washed with ethanol, sulfuric acid, Washing with water until the pH is neutral, conventional centrifugation, and drying to obtain cubic silicon carbide nanowires.

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Abstract

The invention discloses a low-temperature preparation method of cubic silicon carbide nano-wires, which comprises the following steps: silica flour, tetrachloroethylene, sodium and sublimed sulfur are mixed in a mol radio of 0.5 to 4 : 1 : 2 to 8 : 0.5 to 2 and then sealed in an autoclave for reaction under the condition of 120 to 260 DEG C and 5 MPa to 18 MPa for 10 to 55 hours, or under the condition of 260 to 600 DEG C and 7 MPa to 18 MPa for 10 to 55 hours, with the same ingredients and without adding sulfur. After alcohol washing, pickling or igniting, then the product is pickled and washed with water until the product shows a neutral pH, and finally the cubic silicon carbide mano-wires are obtained after conventional centrifugal separation and drying. Compared with the prior art, the method has the advantages of low reaction temperature, low material cost and easy availability, simple reaction, easy control for the size and dimension of the product, enhanced toughness of ceramic and easy realization for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of silicon carbide nanometer materials, in particular to a low-temperature preparation method of cubic silicon carbide (3C-SiC) nanowires. Background technique [0002] Silicon carbide has very high strength and toughness, and can be widely used as a reinforcing agent for ceramics, metals and polymer matrix composites (Adv. Mater., 2000, 12, 1186). 3C-SiC is a wide bandgap semiconductor (2.3eV), which has the advantages of high operating temperature (up to 600°C), small on-state resistance, good thermal conductivity, and high pn junction withstand voltage, so it is an important new type of power in the 21st century. One of semiconductor device materials. [0003] Cutler et al. heated specially treated rice husks to 2000°C to grow SiC whiskers (J.Am.Ceram.Soc.Bull., 1975, 54, 195; US patent, 3754076.1973). Dai H.J. et al. combined carbon nanotubes with SiO or SiI with high vapor pressure at 1...

Claims

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Application Information

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IPC IPC(8): C01B31/36B82B3/00
Inventor 钱逸泰鞠治成邢政徐立强马小健
Owner SHANDONG UNIV
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