A continuous purification method for high-purity tungsten hexafluoride

A technology of tungsten hexafluoride and purification method, which is applied in the direction of tungsten halide, etc., can solve the problems of low purity of tungsten hexafluoride, non-continuous operation, high cost, etc., and achieve excellent purification effect, increase production efficiency, and low cost.

Active Publication Date: 2022-03-22
PERIC SPECIAL GASES CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

[0008] To sum up, there are many existing literatures on the purification of tungsten hexafluoride, and the methods such as hydrogen fluoride removal adsorption tower and batch distillation tower are generally used. Generally, the purity requirements of crude tungsten hexafluoride gas are relatively strict, or continuous operation is not possible. The efficiency is low, the cost is high, and the purity of the produced tungsten hexafluoride is not high

Method used

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  • A continuous purification method for high-purity tungsten hexafluoride

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Experimental program
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Effect test

Embodiment 1

[0033] (1) Continuously fill the cooling circulation system with liquid nitrogen through the cooling medium inlet 2 to maintain the temperature of the low-temperature purification tower 1 at -180°C to -150°C, and vacuum the interior of the low-temperature purification tower 1 to below -0.07MPa ;

[0034] (2) Then, through the feed port I4, the tungsten hexafluoride crude product gas with a purity of 33.1vol% is continuously introduced into the low-temperature purification tower 1 (see Table 1 for its impurity composition and content), and the tungsten hexafluoride gas condenses rapidly. Huacheng solid, when the pressure in the low temperature purification tower 1 is higher than -0.03MPa, open the valve of the vent pipe 6 to release the pressure to -0.05MPa by vacuuming, discharge the impurity gas while releasing the pressure, and then close the vent pipe 6 When the pressure is higher than -0.03MPa again, the valve is repeatedly vented, and when the solid tungsten hexafluoride ...

Embodiment 2

[0043] (1) Continuously fill the cooling circulation system with liquid nitrogen through the cooling medium inlet 2 to maintain the temperature of the low-temperature purification tower 1 at -180°C to -150°C, and vacuum the interior of the low-temperature purification tower 1 to below -0.07MPa ;

[0044] (2) Then, through the feed port I4, the tungsten hexafluoride crude product gas with a purity of 83.2vol% is continuously introduced into the low-temperature purification tower 1 (see Table 3 for its impurity composition and content), and the tungsten hexafluoride gas condenses rapidly. Huacheng solid, when the pressure in the low temperature purification tower 1 is higher than 0MPa, open the valve of the open pipe 6 to release the pressure to -0.02MPa by vacuuming, and discharge the impurity gas while releasing the pressure, then close the valve of the pipe 6, wait When the pressure is higher than 0 MPa again, the emptying is repeated, and when the solid tungsten hexafluoride...

Embodiment 3

[0053] (1) Continuously fill the cooling circulation system with liquid nitrogen through the cooling medium inlet 2 to maintain the temperature of the low-temperature purification tower 1 at -180°C to -150°C, and vacuum the interior of the low-temperature purification tower 1 to below -0.07MPa ;

[0054] (2) Then, through the feed port I4, the tungsten hexafluoride crude product gas with a purity of 65.3vol% is continuously introduced into the low-temperature purification tower 1 (see Table 5 for its impurity composition and content), and the tungsten hexafluoride gas condenses rapidly. Huacheng solid, when the pressure in the low temperature purification tower 1 is higher than -0.01MPa, open the valve of the vent pipe 6 to release the pressure to -0.03MPa by vacuuming, discharge the impurity gas while releasing the pressure, and then close the vent pipe 6 When the pressure is higher than -0.01MPa again, the valve is repeatedly vented, and when the solid tungsten hexafluoride ...

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Abstract

The invention relates to a continuous purification method of high-purity tungsten hexafluoride, belonging to the field of fluorine-containing fine chemical separation technology. In the method, the impurity gas is firstly sublimated into a solid through a low-temperature purification tower, and then the tungsten hexafluoride with a purity of 99.9999 vol% is obtained through high-efficiency rectification by adjusting the rectification process parameters. The method of the invention can realize the purification of crude tungsten hexafluoride gas with a purity of more than 30 vol%, has wide application range, strong operability, high yield, low cost, high efficiency and is easy for large-scale production.

Description

technical field [0001] The invention relates to a continuous purification method of high-purity tungsten hexafluoride, belonging to the field of fluorine-containing fine chemical separation technology. Background technique [0002] Tungsten hexafluoride is the only tungsten fluoride that exists stably and is used in industrial production. In the production of ultra-large-scale circuits and semiconductor materials, the chemical deposition process of metal tungsten uses tungsten hexafluoride as the raw material. The use of chemical deposition process can largely avoid soft errors caused by uranium, thorium and other radioactive particles in memory circuits, and has the advantages of low resistivity, high resistance to electromigration, and excellent flatness. The tungsten hexafluoride required by the semiconductor industry has a fairly high purity in order to ensure the stability and yield of semiconductor products. [0003] Chinese patent CN104973629A is a method for purifyi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/04
CPCC01G41/04C01P2006/80C01P2002/82
Inventor 张琴张长金杨万吉王占卫彭立培张帅李丹丹胡帅王志民谢兵飞
Owner PERIC SPECIAL GASES CO LTD
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