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Preparation method of high-purity tungsten hexafluoride

A tungsten hexafluoride, high-purity technology, applied in tungsten halide and other directions, can solve the problems of uneconomical, cumbersome post-processing, low product purity, etc., and achieve the effect of reducing processing cost, ensuring safety, and having high industrial application value.

Active Publication Date: 2017-04-26
南大光电(淄博)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of high-purity tungsten hexafluoride, which solves the problems of low product purity, uneconomical, and cumbersome post-processing existing in the existing process, and has the advantages of safety, economy, high product purity, energy saving, environmental protection, and impurity few features

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Examples

Experimental program
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Effect test

Embodiment 1

[0019] NF with a purity of 99.999% 3 into the cracker, in tungsten nitride and copper fluoride (W 2 N:CuF 2 =1:1) under the catalytic action of cracking, the cracking temperature is controlled at 300°C, the cracked gas enters the reactor at a flow rate of 2-3L / min, and reacts with the tungsten powder in the reactor at 500°C, and the reaction pressure is 0.2Mpa, the gas generated by the reaction is collected after condensation, and the crude product of tungsten hexafluoride is obtained. After distillation (10-30°C, 0-0.5Mpa) and rectification (15-30°C, 0-0.2Mpa), high-purity Tungsten hexafluoride gas.

[0020] The purity of the high-purity tungsten hexafluoride gas obtained in this implementation was tested, and the test results are shown in Table 1.

Embodiment 2

[0022] NF with a purity of 99.995% 3 into the cracker, in tungsten nitride and nickel fluoride (W 2 N:NiF 2 =1:8) under the catalytic action of cracking, the cracking temperature is controlled at 280°C, the cracked gas enters the reactor at a flow rate of 2-3L / min, and reacts with the tungsten powder in the reactor at 500°C, and the reaction pressure is 0.2Mpa, the gas generated by the reaction is collected after condensation, and the crude product of tungsten hexafluoride is obtained. After distillation (10-30°C, 0-0.5Mpa) and rectification (15-30°C, 0-0.2Mpa), high-purity Tungsten hexafluoride gas.

[0023] The purity of the high-purity tungsten hexafluoride gas obtained in this implementation was tested, and the test results are shown in Table 1.

Embodiment 3

[0025] NF with a purity of 99.96% 3 into the cracker, in tungsten nitride and ferric fluoride (W 2 N:FeF 3 =1:10) under the catalytic action of cracking, the cracking temperature is controlled at 250°C, the cracked gas enters the reactor at a flow rate of 2-3L / min, and reacts with the tungsten powder in the reactor at 500°C, and the reaction pressure is 0.2Mpa, the gas generated by the reaction is collected after condensation, and the crude product of tungsten hexafluoride is obtained. After distillation (10-30°C, 0-0.5Mpa) and rectification (15-30°C, 0-0.2Mpa), high-purity Tungsten hexafluoride gas.

[0026] The purity of the high-purity tungsten hexafluoride gas obtained in this implementation was tested, and the test results are shown in Table 1.

[0027] Table 1 Test results

[0028]

[0029] It can be seen from Table 1 that the product obtained by the preparation method of the present invention has high purity, and the subsequent treatment process is not complicate...

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Abstract

The invention relates to a preparation method of high-purity tungsten hexafluoride, and belongs to the technical field of fluorine chemical industry. The preparation method comprises the following steps: introducing nitrogen trifluoride gas into a cracker containing a catalyst to perform cracking; then enabling a fluorine-nitrogen mixture obtained by cracking to react with tungsten powder; performing condensation to obtain a tungsten hexafluoride crude product; and performing distillation and rectification to obtain tungsten hexafluoride of which the purity reaches 99.999%. The preparation method provided by the invention is safe and economical, the introduction of the catalyst ensures that nitrogen is not needed to be additionally introduced into a feed gas to ensure the safety of reaction, the purity of the obtained product reaches a 6N level, and the subsequent treatment cost is reduced, so that the preparation method is economical and environment-friendly and has great industrial application values.

Description

technical field [0001] The invention relates to a preparation method of high-purity tungsten hexafluoride, which belongs to the technical field of fluorine chemical industry. Background technique [0002] Among the tungsten fluorides, tungsten hexafluoride is the only species that exists stably and has been industrially produced. Its main use is as a raw material for metal tungsten chemical vapor deposition (CVD) process in the electronics industry, especially the products made of it. wxya 2 It can be used as a wiring material in a large scale integrated circuit (LSI), and a composite coating of tungsten and rhenium can also be prepared by a mixed metal CVD process for the manufacture of X-ray emitting electrodes and solar absorbers. In addition, high-purity tungsten hexafluoride is mainly used as a raw material for semiconductor electrodes and conductive pastes in the electronics industry. The purity of tungsten hexafluoride in LSI must be above 99.999%. The traditional p...

Claims

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Application Information

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IPC IPC(8): C01G41/04
CPCC01G41/04C01P2006/80
Inventor 宋学章周杰潘波李文田玲玲
Owner 南大光电(淄博)有限公司
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