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Process for preparing silicon nitride nano material

A technology of nanomaterials and silicon nitride, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of raw materials toxicity, performance impact, and high price

Inactive Publication Date: 2007-03-07
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because in the above-mentioned method for preparing silicon nitride nanomaterials, some raw materials used are toxic, some are more expensive, some reaction conditions are harsher, and the prepared Si 3 N 4 The purity is not high, which affects its performance and has certain limitations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. Weigh 12 grams of phenolic resin and 1.2 grams of ferric nitrate in a beaker, add 35 milliliters of absolute ethanol, stir to dissolve.

[0021] 2. Add 50 ml tetraethyl orthosilicate (TEOS) and 0.3 g oxalic acid under stirring condition, and hydrolyze TEOS at room temperature for 24 hours to form silica sol.

[0022] 3. Add 0.2 g of curing agent hexamethylenetetramine to accelerate the solidification of the sol to form a gel, and then dry at 110° C. for 36 hours to obtain a silica xerogel.

[0023] 4. Burn the obtained xerogel in a muffle furnace at 500°C for 10 hours to remove the template agent phenolic resin to obtain porous silica.

[0024] 5. After mixing porous silica and silicon powder at a molar ratio of 1:1, heat to 1300°C at a rate of 8°C / min under nitrogen gas (flow rate: 200ml / min), keep the temperature constant for 10 hours, and cool to room temperature .

[0025] 6. The original product was first oxidized in air at 700°C for 3 hours, then soaked in a ...

Embodiment 2

[0027] 1. Weigh 20 grams of sucrose and 1.2 grams of cobalt nitrate in a beaker, add 100 milliliters of absolute ethanol, and stir to dissolve them.

[0028] 2. Add 100 ml tetraethyl orthosilicate (TEOS) and 0.2 g hydrochloric acid under stirring condition, and hydrolyze TEOS at room temperature for 72 hours to form silica sol.

[0029] 3. Add 0.4 g of curing agent hexamethylenetetramine to accelerate the solidification of the sol to form a gel, and then dry at 150° C. for 12 hours to obtain a silica xerogel.

[0030] 4. Burn the obtained xerogel in a muffle furnace at 800°C for 2 hours to remove the template agent sucrose to obtain porous silica.

[0031] 5. After mixing porous silicon dioxide and silicon powder at a molar ratio of 2:1, heat to 1300°C at a heating rate of 5°C / min under ammonia gas (flow rate: 100ml / min), keep the temperature constant for 20 hours, and cool to At room temperature, the original product was obtained.

[0032] 6. The original product was first ...

Embodiment 3

[0034] 1. Weigh 10 grams of cetyltrimethylammonium bromide and 5.0 grams of lanthanum nitrate in a beaker, add 50 milliliters of absolute ethanol, and stir to dissolve them.

[0035] 2. Add 50 ml tetraethyl orthosilicate (TEOS) and 0.3 g oxalic acid under stirring condition, and hydrolyze TEOS at room temperature for 48 hours to form silica sol.

[0036] 3. Add 0.2 g of curing agent hexamethylenetetramine to accelerate the solidification of the sol to form a gel, and then dry at 60° C. for 72 hours to obtain a silica xerogel.

[0037] 4. Burn the obtained xerogel in a muffle furnace at 500°C for 10 hours to remove the template agent hexadecyltrimethylammonium bromide to obtain porous silica.

[0038] 5. After porous silicon dioxide and silicon powder are mixed in a molar ratio of 1:1, under nitrogen flow (flow rate: 200ml / min), heat up to 1200°C at a heating rate of 15°C / min, keep the temperature constant for 20 hours, and cool to room temperature.

[0039] 6. The original p...

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PUM

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Abstract

The invention discloses a preparing method of silicon nitride nanometer material, which comprises the following steps: stirring molding agent and nitrate to dissolve; adding silicic carbethoxy and catalyst; hydrolyzing silicic carbethoxy into silica sol under indoor temperature; adding hardener to form sol gel; drying to obtain dried gel of silica; sintering to obtain porous silica; blending porous silica and silicon powder according to rate; aerating nitrogen or ammonia gas; heating to 1000-1500 deg.c; insulating for 2-30h; cooling to indoor temperature to obtain original product; oxidizing for 2-10h; immersing in the composite acid with alcaine and fluohydric acid or nitrate and fluohydric acid; washing; drying to obtain ladder-shaped, feather-shaped or wheat-shaped silicon nitride nanometer material.

Description

technical field [0001] The invention relates to a preparation method of a silicon nitride nanometer material, in particular to a preparation method of a silicon nitride nanometer material with a special shape, such as a ladder shape, a feather shape or a wheat ear shape. technical background [0002] Silicon nitride is an advanced engineering ceramic and semiconductor material. The material has high room temperature and high temperature strength, high hardness, corrosion resistance, oxidation resistance and good thermal shock and mechanical shock resistance. It is considered by the material science community to be the most comprehensive performance in the field of structural ceramics. Nickel-based alloy is a new material widely used in high-tech and high-temperature fields. For example, Si 3 N 4 Due to its excellent high temperature resistance, high modulus, high strength, low expansion coefficient and good thermal and chemical stability, whiskers can be added to plastic ...

Claims

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Application Information

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IPC IPC(8): C01B21/068
Inventor 郭向云王峰靳国强
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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