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Method for preparing tungsten hexafluoride gas

A technology of tungsten hexafluoride and gas, which is applied in the field of preparation of tungsten hexafluoride gas, can solve the problems that the purity of tungsten hexafluoride products is difficult to meet the requirements of high-purity gas, high cost, and high purification cost

Active Publication Date: 2007-11-14
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

especially when junior WF 6 When the HF content in the gas is too high, purify and refine to produce high-purity WF 6 The cost of gas will be high
[0003] The traditional method uses ordinary fluorine gas and tungsten powder to directly react to prepare tungsten hexafluoride. Because fluorine gas contains more HF impurities and is introduced into the product, the purity of tungsten hexafluoride product is difficult to meet the requirements of high-purity gas, and the purification cost is high.

Method used

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  • Method for preparing tungsten hexafluoride gas

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Embodiment 1

[0018] As shown in the accompanying drawings, the entire preparation system is cleaned up in advance with a vacuum pump 1 by vacuuming. The purity of raw fluorine gas is 99%, of which H 2 The O content is 1 ppmv or less, and the HF impurity content is 10 ppmv. Fluorine gas and high-purity nitrogen enter the cracker 9 through pipelines 7 and 8 respectively at a weight ratio of 1:4 at a rate of 1 L / min for preheating. The preheating temperature is 80±5°C, the operating pressure is 0.2MPa, the gas residence time is 5min, and then enters the reactor 10 through the pipeline 5. The cracker 9 has a diameter of 100 mm, a length of 500 mm, and a coil pipe inside. The cracker 9 is made of Monel material. The reactor 10 has a diameter of 300 mm and a height of 600 mm, and is made of Monel material. 10kg of tungsten powder with a purity of 99.95% and a size of 80 mesh is added to the inside. The temperature of the reactor 10 is 150±10° C., the operating pressure is 0.2 MPa, and the re...

Embodiment 2

[0021] The whole preparation system is cleaned up by vacuuming in advance, as shown in the accompanying drawing. The raw material fluorine gas is replaced with nitrogen trifluoride gas. Raw material NF 3 The purity of the gas is 99.9%, and the contents of HF and water are both below 1ppmv. Raw material NF 3 Gas and high-purity nitrogen are passed into the cracker at a rate of 1 L / min at a ratio of 1:1. The operating temperature of the cracker is controlled at 450±10°C, the operating pressure is controlled at 0.2MPa, and the cracking time of the raw gas in the cracker is 5 minutes before entering the reactor. 10kg of tungsten powder with a purity of 99.95% and a size of 80 mesh was added to the reactor. The temperature of the reactor is 150±10°C, the operating pressure is 0.2MPa, and the reaction time between cracked gas and tungsten powder is 5min. synthetic WF 6 The gas is then liquefied and collected with a cryogenic collector. The temperature of the cryogenic collect...

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Abstract

The invention relates to a kind of preparation method of tungsten hexafluoride gas, mix (F2) and high purity nitrogen(N2 ) with proportion of 1:0.5-20 and add them into pyrolysis device, warm-up temperature is 10-100 degree C, pressure is 0-0.6 MPa, time used is for 1min-20min,then add them into reactor where there is raw material of wolframium (W)of 5-15Kg, the reaction temperature of fluorine gas and raw material of wolframium is between 20 degree C and 400 degree C, the reaction time is for1min-20min, fluidify and collect tungsten hexafluoride gas made in the reaction by wipe low-boiling impurity such as fluorine gas, nitrogen and nitrogen trifluoride off, after collect WF6 gas of 10kg-50kg in the low temperature collector, stop collecting it and heat up to press WF6 into carboy for keeping, using pipe to connect pyrolysis device, reactor and low temperature collector. Purity of tungsten hexafluoride gas is up to more than 99.5%.

Description

technical field [0001] The invention relates to a preparation method of tungsten hexafluoride gas. Background technique [0002] In tungsten fluoride, WF 6 It is the only variety that is stable and industrially produced. Its main use is as a raw material for metal tungsten chemical vapor deposition (CVD) process in the electronics industry, especially WSi made of it 2 Can be used as wiring material in large scale integration (LSI). The composite coating of tungsten and rhenium is prepared by mixed metal CVD process, which can be used in the manufacture of X-ray emitting electrodes and solar absorbers. In addition, WF 6 In the electronics industry, it is also mainly used as a raw material for semiconductor electrodes and conductive pastes. WF 6 There are also many non-electronic applications. For example, tungsten can generate hard tungsten carbide on the surface of steel by CVD technology, which can be used to improve the surface properties of steel. It can also be us...

Claims

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Application Information

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IPC IPC(8): C01G41/04
Inventor 李本东杨献奎王占卫李绍波袁晓燕隋希平董露荣
Owner PERIC SPECIAL GASES CO LTD
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