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Low-temperature solid phase reaction preparation of silicon nitride nano-material

A technology of solid-state reaction and silicon nitride, which is applied in the direction of polycrystalline material growth, self-solidification, chemical instruments and methods, etc., can solve the problems of repeated difficulties, high reaction pressure, and difficulty in applying industrial production, etc., and achieves simple and enhanced methods. Low requirements for toughness, environment and equipment conditions

Inactive Publication Date: 2008-10-29
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is difficult to repeat and the reaction pressure is relatively high, which makes it difficult to apply to industrial production.

Method used

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  • Low-temperature solid phase reaction preparation of silicon nitride nano-material
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  • Low-temperature solid phase reaction preparation of silicon nitride nano-material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: Low-temperature synthesis of silicon nitride nanomaterials

[0025] Take 0.8g of silicon powder, 3g of powdered thiosemicarbazide, 3g of sodium azide and 2g of iodine, mix them evenly, put them into a 20mL special stainless steel reaction kettle, seal it and place it in an electric heating constant temperature blast drying oven, and dry it at 60 °C (furnace temperature controlled at ±5 °C) for 12 hours; after stopping the heating, cool the reaction kettle to room temperature naturally; The mixed solution of hydrofluoric acid and nitric acid (the volume ratio of hydrofluoric acid and nitric acid is 1:3) was washed to remove elemental silicon; vacuum drying was carried out at 50° C. for 6 hours, and finally an off-white powder product was obtained.

[0026] Cu Kα rays (wavelength λ=1.54178 ) is a diffraction light source for X-ray diffraction analysis of the product.

[0027] figure 1 The X-ray diffraction spectrum (XRD) of the product was prepared by us...

Embodiment 2

[0031] Example 2: Low-temperature synthesis of β-phase silicon nitride nanorods

[0032] Take 0.8g of silicon powder, 5g of powdered thiosemicarbazide, 3g of sodium azide and 1g of aluminum powder, mix them evenly, put them into a 20mL special stainless steel reaction kettle, seal it and place it in an electric constant temperature blast drying oven, React at 170°C (furnace temperature controlled at ±5°C) for 10 hours; after stopping heating, cool the reaction kettle to room temperature naturally; The mixed liquid of hydrofluoric acid and nitric acid (the volume ratio of hydrofluoric acid and nitric acid is 1:3) was washed to remove elemental silicon; vacuum-dried at 50° C. for 6 hours, finally an off-white powder product was obtained.

[0033] figure 2 It is the X-ray diffraction spectrum (XRD) of the product prepared by using silicon powder, thiosemicarbazide, sodium azide and aluminum powder at 170° C. for 10 hours. Stronger diffraction peaks can be indexed as simple hex...

Embodiment 3

[0037] Embodiment 3: Low-temperature synthesis of silicon nitride nanomaterials

[0038] Take 0.8g of silicon powder, 4g of powdery thiosemicarbazide and 3g of sodium azide, mix them evenly, put them into a 20mL special stainless steel reaction kettle, seal them and place them in an electric heating constant temperature blast drying oven, at 170°C (furnace temperature controlled at ±5°C) for 10 hours; after stopping the heating, cool the reaction vessel to room temperature naturally; open the vessel, wash the product with acid and water until the pH is neutral, and centrifuge, then pass the product through hydrofluoric acid and nitric acid The mixed liquid (the volume ratio of hydrofluoric acid and nitric acid is 1:3) was washed to remove elemental silicon; vacuum-dried at 50° C. for 6 hours, finally an off-white powder product was obtained.

[0039] image 3 The X-ray diffraction spectrum (XRD) of the product was prepared by using silicon powder, thiosemicarbazide and sodium...

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Abstract

The invention discloses a method for preparing a silicon nitride nano-material by using solid phase reaction at a low temperature. The method comprises the following steps: silicon powder, powdery thiosemicar bazide, sodium azide and iodine are evenly mixed according to the mole ratio of 0.386 to 0.926:0.476 to 0.953:1:0.171 to 0.256 and sealed in a high-pressure autoclave, and react for 12 plus or minus 0.5 hours at the temperature of 60 plus or minus 5 DEG C; or the silicon powder, the powdery thiosemicar bazide, the sodium azide and alluminium powder are evenly mixed according to the mole ratio of 0.386 to 0.926:0.716 to 1.193:1:0.804 and sealed in the high-pressure autoclave, and react for 10 plus or minus 0.5 hours at the temperature of 170 plus or minus 5 DEG C; or the silicon powder, the powdery thiosemicar bazide and the sodium azide are evenly mixed according to the mole ratio of 0.386 to 0.926:0.716 to 1.193:1 and sealed in the high-pressure reactor, and react for 10 plus or minus 0.5 hours at the temperature of 170 plus or minus 5 DEG C; the pH of the product is neutral though water cleaning and water washing; centrifugal separation and drying are performed; then acid is added for scrubbing, monatomic silicon is removed; and the silicon nitride nano-materials are obtained. The method has the advantages that the reaction temperature is lower; the appearance of the obtained product is good; the diameters of the nano-rods are even; and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of silicon nitride nanometer material preparation, and in particular relates to a method for synthesizing silicon nitride nanometer material at low temperature by using solid phase reaction in an autoclave. Background technique [0002] Silicon nitride has remarkable properties such as high melting point, high hardness, toughness, high thermal stability, and excellent wear resistance and corrosion resistance, so it has become an excellent engineering material and has broad application prospects. [0003] Netherlands "Materials Science" (JOURNAL OF MATERIALS SCIENCE 33(24): 5803-5810 DEC 1998) reported elongated β-Si 3 N 4 The particles have the property of inhibiting the brittleness of ceramics, and are a kind of reinforcing and toughening agent for ceramic materials with excellent performance. The US "Applied Physics Letters" (APPLIED PHYSICS LETTERS 71 (16): 2271-2273 OTC 1997) reported that silicon powd...

Claims

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Application Information

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IPC IPC(8): C30B29/30C30B29/62C30B1/10
Inventor 钱逸泰郭春丽李凤侠徐立强马小健
Owner SHANDONG UNIV
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