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Preparation method of high-purity silicon tungsten powder

A high-purity, silicon-tungsten technology, applied in the field of powder metallurgy, can solve the problems of low product purity, low reduction temperature, and high oxygen content of high-purity silicon powder, and achieve the effect of broad application market, reducing C deposition, and reducing C content

Pending Publication Date: 2022-05-27
CHONGYI ZHANGYUAN TUNGSTEN
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Problems solved by technology

However, there are the following problems in the preparation of silicon tungsten powder by traditional technology: 1. The reduction temperature is low, the reaction time is long, and time-consuming; 2. The tubular reduction furnace is used, the equipment is complicated, and it is not energy-saving; 3. The product purity is low, and high-purity silicon tungsten cannot be obtained. powder products
[0005] In addition, due to the high oxygen content of high-purity silicon tungsten powder, silicon dioxide is easily generated during the preparation of silicon tungsten powder, resulting in impure components and high oxygen content of silicon tungsten powder, which cannot meet the requirements of high-purity silicon tungsten powder products. quality requirements

Method used

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preparation example Construction

[0025] The present invention provides a preparation method of high-purity silicon-tungsten powder, which is characterized in that, comprising the following steps:

[0026] (1) Mix the high-purity tungsten powder and the high-purity silicon powder uniformly in a three-dimensional mixer, wherein the mixing medium is high-purity silicon balls;

[0027] (2) The mixed powder is placed in a high-temperature sintering furnace for sintering, and a mixed gas of high-purity hydrogen and high-purity methane is first introduced to carry out the first sintering process, wherein the flow volume ratio of the mixed gas is H 2 :CH 4 1000:1~500:1, then turn off the methane, and pass in high-purity hydrogen to continue the second sintering process;

[0028] (3) The sintered silicon-tungsten powder is subjected to gas breaking treatment to prepare high-purity silicon-tungsten powder.

[0029] Further, in the embodiment of the present invention, the high-purity tungsten powder described in step ...

Embodiment 1

[0043] 1. The high-purity tungsten powder and the high-purity silicon powder are mixed evenly with argon gas as a protective gas in the three-dimensional mixer. Among them, the Si content is 29.7%, the mixing time is 3h, the mixing medium is high-purity silicon balls, and the ball-to-material ratio is 1:3.

[0044] 2. Put the mixed powder in a high-temperature sintering furnace for sintering, the sintering temperature is 1200 ℃, and the mixed gas of high-purity hydrogen and high-purity methane is introduced, and the gas flow ratio is H 2 :CH 4 1000:1, sintered for 2h; then turned off the methane, sintered with pure hydrogen for 1h, and passed high-purity argon to cool down after the reaction was completed.

[0045] 3. The sintered silicon-tungsten powder is subjected to gas breaking treatment to prepare high-purity silicon-tungsten powder.

[0046] 4. The Si content in the high-purity silicon-tungsten powder is 29.9%, the C content is 100ppm, and the O content is 400ppm.

Embodiment 2

[0048] 1. The high-purity tungsten powder and the high-purity silicon powder are mixed evenly with argon gas as a protective gas in the three-dimensional mixer. Among them, the Si content is 29.7%, the mixing time is 2h, the mixing medium is high-purity silicon balls, and the ball-to-material ratio is 1:2.

[0049] 2. Put the mixed powder in a high-temperature sintering furnace for sintering, the sintering temperature is 1300 ℃, and the mixed gas of high-purity hydrogen and high-purity methane is introduced, and the gas flow ratio is H 2 :CH 4 1000:1, sintered for 2 hours; then turned off the methane, sintered with pure hydrogen for 3 hours, and cooled with high-purity argon after the reaction was completed.

[0050] 3. The sintered silicon-tungsten powder is subjected to gas breaking treatment to prepare high-purity silicon-tungsten powder.

[0051] 4. The Si content in the high-purity silicon-tungsten powder is 29.7%, the C content is 60ppm, and the O content is 350ppm.

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Abstract

The invention relates to a preparation method of high-purity silicon-tungsten powder, and provides the preparation method of the high-purity silicon-tungsten powder in order to solve the problems that silicon dioxide is easily generated in the traditional silicon-tungsten powder preparation process, the oxygen content in the high-purity silicon-tungsten powder cannot be effectively reduced and the like. According to the preparation method, high-purity tungsten powder and high-purity silicon powder are used as raw materials, high-purity silicon tungsten powder aggregate is prepared after mixing and high-temperature sintering, and then the high-purity silicon tungsten powder with good dispersity is prepared after gas breaking treatment. By adopting the preparation method of the high-purity silicon-tungsten powder, the high-purity silicon-tungsten powder with better dispersity can be prepared, the requirement of a high-purity tungsten-silicon target material on a high-purity silicon-tungsten powder raw material can be better met, and the application market in the fields of electronic gate materials and electronic films is very wide.

Description

technical field [0001] The invention belongs to the field of powder metallurgy, and particularly relates to a preparation method of high-purity silicon-tungsten powder. Background technique [0002] Tungsten is a non-ferrous metal and an important strategic metal. Tungsten ore was called "heavy stone" in ancient times. Tungsten is a silver-white lustrous metal with high hardness and high melting point. It is not eroded by air at room temperature, and its chemical properties are relatively stable. China is the world's largest tungsten storage country. Tungsten has the advantages of high melting point, high strength, low thermal expansion coefficient, low resistivity, good thermal stability, etc., and is widely used in semiconductor integrated circuits, solar photovoltaic and other sputtering coating fields. Vacuum sputtering is that electrons collide with argon atoms in the process of accelerating to the substrate under the action of an electric field, ionizing a large numb...

Claims

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Application Information

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IPC IPC(8): B22F3/10B22F9/04
CPCB22F9/04B22F3/101B22F2009/041B22F2201/013B22F2201/00B22F2301/20
Inventor 张龙辉徐国钻周俊安羊求民王韶毅刘莉林丽萍黄春燕黄月玲
Owner CHONGYI ZHANGYUAN TUNGSTEN
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