Preparation method of silicon nitride nano wire and nano band powder material
A silicon nitride nanometer and powder material technology, applied in nanostructure manufacturing, chemical instruments and methods, nitrogen compounds, etc., can solve the problems of high preparation cost and low temperature performance
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Embodiment 1
[0038] Embodiment 1: Preparation of silicon nitride nanowires
[0039] Take 3.8 grams of NaN3 Add 2.69 grams of metal Na to a stainless steel reactor with a volume of about 60 ml, and then add 5 ml of liquid SiCl 4 . SiCl 4 It is analytical grade reagent, white solid crystal NaN 3 and metal Na are chemically pure reagents. Metal Na was removed from kerosene, blotted dry with filter paper, and cut into small pieces. Operations were carried out in a glove box filled with dry argon at room temperature. Cover and seal the reaction kettle, then put it into a well-type crucible furnace, react at a constant temperature of 450°C for 5 hours, cool to room temperature naturally, open the kettle and take out the reaction product. The product was washed with water, washed with absolute ethanol and centrifuged to remove the by-product sodium chloride, and dried in a vacuum oven at 80° C. for 24 hours to obtain 1.895 g of a white powder product. After structure, composition and morpho...
Embodiment 2
[0040] Embodiment 2: Preparation of silicon nitride nanowires
[0041] Take 3.25 grams of NaN 3 Add 3.0 grams of metal Na to a stainless steel reactor with a volume of about 60 ml, and then add 5 ml of liquid SiCl 4 . React at a constant temperature of 450°C for 2 hours, cool down to room temperature naturally, open the kettle and take out the reaction product. All the other operations are the same as above-mentioned example 1, obtain 1.947 gram white powder products. After structure, composition and morphology analysis, it is proved that the product is pure silicon nitride, in which β-Si 3 N 4 About 90.3%, α-Si 3 N 4 About 9.7% relative to SiCl 4 The total yield is 94.4%, and the morphology of the product is dominated by nanowires with a small amount of uniform nanobelts.
Embodiment 3
[0042] Embodiment 3: Preparation of silicon nitride nanobelts
[0043] Take 2.70 grams of NaN 3 Add 3.15 grams of metal Na to a stainless steel reactor with a volume of about 60 ml, and then add 5 ml of liquid SiCl 4 . React at a constant temperature of 500°C for 3.5 hours, cool down to room temperature naturally, open the kettle and take out the reaction product. All the other operations are the same as above-mentioned example 1, obtain 1.863 gram white powder products. After structure, composition and morphology analysis, it is proved that the product is pure silicon nitride, in which β-Si 3 N 4 About 89.7%, α-Si 3 N 4 About 10.3% relative to SiCl 4 The total yield is 90.6%, and the products are mainly nanowires, and also contain more nanorods and nanobelts.
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