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Reactive ultrasonic rectification and purification method for HF electronic gas

An electronic gas, purification method technology, applied in chemical instruments and methods, fractionation, compounds of elements of Group 4/14 of the periodic table, etc. Efficient water removal and other issues

Pending Publication Date: 2020-10-23
ZHEJIANG KAISN FLUOROCHEM +1
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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 HF electronic gas, which causes the strong reactivity and corrosion of HF, and causes secondary pollution of HF electronic gas by impurities such as metal ions, reduces the purity and consistency of HF electronic 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 HF 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 corrosiveness of aqueous HF , Oxide adsorption materials such as activated alumina, silica, silica-alumina oxide molecular sieves, etc. can react with HF, and cannot be used to efficiently remove water from HF. Carbon-based materials such as activated carbon have limited moisture adsorption efficiency and capacity in HF ; Moreover, HF is strongly hydrophilic, and HF also has a strong hydrogen bond with water, so it is difficult to effectively remove the water in HF to the ppb level by conventional distillation

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0027] A reactive ultrasonic distillation purification method for HF electron gas, the operation steps are:

[0028] Add 50Kg of moisture reactant to 1000Kg of liquefied HF, 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, and the bottom of the tower is Connect the reboiler, the hydrogen fluoride gas generated by the heating of the reboiler is condensed through the condenser, the reflux ratio is controlled to be between 1.2, 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 minus 20 °C, the temperature at the bottom of the tower is -10 °C; the liquefied HF after rectification is filtered through a filter membrane; the rectification tower is in an ultrasonic field, its ultrasonic frequency is 30KHz, and its ultrasonic power is 10W / cm2; it is cha...

Embodiment 2

[0038] A reactive ultrasonic distillation purification method for HF electron gas, the operation steps are:

[0039]Add 50Kg of moisture reactant to 1000Kg of liquefied HF, 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, and the bottom of the tower is Connect the reboiler, the hydrogen fluoride gas generated by the heating of the reboiler is condensed through the condenser, the reflux ratio is controlled to be between 1.2, 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 minus 20 °C, the temperature at the bottom of the tower is -10 °C; the liquefied HF after rectification is filtered through a filter membrane; the rectification tower is in an ultrasonic field, its ultrasonic frequency is 30KHz, and its ultrasonic power is 10W / cm2; it is char...

Embodiment 3

[0049] A reactive ultrasonic distillation purification method for HF electron gas, the operation steps are:

[0050] Add 100Kg of moisture reactant to 5000Kg of liquefied HF, 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, and the bottom of the tower is Connect the reboiler, the hydrogen fluoride gas generated by heating the reboiler is condensed by the condenser, the reflux ratio is controlled to be between 2.5, the theoretical plate number of the rectification column is 24, the rectification pressure is 15bar, and the tower top temperature is minus 40 °C, the temperature at the bottom of the tower is 5 °C; the liquefied HF after rectification is filtered through a filter membrane; the rectification tower is in an ultrasonic field, its ultrasonic frequency is 100KHz, and its ultrasonic power is 40W / cm2; it is characterized in that the ...

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Abstract

The invention relates to the field of high-purity gas purification, in particular to a reactive ultrasonic rectification and purification method for HF electronic gas. According to the reactive ultrasonic rectification and purification method for the HF electronic gas, a small amount of carbonyl fluoride and thionyl chloride are added into liquefied HF containing trace water respectively, and CO2or SO2 generated by a reaction of carbonyl fluoride or thionyl chloride with water is removed through rectification, so the purpose of HF dehydration and purification is achieved; besides, the liquefied HF is placed in an ultrasonic field for rectification and purification, so the reaction of carbonyl fluoride, thionyl chloride and trace moisture in the liquefied HF can be promoted, the escape ofCO2 or SO2 from the liquefied HF is accelerated, and the residue of CO2 or SO2 in the liquefied HF is effectively reduced; and the method belongs to a reactive conversion-ultrasonic degassing coupledmethod for water, and has the advantages of high purity and extremely low water 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 HF electron gas. Background technique [0002] HF 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 method of high-purity electronic gas. [0003] CN201810154986.6 discloses an electronic-grade hydrofluoric acid production device, including a tank body, a bracket is evenly arranged on the outside of the bottom of the tank body, a liquid inlet is arranged on one side of the top of the tank body, and the top of the tank body is far away from A fan is arranged on one side of the liquid inlet, and a gas delivery pipe is installed at the output end of the fan, and a condensation chamber is arranged in the middle of the side of the tank away from the liquid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/19B01D3/14C07F7/08
CPCC01B7/195B01D3/14C07F7/0889C01P2006/80Y02P20/10
Inventor 叶向荣程文海李军夏添赵晓亚张广第张晓东
Owner ZHEJIANG KAISN FLUOROCHEM
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