Preparation method of aluminum nitride powder

A technology of aluminum nitride and powder, which is applied in the field of preparation of aluminum nitride powder, which can solve the problems of large particle size, unstable quality, and decreased surface area, and achieve the effect of large reaction area and activity, and lower temperature

Active Publication Date: 2022-05-20
青州方舟新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since alumina and carbon basically do not react below 1100°C, intermediate species are mainly formed between 1100-1300°C and the reaction is slow. Therefore, before the temperature of the mixture reaches 1300°C, the self-sintering of the alumina microparticles, the interparticle Merger is inevitable, and the surface area will drop sharply. This problem may be one of the main reasons for the high nitriding reaction temperature, large product particle size, and unstable quality.
On the other hand, in order to convert the alumina raw material as much as possible, more than 20% of the carbon powder is generally added. This part of the remaining carbon needs to be removed during the oxidation treatment process at 600-800°C, but there will be Partial aluminum nitride oxidation, this step is usually not easy to achieve a reasonable balance of carbon content and oxygen content; an appropriate amount of oxygen is conducive to the sintering of aluminum nitride, but if the oxygen content is more than 1.2m%, it will reduce the aluminum nitride ceramics thermal conductivity; for example, more than 0.2m% carbon residue may not only make the aluminum nitride powder darker, but also may reduce the electrical insulation performance of the prepared ceramics
The average particle size of aluminum nitride powder is more than 1μm, or the specific surface area is less than 5m 2 / g, it is usually difficult to prepare dense ceramic products with high thermal conductivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare aluminum nitride powder according to the following steps:

[0031] A. Take a pseudo-boehmite dry powder M4kg (containing Al 2 o 3 2667g, average diameter 1.6μm, calcined at 400℃, the pore volume of alumina powder is 0.61ml / g, and the specific surface area is 385 m 2 / g, the specific surface area of ​​micropores with a diameter below 2nm is 260 m 2 / g, volume 0.16ml / g; Na300mg / kg, Fe47 mg / kg, Si260 mg / kg), carbon powder X1333g (water-soluble carbon black, ash content 180mg / kg, specific surface area 460 m 2 / g, 15nm) placed in a high-speed shearing machine for 60 minutes to crush and mix, then transferred to a kneader, added 4000ml of an aqueous solution containing 110g of acetic acid, kneaded for 1hr, and extruded most of the wet material through a hydraulic plunger into a diameter of Φ8mm Strips, the extruded strips were dried in an oven at 125°C for 6hrs, and the dried strips were roasted at 400°C for 4hrs under anaerobic conditions to obtain molding materia...

Embodiment 2

[0038] Take a part of the wet mass kneaded in Step B of Example 1 for 1 hr and press it into a columnar block of Φ40╳60mm by a hydraulic press, and dry it in an oven at 125°C for 10 hr; Anaerobic roasting and carbonization, as well as high-temperature reduction nitriding and charcoal burning operations, the main difference is that the carbon tube furnace nitrogen atmosphere is 1420 ℃ constant temperature reaction for 6 hours, and the muffle furnace and air atmosphere are 500 ℃ ╳ 16hr charcoal burning, until all materials are taken out and checked The surface and cross-section of the block are all very light in color; the light-colored aluminum nitride strip obtained after charcoal burning does not drop powder and is easy to crush.

Embodiment 3

[0040] Pseudoboehmite dry powder M3kg (containing Al 2 o 3 2000g), put carbon powder X1000g in a ball mill, add 6000ml of an aqueous solution containing 160g of acetic acid and 50g of polyacrylic acid (average molecular weight 3600), and spray granulate at 200-250°C after ball milling for 15 hours to obtain a particle with an average particle size of 146μm Granulated powder; the granulated powder was roasted at 420°C for 4hrs under anaerobic conditions to obtain molding materials; basically according to Steps B-E of Example 1, sucrose solution impregnation, drying, anaerobic roasting and carbonization, and high-temperature reduction nitriding and charcoal operations were performed , until the aluminum nitride powder is taken out and inspected, the color of the crushed aluminum nitride powder is all very light; the light-colored aluminum nitride strip obtained after charcoal burning does not drop powder and is easy to crush.

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Abstract

The invention provides a method for preparing aluminum nitride powder, which comprises the steps of: mixing and dispersing aluminum hydroxide powder and carbon powder, adding acid-containing aqueous solution, kneading or ball milling, forming, drying, roasting under anaerobic conditions, impregnating Sucrose or glucose solution and dried, roasted under anaerobic conditions, and / or through thermal cracking of introduced hydrocarbons, carbon deposits in the inner pores of the molding material, in a flowing nitrogen atmosphere, carry out reduction nitriding reaction at 1400‑1600 °C, and then Carry out low-temperature charcoal-burning treatment to produce aluminum nitride powder with low oxygen and carbon content. The present invention separates most of the alumina particles by generating carbon deposits in the inner pores of the alumina with larger specific surface area and inner pore volume, and significantly reduces the internal temperature of the alumina particles during the subsequent temperature rise and high-temperature reduction nitriding stages. And the sintering between particles, reduce the temperature of nitriding reaction or shorten the reaction time.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and in particular relates to a preparation method of aluminum nitride powder. Background technique [0002] Aluminum nitride (AlN) is a nitride material with rapid application development in recent years, which has high thermal conductivity, insulation performance and chemical stability. It can be kept stable at about 1500℃ in a non-oxidizing atmosphere and is not infiltrated and corroded by metals such as aluminum, copper, silver, and lead. It can be used as the basic ingredient for vacuum aluminum-plating evaporation boats, metal melting crucibles, and casting molds. It can be made GaAs crystal melting crucible. Properly prepared aluminum nitride ceramics have a thermal conductivity of over 180 w / m.k, good thermal shock resistance, and can be used as high-power circuit substrates; heat-conducting ceramics containing aluminum nitride also have a certain market. [0003] The basi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072
CPCC01B21/0726C01P2006/80C01P2006/12
Inventor 颜继鹏张春先王军令晓阳姜能明姜兴全
Owner 青州方舟新材料有限公司
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