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A reactive ultrasonic distillation purification method for hcl electron gas

An electronic gas and purification method technology, applied in chlorine/hydrogen chloride purification, chemical instruments and methods, chlorine/hydrogen chloride, etc., can solve the problem of damage to semiconductor device performance and yield, moisture adsorption efficiency and limited capacity, HCL electronic gas purity, Consistency drops, etc.

Active Publication Date: 2021-12-17
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Moisture is one of the deadliest impurities in HCL electron gas, which triggers the strong reactivity and corrosion of HCL, causes secondary pollution of HCL electron gas by metal ions and other impurities, reduces the purity and consistency of HCL electron gas, and damages the performance of semiconductor devices and yield rate; the production of advanced micro-nano electronics requires strict control of the moisture content of HCL electronic gas to < 1 ppmv; the above inventions and existing patents generally use adsorbents and rectification to remove water, but due to the strong reactivity and Corrosive, oxide adsorption materials such as activated alumina, silica, silicon aluminum oxide molecular sieve, etc. can react with HCL, and activated alumina, silicon aluminum oxide molecular sieve, etc. can react with HCL, and cannot be used for efficient water removal of HCL , activated carbon and other carbon-based materials have limited adsorption efficiency and capacity for water in HCL; moreover, HCL is strongly hydrophilic and has a strong hydrogen bond with water, so it is difficult to effectively remove the water in HCL to the ppb level by conventional distillation

Method used

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  • A reactive ultrasonic distillation purification method for hcl electron gas

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Effect test

Embodiment 1

[0026] A reactive ultrasonic distillation purification method for HCL electron gas, the operation steps are:

[0027] Add 30Kg of thionyl chloride to 1000Kg of liquefied HCL, stir evenly in the mixing tank, and then pump the mixed liquid into the middle of the rectification tower for rectification. The top of the rectification tower is connected to the condenser. The bottom is connected to the reboiler, and the hydrogen chloride gas generated by the heating of the reboiler is condensed by the condenser, the reflux ratio is controlled to be between 10, the theoretical plate number of the rectification tower is 10, the rectification pressure is 5bar, and the temperature at the top of the tower is below zero 18°C, the temperature at the bottom of the tower is -10°C; the liquefied HCL after rectification is filtered through a filter membrane; the rectification tower is in an ultrasonic field, the ultrasonic frequency is 30KHz, and the ultrasonic power is 12W / cm 2 ; It is character...

Embodiment 2

[0037] A reactive ultrasonic distillation purification method for HCL electron gas, the operation steps are:

[0038] Add 65Kg of thionyl chloride into 3000Kg of liquefied HCL, stir evenly in the mixing tank, and then pump the mixed liquid into the middle of the rectification tower for rectification. The top of the rectification tower is connected to the condenser, the tower The bottom is connected to the reboiler, and the hydrogen chloride gas generated by the heating of the reboiler is condensed by the condenser, the reflux ratio is controlled to be 1.8, the theoretical plate number of the rectification tower is 18, the rectification pressure is 11bar, and the temperature at the top of the tower is minus 25°C , the temperature at the bottom of the tower is -3°C; the liquefied HCL after rectification is filtered through a filter membrane; the rectification tower is in an ultrasonic field, its ultrasonic frequency is 55KHz, and its ultrasonic power is 26W / cm 2 ; It is characte...

Embodiment 3

[0048] A reactive ultrasonic distillation purification method for HCL electron gas, the operation steps are:

[0049] Add 100Kg of thionyl chloride into 4000Kg of liquefied HCL, stir evenly in the mixing tank, and then pump the mixed liquid into the middle of the rectification tower for rectification. The top of the rectification tower is connected to the condenser, the tower The bottom is connected to the reboiler, and the hydrogen chloride gas generated by the heating of the reboiler is condensed by the condenser, the reflux ratio is controlled to be between 2.6, the theoretical plate number of the rectification tower is 26, the rectification pressure is 13bar, and the temperature at the top of the tower is below zero 41°C, the temperature at the bottom of the tower is 5°C; the liquefied HCL after rectification is filtered through the filter membrane; the rectification tower is in the ultrasonic field, the ultrasonic frequency is 100KHz, and the ultrasonic power is 36W / cm 2 ...

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Abstract

The present invention relates to the field of high-purity gas purification, and specifically relates to a reactive ultrasonic rectification and purification method of HCL electronic gas; a reactive ultrasonic rectification and purification method of HCL electronic gas of the present invention, and the present invention is used in liquefaction containing trace amounts of water A small amount of thionyl chloride is added to liquefied HCL, and the CO generated by the reaction of thionyl chloride and water is removed by rectification. 2 or SO 2 , to achieve the purpose of dehydration and purification of HCL; in addition, placing liquefied or liquefied HCL in an ultrasonic field for rectification and purification can promote the reaction of thionyl chloride with trace water in liquefied or liquefied HCL, and accelerate the CO 2 or SO 2 Evolution from liquefied or liquefied HCL, effectively reducing CO 2 or SO 2 Residue in liquefied or liquefied HCL; the invention belongs to the coupling method of moisture reactive conversion and ultrasonic degassing, and has the advantages of high purity and extremely low moisture content.

Description

technical field [0001] The invention relates to the field of high-purity gas purification, in particular to a reactive ultrasonic rectification and purification method for HCL electron gas. Background technique [0002] HCL electron gas is an important etching and cleaning gas in the manufacture of micro-nano electronics, currently completely dependent on imports; many domestic units are also actively exploring the preparation of high-purity electronic gas. [0003] 201910386663.4 provides a new method for the deep purification of electronic grade hydrogen chloride, a new purification material and its preparation method. By acidifying and acyl chlorinating the HCL corrosion-resistant high specific surface carbon material, its activity and selectivity for removing trace moisture in electronic grade hydrogen chloride are improved. Applying the new purification material to hydrogen chloride electron gas purification can reduce the moisture content of hydrogen chloride electron...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/07
CPCC01B7/0712
Inventor 叶向荣陈刚李军夏添张广第张晓东
Owner ZHEJIANG BRITECH CO LTD
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