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Preparation method of high-purity sphere-like nanometer AlN (aluminum nitride) particle

A technology of nano-aluminum nitride and spherical particles, applied in chemical instruments and methods, nitrogen compounds, nanotechnology, etc., to achieve the effects of low cost, narrow particle size distribution range, and wide range of raw materials

Active Publication Date: 2018-11-23
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method of high-purity sphere-like nanometer AlN (aluminum nitride) particle
  • Preparation method of high-purity sphere-like nanometer AlN (aluminum nitride) particle
  • Preparation method of high-purity sphere-like nanometer AlN (aluminum nitride) particle

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Experimental program
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Effect test

Embodiment 1

[0084] The preparation method of high-purity, spherical nano-AlN comprises the following steps:

[0085] (1) Al 2 o 3 Powder: Ca(NO 3 ) 2 4H 2 O+Y(NO 3 ) 3 ·6H 2 O+KF: Water-soluble starch is weighed according to the mass ratio of 1:(0.15+0.2+0.05):4, mix the above materials, add a certain amount of water, the ratio of water to powder mass is 3:1, and use corundum The ball is used as the grinding medium, and the ball is milled in a corundum tank for 4 hours, and the speed of the ball mill is 400 rpm. After the ball milling, the slurry is sprayed and granulated to obtain fluffy micron-sized spherical particles. Aluminum oxide primary particles are accumulated;

[0086] (2) Transfer the micron-sized spherical particles into the corundum sagger, put the sagger into the microwave synthesis reaction chamber, use silicon carbide wafers as auxiliary heat, and inject atmospheric nitrogen to carry out powder synthesis. The synthesis process is divided into 2 stages: The first...

Embodiment 2

[0090] The preparation method of high-purity, spherical nano-AlN powder comprises the following steps:

[0091] (1) Al 2 o 3 Powder:Mg(NO 3 ) 2 +Gd(NO 3 ) 3 ·6H 2 O+NaF: sucrose is weighed according to the mass ratio of 1:(0.18+0.25+0.07):6, the above materials are mixed, a certain amount of water is added, the ratio of water to powder mass is 4.5:1, and corundum balls are used as Grinding media, ball milling in a corundum tank for 6 hours, the ball mill speed is 400 rpm, spray granulation of the slurry after ball milling, to obtain fluffy micron-sized spherical particles, the particles are wrapped by carbon precursor - soluble inorganic salt and alumina The accumulation of primary particles;

[0092] (2) Transfer the micron-sized spherical particles into the corundum sagger, put the sagger into the microwave synthesis reaction chamber, use silicon carbide wafers as auxiliary heat, and inject atmospheric nitrogen to carry out powder synthesis. The synthesis process is d...

Embodiment 3

[0096] The preparation method of high-purity, spherical nano-AlN comprises the following steps:

[0097] (1) Al 2 o 3 Powder: Ca(NO 3 ) 2 4H 2 O+Ce(NO 3 ) 3 ·6H 2 O+KF: Water-soluble dextrin is weighed according to the mass ratio of 1:(0.25+0.15+0.06):5.5, mix the above materials, add a certain amount of water, the ratio of water to powder mass is 5:1, use Corundum balls are used as grinding media, milled in a corundum tank for 6 hours, the speed of the ball mill is 400 rpm, and the slurry is sprayed and granulated after ball milling to obtain fluffy micron-sized spherical particles, which are soluble inorganic salts wrapped by carbon precursors Accumulated with alumina primary particles;

[0098] (2) Transfer the micron-sized spherical particles into the corundum sagger, put the sagger into the microwave synthesis reaction chamber, use silicon carbide wafers as auxiliary heat, and inject atmospheric nitrogen to carry out powder synthesis. The synthesis process is div...

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Abstract

The invention discloses a preparation method of a high-purity sphere-like nanometer AlN (aluminum nitride) particle. The preparation method comprises the following steps of (1) weighing an Al2O3 (aluminum oxide) powder, soluble inorganic salt and a water-soluble organic precursor according to a mass ratio, mixing, adding water, performing ball grinding, spraying and granulating, so as to obtain amicrometer spherical particle; (2) synthesizing the micrometer spherical particle by microwaves under the nitrogen atmosphere in two stages, wherein in the first stage, the room temperature is heatedto the temperature of 800 to 1200 DEG C at the heating speed of 0.1 to 5 DEG C / min, and the increased temperature is warmed; in the second stage, the temperature is increased to 1200 to 1800 DEG C atthe heating speed of 1 to 20 DEG C / min, and the increased temperature is warmed, so as to obtain the nanometer aluminum nitride particle containing trace carbon; (3) decarbonizing the nanometer aluminum nitride particle containing trace carbon under the CO2 (carbon dioxide) atmosphere, so as to obtain the high-purity sphere-like nanometer AlN particle. The preparation method has the advantages that the raw materials are wide and are easy to obtain, the equipment and technology are simpler, the cost is lower, and the preparation technology is especially suitable for industrialized production. The prepared AlN powder has the advantages that the purity is high, the particle size distribution range is broad, the specific surface area is high, and the like.

Description

technical field [0001] The invention relates to a method for preparing high-purity, quasi-spherical nano-aluminum nitride particles, and belongs to the technical field of preparing nano-aluminum nitride. Background technique [0002] AlN (aluminum nitride) ceramics have excellent comprehensive properties, such as high thermal conductivity (140-260W·(m K) -1 ), high resistivity (>10 14 Ω cm), dielectric constant (8.8 1MHz) and dielectric loss (5-10×10 14 ), a thermal expansion coefficient close to that of silicon (4.3×10 -6 m / ℃), low density (theoretical density 3.26g cm -3 ) are widely used in high-temperature electronic equipment such as electronic substrates, heat sinks, heat dissipation substrates between thyristors and heat sinks, semiconductor laser insulation and heat dissipation components, and field effect transistors. [0003] Secondly, AlN ceramics have good high-temperature mechanical properties (compared to Al 2 o 3 Similar bending strength), chemical st...

Claims

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Application Information

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IPC IPC(8): C01B21/072B82Y40/00
CPCB82Y40/00C01B21/072C01P2002/72C01P2004/03C01P2004/62C01P2004/64C01P2006/12
Inventor 高朋召刘小磐程磊郑航博吴迪王玲
Owner HUNAN UNIV
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