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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  • Abstract
  • Description
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  • 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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[0083] Example 1

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

[0085] (1) The 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, the above materials are mixed, a certain amount of water is added, and the mass ratio of water to powder is 3:1, using corundum The ball is used as the grinding medium, and the ball is milled in a corundum tank for 4 hours, and the ball mill rotates at 400 rpm. Alumina primary particles are piled up;

[0086] (2) Transfer the micron-sized spherical particles into the corundum saggar, put the saggar into the microwave synthesis reaction chamber, use silicon carbide wafers as auxiliary heat, and pass normal pressure nitrogen to carry out powder synthesis. The synthesis process is divided into 2 sections: The first stage: using a heating rate of 1 °C / min to increase from room temperature to 100...

Example Embodiment

[0089] Example 2

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

[0091] (1) The 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, and a certain amount of water is added. The mass ratio of water and powder is 4.5:1, and corundum balls are used as The grinding medium was ball-milled in a corundum tank for 6h, and the ball mill speed was 400 rpm, and the slurry after ball milling was spray-granulated to obtain fluffy micron-sized spherical particles, which were wrapped by carbon precursor-soluble inorganic salts and alumina Primary particles are accumulated;

[0092] (2) Transfer the micron-sized spherical particles into the corundum saggar, put the saggar into the microwave synthesis reaction chamber, use silicon carbide wafers as auxiliary heat, and pass normal pressure nitrogen to carry out powder s...

Example Embodiment

[0095] Example 3

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

[0097] (1) The 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, the above materials are mixed, a certain amount of water is added, and the mass ratio of water to powder is 5:1. Corundum balls were used as grinding media, ball-milled in a corundum tank for 6 hours, the ball mill speed was 400 rpm, and the slurry after ball-milling was spray-granulated to obtain fluffy micron-sized spherical particles, which were wrapped by carbon precursor-soluble inorganic salts Accumulated with primary alumina particles;

[0098] (2) Transfer the micron-sized spherical particles into the corundum saggar, put the saggar into the microwave synthesis reaction chamber, use silicon carbide wafers as auxiliary heat, and pass normal pressure nitrogen to carry out powder sy...

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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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