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

A solid-phase reaction, silicon nitride technology, applied in the direction of polycrystalline material growth, self-solid, chemical instruments and methods, etc., can solve the problems of repeated difficulties, difficult to apply industrial production, high reaction pressure, etc. Effects requiring low toughness, environmental and equipment conditions

Inactive Publication Date: 2009-11-18
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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] Example 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 them and place them in an electric heating constant temperature blast drying oven, and place them in an electric heating constant temperature blast drying oven. ℃ (furnace temperature is controlled at ± 5 ℃) and react for 12 hours; after heating is stopped, the reaction kettle is naturally cooled to room temperature; the kettle is opened, the obtained product is washed with acid and water to neutral pH, centrifuged, and then the obtained product is subjected to hydrogen 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-dried at 50° C. for 6 hours to finally obtain a gray-white powder product.

[00...

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 and place them in an electric heating constant temperature blast drying oven, and place them in an electric heating constant temperature blast drying oven. 170°C (furnace temperature is controlled at ±5°C) for 10 hours; after heating is stopped, the reaction kettle is naturally cooled to room temperature; the kettle is opened, the obtained product is washed with acid and water to neutral pH, centrifuged, and then the obtained product is subjected to 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-dried at 50° C. for 6 hours, and finally a gray-white powder product was obtained.

[003...

Embodiment 3

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

[0038] Take 0.8g of silicon powder, 4g of powdered thiosemicarbazide and 3g of sodium azide, mix them evenly, put them into a 20mL special stainless steel reaction kettle, seal and place them in an electric heating constant temperature blast drying oven, at 170 ℃ (furnace temperature) Controlled at ±5°C) and reacted for 10 hours; after heating was stopped, the reaction kettle was naturally cooled to room temperature; the kettle was opened, the resulting product was washed with acid and water to pH neutrality, centrifuged, and then the resulting product was subjected to hydrofluoric acid and nitric acid The mixed solution (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, and finally a gray-white powder product was obtained.

[0039] image 3 X-ray diffraction spectrum (XRD) of the product prepared with silicon p...

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Abstract

The invention discloses a method for preparing silicon nitride nanometer material at low temperature by using solid-state reaction. : 0.171-0.256 mixed evenly, sealed in an autoclave, and reacted at 60±5°C for 12±0.5 hours; or silicon powder, powdered thiosemicarbazide, sodium azide and aluminum powder in a molar ratio of 0.386-0.926:0.716 -1.193:1:0.804 mixed evenly, sealed in an autoclave, and reacted at 170±5°C for 10±0.5 hours; or silicon powder, powdered thiosemicarbazide, sodium azide molar ratio 0.386-0.926:0.716-1.193 : 1 mixed evenly, sealed in an autoclave, and reacted at 170±5°C for 10±0.5 hours; the product was washed with acid and water until the pH was neutral, centrifuged and dried, and then washed with mixed acid to remove elemental silicon to obtain silicon nitride nanomaterials. The reaction temperature of the method of the invention is low, the obtained product has good appearance and uniform diameter of nanorods, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of silicon nitride nanomaterial preparation, and particularly relates to a method for synthesizing silicon nitride nanomaterials 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, strong toughness, high thermal stability, and excellent wear and corrosion resistance, so it has become an excellent engineering material and has a wide range of application prospects. [0003] JOURNAL OF MATERIALS SCIENCE 33(24): 5803-5810DEC 1998 reported elongated β-Si 3 N 4 The particles have the property of inhibiting the brittleness of ceramics, and are a reinforcing and toughening agent for ceramic materials with excellent performance. American "Applied Physics Letters" (APPLIED PHYSICS LETTERS 71(16): 2271-2273OTC 1997) reported that silicon powder, SiO 2 Silicon nitride nanorods were grown in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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