A kind of high-purity aluminum nitride powder and its preparation method

A technology of aluminum nitride and powder, which is applied in the field of high-purity aluminum nitride powder and its preparation, can solve the problems of complex process and low purity of aluminum nitride powder, and achieve simple process, high single-shot output and uniform particle size Effect

Active Publication Date: 2018-09-11
HEBEI LIFU CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a high-purity aluminum nitride powder and its preparation method to solve the problems of low purity and complicated process of the aluminum nitride powder prepared in the prior art

Method used

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  • A kind of high-purity aluminum nitride powder and its preparation method
  • A kind of high-purity aluminum nitride powder and its preparation method
  • A kind of high-purity aluminum nitride powder and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 50g of metal Al powder with a purity of 99.99wt%, a spherical particle shape, and a particle size of 20μm in a glove box, and then weigh 5g of a reaction with a purity of 99.99wt%, a spherical particle shape, and a particle size of 2μm Additive AlN powder (additive A), mixed thoroughly for 20 minutes and then charged into a molybdenum crucible. Put the mixed material into the sintering furnace, evacuate it to 20KPa, feed in a nitrogen-hydrogen mixture with a volume ratio of 1:1, control the flow rate at 1.5L / min, and then raise the temperature at a rate of 5°C / min to 600°C, holding time 4h. Afterwards, the temperature was lowered to 300°C at a rate of 5°C / min, and naturally cooled to room temperature to obtain a primary sintered product, which was then ball milled in a glove box to about 3 μm for use.

[0025] Add reaction flux B (NH 4 HCO 3 and AlCl 3 The mixture, the mass ratio is 1:2) 1.67g, after fully mixing for 20 minutes, put it into the vacuum box furn...

Embodiment 11-17

[0033] With reference to the preparation method of Example 1, change the particle size of the primary sintered product to be used, NH in flux B 4 HCO 3 and AlCl 3 The ratio of other process conditions is the same as in Example 1. The N content and particle morphology of the aluminum nitride powder obtained are tested, and the results are shown in Table 2.

[0034] Table 2

[0035]

[0036] It can be seen from Table 2 that the particle size of the primary sintered product directly affects the particle size of the product, and the product particle size can be adjusted by changing the particle size of the primary sintered product as required. NH in flux B 4 HCO 3 with AlCl 3 The mass ratio of the product has a great influence on the particle size and uniformity of the product, and its optimal ratio is 1:2.

Embodiment 18-34

[0038] With reference to the preparation method of Example 1, the primary sintering conditions and secondary sintering conditions were changed, and other process conditions were the same as in Example 1. The N content and particle morphology of the prepared aluminum nitride powder were tested, and the results are shown in the table 3.

[0039] table 3

[0040]

[0041] It can be seen from Table 3 that by changing the temperature and holding time of the primary sintering and secondary sintering, as the sintering temperature increases, the nitriding rate first increases and then decreases, and the particle uniformity first becomes better and then gradually deteriorates , the particles agglomerate and the particle size becomes larger; with the extension of the holding time, the nitriding rate is slightly improved and the particle size becomes larger; when the primary sintering temperature is 600°C, the holding time is 4h, and the secondary sintering temperature is 900°C , whe...

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Abstract

The invention provides high-purity aluminum nitride powder. According to the powder, the AlN content is greater than or equal to 95.2%, the N content is greater than or equal to 32.5wt%, and the particle sizes are 1-5 microns. The invention further provides a method for preparing the high-purity aluminum nitride powder. The method comprises the steps of sintering specific aluminum powder through adding a reaction additive, adding the obtained product to a reaction flux and carrying out secondary sintering; and finally carrying out crushing and grading to obtain a product. The prepared high-purity aluminum nitride is high in purity and uniform in particle size; the preparation method is simple in technology, easy to operate and low in cost; the nitriding rate of the aluminum nitride powder is greatly improved; the high-purity aluminum nitride powder is controllable in particle size, high in yield and stable in batch performance; and industrial massive production can be carried out.

Description

technical field [0001] The invention relates to a nitride material, in particular to a high-purity aluminum nitride powder and a preparation method thereof. Background technique [0002] With the rapid development of modern electronic technology, the whole machine is required to develop in the direction of miniaturization, light weight, high integration and high reliability. At the same time, devices are becoming more and more complex, which will lead to an increase in the size of the substrate and an increase in integration, which will increase the power dissipation of the substrate. Therefore, the heat dissipation of the substrate and the selection of materials have become important issues. The thermal conductivity of AlN ceramics is higher than that of Al 2 o 3 Ceramics are 8 to 10 times higher, and their electrical properties such as volume resistivity, breakdown field strength, and dielectric loss are comparable to those of Al 2 o 3 Comparable to ceramics, with low ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072C04B35/626
CPCC01B21/0722C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2006/80C04B35/581C04B35/6265
Inventor 杨志平路亚娟许明亮赵金鑫
Owner HEBEI LIFU CHEM TECH
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