Method for preparing nano aluminum nitride powder

A nano-aluminum nitride and powder technology, applied in the field of material science, can solve the problems of agglomeration, uneven distribution of components, and inconsistent particle diameter distribution of aluminum nitride powder, and achieve fine particle size, uniform particle distribution, and uniform distribution. Effect

Active Publication Date: 2011-02-16
深圳特新界面科技有限公司
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Problems solved by technology

However, due to the different properties of the aluminum source and the carbon source, the segregation of similar elements is very easy to occur in the wet chemical preparation process, resulting in uneven distribution of the aluminum source and the carbon source, which affects the preparation of nano-aluminum nitride by carbothermal reduction. The quality of the powder leads to incomplete reduction and nitriding of the final product, uneven distribution of components, inconsistent particle diameter distribution of aluminum nitride powder, and even serious agglomeration

Method used

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  • Method for preparing nano aluminum nitride powder
  • Method for preparing nano aluminum nitride powder
  • Method for preparing nano aluminum nitride powder

Examples

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Effect test

Embodiment 1

[0022] Weigh 1.0 mol of aluminum nitrate and dissolve in absolute ethanol to form a 4.0 mol / l solution, weigh 0.4 mol of citric acid and dissolve in 1.6 mol of ethylene glycol, mix the above two solutions; dissolve 1.0 mol of glucose in deionized water A 3.0 mol / l solution was formed and then added to the above solution to form a mixed solution. Stir the mixed solution evenly, heat up to 130° C. for 2 hours, and then continue to heat up to 200° C. for 2 hours to obtain a crisp black substance. The above crisp black substance was calcined at 800°C for 1 hour in a nitrogen atmosphere, ground in a mortar after cooling, then placed in a flowing nitrogen atmosphere, and kept at 1450°C for 2 hours to obtain a black powder; The black powder is kept in air at 700°C for 2 hours for decarburization to obtain nano-aluminum nitride powder. The above-mentioned nano-aluminum nitride powder is detected by X-ray diffraction, and the result shows that it is a single AlN phase (see figure 1 )...

Embodiment 2

[0024] Weigh 1.0mol aluminum acetate and dissolve it in acetone to form a 2.0mol / l solution, weigh 1.0mol citric acid and dissolve it in 8.0mol ethylene glycol, and mix the above two solutions; dissolve 0.2mol sucrose in deionized water to form a 2.0mol / l solution. mol / l solution, and then added to the above solution to form a mixed solution. After the mixed solution was stirred evenly, the temperature was raised to 125° C. for 2 hours, and then the temperature was further raised to 190° C. for 3 hours to obtain a crisp black substance. The above-mentioned crisp black substance was calcined in vacuum at 1000°C for 1 hour, ground in a mortar after cooling, then placed in a flowing nitrogen atmosphere, and kept at 1550°C for 3 hours to obtain a black powder; The powder is kept in air at 750°C for 2 hours for decarburization to obtain nano-aluminum nitride powder. The above-mentioned nano-aluminum nitride powder is detected by X-ray diffraction, and the result shows that it is a...

Embodiment 3

[0026] Weigh 1.0mol aluminum isopropoxide and dissolve it in deionized water to form a 1.0mol / l solution, weigh 0.5mol citric acid and dissolve it in 3.0mol ethylene glycol, mix the above two solutions; dissolve 0.25mol methylcellulose Form a 1.0 mol / l solution in absolute ethanol, and then add to the above solution to form a mixed solution. After the mixed solution was stirred evenly, the temperature was raised to 135° C. for 2 hours, and then the temperature was further raised to 220° C. for 2 hours to obtain a crisp black substance. The above crisp black substance was calcined in a nitrogen atmosphere at 1200°C for 1 hour, ground in a mortar after cooling, then placed in a flowing nitrogen atmosphere, and kept at 1400°C for 4 hours to obtain a black powder; The black powder is kept in air at 760°C for 2 hours for decarburization to obtain nano-aluminum nitride powder. The above-mentioned nano-aluminum nitride powder is detected by X-ray diffraction, and the result shows th...

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Abstract

The invention discloses a method for preparing nano aluminum nitride powder. The method comprises the following steps of: dissolving an aluminum source and a carbon source in a solvent respectively, mixing the dissolved aluminum source and carbon source and glycol solution of citric acid; warming the mixed solution to 125 to 135 DEG C, and keeping the temperature for 2 to 4 hours; continuously warming to 180 to 220 DEG C, and keeping the temperature for 2 to 4 hours to obtain a crisp black substance; calcining the crisp substance at the temperature of between 800 and 1,200 DEG C in vacuum or in the atmosphere of nitrogen; cooling the calcined substance and grinding; and performing a carbothermal reduction reaction at the temperature of between 1,350 and 1,600 DEG C to obtain the nano aluminum nitride powder. Raw materials adopted by the method have a wide source range and are readily available, a preparation process is simple and controllable, and aluminum ions are uniformly distributed in the carbon source by using the complexing action of the citric acid on metallic aluminum ions and the bonding and steric hindrance actions of glycol on the metallic aluminum ions so as to finally obtain the nano aluminum nitride powder with small particle sizes and uniform particle distribution.

Description

technical field [0001] The invention relates to a preparation method of nanometer aluminum nitride powder, which belongs to the technical field of material science. Background technique [0002] Aluminum nitride ceramics have the characteristics of high thermal conductivity, linear expansion coefficient matching silicon, low dielectric constant, excellent electrical insulation performance, corrosion resistance, environmental protection and non-toxicity, and have replaced alumina and beryllium oxide as the current The preferred material for VLSI substrates has been widely used in high-tech fields such as modern electronics and microelectronics. However, aluminum nitride is a covalent compound, and its self-diffusion coefficient is small, making it difficult to sinter densely. In order to reduce the sintering temperature of aluminum nitride ceramics, most researchers add suitable sintering aids, use the sintering aids to react with the aluminum oxide on the surface of aluminu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/072B82B3/00
Inventor 王焕平徐时清杨清华邓德刚赵士龙
Owner 深圳特新界面科技有限公司
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