Method for preparing AlN powder

A powder and solid technology, applied in chemical instruments and methods, nanotechnology for materials and surface science, inorganic chemistry, etc., can solve the problems of long reaction time, high synthesis temperature, complex process, etc., and achieve simple preparation method , low reaction temperature, environmentally friendly effect

Inactive Publication Date: 2019-01-25
SHAANXI UNIV OF SCI & TECH +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing high-purity AlN powder at a relatively low temperature in view of the existing problems in the synthesis of aluminum nitride such as high synthesis temperature, long reaction time, complex process, large product particle size and low purity. method

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  • Method for preparing AlN powder

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Experimental program
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Effect test

Embodiment 1

[0030] According to the Al:N molar ratio of 1:18, weigh 2.4143g (0.01mol) AlCl 3 ·6H 2 O and 5.7318 g (0.06 mol) of guanidine hydrochloride were fully dissolved in 15 mL of ethanol, and then the ethanol was evaporated to dryness at 80° C., and the resulting solid mixture was calcined at 800° C. for 2 h in a nitrogen atmosphere, and then decarburized at 550° C. for 3 h in an air atmosphere. Cool naturally to room temperature to obtain AlN powder.

[0031] Depend on figure 1 It can be seen that the XRD diffraction peaks of the obtained AlN powder are consistent with the standard diffraction peaks, indicating that the prepared AlN has high purity. At the position of the diffraction peak with a 2θ value of 33°, the size of the AlN crystal is calculated using the Debye-Scherrer formula to be 9.4 nm, which means the average particle size of the crystal in the vertical direction of 33°.

Embodiment 2

[0033] According to the Al:N molar ratio of 1:24, weigh 2.4143g (0.01mol) AlCl 3 ·6H 2 O and 7.6424 g (0.08 mol) of guanidine hydrochloride were fully dissolved in 15 mL of methanol, and then the methanol was evaporated to dryness at 70° C., and the resulting solid mixture was roasted at 800° C. for 2.5 h in a nitrogen atmosphere, and then decarburized at 550° C. for 1 h in an air atmosphere. Cool naturally to room temperature to obtain AlN powder with a crystal size of 8.6 nm.

Embodiment 3

[0035] According to the Al:N molar ratio of 1:15, weigh 2.4143g (0.01mol) AlCl 3 ·6H 2 O and 5.8555g (0.05mol) of guanidine acetate were fully dissolved in 15mL of deionized water, then evaporated to dryness at 100°C, and the resulting solid mixture was placed in a mixed atmosphere of ammonia and helium at a volume ratio of 1:9 at 850°C Calcined for 1 hour, then decarburized at 550°C for 3 hours in an air atmosphere, and cooled naturally to room temperature to obtain AlN powder with a crystal size of 15.9 nm.

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Abstract

The invention discloses a method for preparing AlN powder. The method includes first dissolving an aluminum source and a nitrogen source completely in a solvent according to the Al:N molar ratio of 1:1-1:35, mixing evenly, drying the solvent by evaporating, roasting an obtained solid mixture at 500-1000 DEG C for 1-9h in a roasting atmosphere, and then decarburizing the mixture at 200-750 DEG C for 1 to 5h in an air atmosphere to obtain the high-purity AlN powder. The aluminum source is aluminum chloride hydrate, aluminum lactate, aluminum glycinate, aluminum stearate and the like; the nitrogen source is guanidine hydrochloride, guanidine acetate, chitosan, 1,10-phenanthroline; the solvent is any one of deionized water, methanol, ethanol, ethyl acetate, acetone, diethyl ether, benzene andtoluene; the roasting atmosphere is one or two of nitrogen, ammonia, argon and helium. Compared with the conventional AlN preparation method, the method has the advantages of wide reactant range, environmentally-friendly process, simple operation, high product purity and low cost.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a method for preparing AlN powder. Background technique [0002] Aluminum nitride (AlN) is a group III-V covalent compound, which belongs to the diamond-like nitride of the hexagonal wurtzite crystal structure. Its room temperature strength is high (it is Al 2 o 3 More than 5 times of that), the thermal expansion coefficient is small, which can greatly improve the thermal conductivity of plastics and silicone rubber, and is a good heat-shock resistant material; it has strong resistance to molten metal erosion, and is an ideal crucible for melting and casting pure iron, aluminum or aluminum alloys Material; has excellent electrical insulation, resistivity as high as 426Ω·cm, and good dielectric properties. It is an ideal heat dissipation material and packaging material for large-scale integrated circuits, semiconductor module circuits and high-power devi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/072B82Y30/00
CPCB82Y30/00C01B21/072C01P2002/72C01P2004/64
Inventor 何珍红王忠宇王宽刘昭铁
Owner SHAANXI UNIV OF SCI & TECH
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