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A kind of high-purity aluminum nitride powder and aluminum nitride powder purification method

A purification method, aluminum nitride technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve problems such as crystal cracking, high hardness, and impurity exclusion

Active Publication Date: 2021-05-04
SINOMA SYNTHETIC CRYSTALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] At present, there are two main methods for synthesizing aluminum nitride, one is vapor phase physical transport (PVT), and the other is hydride vapor phase epitaxy (HVPE). According to different synthesis principles, the HVPE method has a low synthesis temperature but a slow growth rate. , suitable for thin film growth; the disadvantage of the PVT method is that the synthesis temperature is high, but the synthesis speed is fast, so this method is suitable for bulk crystal growth
The growth of crystals by PVT method is the process of sublimation and decomposition of AlN powder in the high temperature area and crystal growth in the low temperature area, and the carbon and oxygen impurity elements brought by the powder during the growth process affect the properties of the crystal, such as the UV transmittance and thermal conductivity. , high pressure resistance, etc., and even the accumulation of a large number of impurity elements will cause problems such as crystal cracking. In order to solve this problem, the raw material powder needs to be cleaned of impurities. The current method of powder cleaning is to put the powder into a high temperature resistant crucible Then, through high-temperature calcination, the impurities in the powder are eliminated. After the removal of impurities, the powder becomes irregular cylindrical and ceramicized or even crystallized. The cylindrical structure is not conducive to the removal of impurities inside the block, and the high hardness of ceramicization is in the later stage. The crushing and grinding process brings great difficulties, resulting in excessive loss of powder, and the use of mechanical crushing can easily cause secondary pollution of raw materials

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

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Effect test

Embodiment 1

[0030] The aluminum nitride powder purification process of the present embodiment is:

[0031] S1. Mix high-purity Al powder (99.99%) and AlN powder according to the molar ratio of 0.1-0.5:1, and then mix them evenly according to the designed size ratio of the high-temperature calcined crucible (inner diameter of the crucible is Φ60mm, height 60mm), in an inert glove box The tungsten mold (or aluminum) is used to cold-press the mixed powder, and the powder with good fluidity is filled into the tungsten metal mold cavity. The molding pressure is 0.5-4MPa, and the powder is cold-pressed The cylindrical design allows the subsequent high-temperature calcination of the powder to be uniform, thereby facilitating manual crushing and grinding, and reducing secondary pollution caused by mechanical crushing and grinding. The outer diameter of the formed cylinder is 20mm, the ratio of the inner and outer diameters is greater than 1 / 3, and the height is 50-60mm (according to the size of t...

Embodiment 2

[0045] The aluminum nitride powder purification process of the present embodiment is:

[0046] S1. Mix high-purity Al powder (99.99%) and AlN powder according to the molar ratio of 0.1:1, and then mix them evenly according to the designed size ratio of the high-temperature calcined crucible (the inner diameter of the crucible is Φ60mm, and the height is 60mm). The tungsten mold (or aluminum) cold-presses the mixed powder, fills the powder with better fluidity into the tungsten metal mold cavity, and the molding pressure is 0.5-4MPa. It is designed so that the subsequent high-temperature calcination of the powder is uniform, which is beneficial to manual crushing and grinding, and reduces the secondary pollution caused by mechanical crushing and grinding. The outer diameter of the formed cylinder is 20mm, the ratio of the inner and outer diameters is greater than 1 / 3, and the height is 50-60mm (according to the size of the calcined crucible).

[0047] S2. Put the formed powder i...

Embodiment 3

[0060] The aluminum nitride powder purification process of the present embodiment is:

[0061] S1. Mix high-purity Al powder (99.99%) and AlN powder according to the molar ratio of 0.5:1, and then use them in an inert glove box according to the designed size ratio of the high-temperature calcined crucible (the inner diameter of the crucible is Φ60mm, and the height is 60mm). The tungsten mold (or aluminum) cold-presses the mixed powder, fills the powder with better fluidity into the tungsten metal mold cavity, and the molding pressure is 0.5-4MPa. It is designed so that the subsequent high-temperature calcination of the powder is uniform, which is beneficial to manual crushing and grinding, and reduces the secondary pollution caused by mechanical crushing and grinding. The outer diameter of the formed cylinder is 20mm, the ratio of the inner and outer diameters is greater than 1 / 3, and the height is 50-60mm (according to the size of the calcined crucible).

[0062] S2. Put th...

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Abstract

The invention relates to a high-purity aluminum nitride powder and a method for purifying the aluminum nitride powder. Use reducing gas to perform high-temperature gas washing treatment on the synthesis cavity where the mixed powder of Al powder and AlN powder is located, to remove the oxygen in the synthesis cavity; in a vacuum state, at the first purification temperature, remove the mixed Hydroxide in the powder impurities, at the second purification temperature, remove the carbon in the mixed powder impurities, and at the third purification temperature, use the Al steam to remove the aluminum oxide in the mixed powder impurities . The purification method is simple, through the rational design of the impurity removal sequence and the corresponding purification steps, and the addition of Al powder, the decomposition of AlN powder in the purification process is effectively suppressed, and the loss of raw materials is reduced. Through high-frequency combustion infrared absorption method and inert gas pulse Infrared thermal conductivity test shows that the carbon content of the aluminum nitride powder obtained in the present invention is 42PPM, the oxygen content is 220PPM, and the purity is high.

Description

technical field [0001] The invention relates to the preparation of aluminum nitride, in particular to a high-purity aluminum nitride powder and a method for purifying the aluminum nitride powder. Background technique [0002] Semiconductor materials and synthesis technology are the cornerstone of the development of modern information technology. In the 20th century, the first and second generation semiconductor materials represented by silicon (Si) and gallium arsenide (GaAs) promoted the rapid development of electronics and optoelectronic technology, and entered the 21st century. , with higher requirements for material performance, the third-generation semiconductor materials represented by aluminum nitride (AlN), silicon carbide (SiC), and gallium nitride (GaN) make up for the intrinsic properties of the first and second-generation materials Insufficient, has greatly promoted the development of the semiconductor industry. [0003] AlN has a direct band gap of 6.2eV, a wid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072
CPCC01B21/0722C01B21/0728
Inventor 周振翔陈建荣田庭燕何敬晖崔松满
Owner SINOMA SYNTHETIC CRYSTALS CO LTD