Preparation method and application method of HF electron gas deep purification material

An electronic gas and application method technology, applied in chemical instruments and methods, hydrogen fluoride, inorganic chemistry, etc., can solve the problem of limited moisture adsorption efficiency and capacity, HF electronic gas purity, decreased consistency, damage to semiconductor device performance and yield, etc. problems, to achieve the effect of low moisture content, strong water absorption performance, and extreme moisture content

Active Publication Date: 2020-07-17
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 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, silicon aluminum 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, the adsorption efficiency and capacity of water in HF Limited; and HF is strongly hydrophilic, and HF also has a strong hydrogen bond with water. It is difficult to effectively remove the water in HF to the ppb level by conventional distillation

Method used

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  • Preparation method and application method of HF electron gas deep purification material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation and application method of a HF electron gas deep purification material, the preparation method of the material is as follows:

[0023] Dissolve 15.2g of acetate in 2000g of pure water, stir for 10min, after dissolving evenly, add 126.4g of disodium edetate, stir for 10min, form a mixed solution, then add 7.2g of ammonium fluoride, stir and mix evenly Add ammonia water dropwise to adjust the pH value of the solution to 9; then add 130g mesoporous activated carbon (AC) and 0.1g inducer sodium tetrafluoroborate, control the temperature at 40°C and stir for 20min, then transfer the mixture into a hydrothermal reaction kettle, and control the temperature Crystallization reaction at 140°C for 80min; then slowly cooled to room temperature, the material was filtered out, washed with absolute ethanol, repeated 3 times, and then the obtained material was dried in an oven at 120°C for 10h to obtain a metal fluoride-loaded activated carbon material AC / MF x •nH 2 O,...

Embodiment 2

[0032] A preparation and application method of a HF electron gas deep purification material, the preparation method of the material is as follows:

[0033] Dissolve 26.1g of acetate in 3000g of pure water, stir for 20min, after dissolving evenly, add 154.6g of disodium edetate, stir for 15min, form a mixed solution, then add 7.4g of ammonium fluoride, stir and mix evenly Add ammonia water dropwise to adjust the pH value of the solution to 10; then add 150g mesoporous activated carbon (AC) and 0.3g inducer sodium tetrafluoroborate, control the temperature at 50°C and stir for 30min, then transfer the mixture into a hydrothermal reaction kettle, and control the temperature Crystallization reaction at 160°C for 100min; then slowly cool to room temperature, filter out the material, and wash with absolute ethanol, repeat 4 times, then dry the obtained material in an oven at 140°C for 15h to obtain a metal fluoride-loaded activated carbon material AC / MF x •nH 2 O, after deep dehy...

Embodiment 3

[0042] A preparation and application method of a HF electron gas deep purification material, the preparation method of the material is as follows:

[0043] Dissolve 45.4g of acetate in 4000g of pure water, stir for 30min, after dissolving evenly, add 186.5g of disodium ethylenediaminetetraacetate, stir for 20min, form a mixed solution, then add 7.8g of ammonium fluoride, stir and mix evenly Add ammonia water dropwise to adjust the pH value of the solution to 11; then add 170g mesoporous activated carbon (AC) and 0.5g inducer sodium tetrafluoroborate, control the temperature at 60°C and stir for 50min, then transfer the mixture into a hydrothermal reaction kettle, and control the temperature Crystallization reaction at 180°C for 120min; then slowly cooled to room temperature, the material was filtered out, washed with absolute ethanol, repeated 5 times, and then the obtained material was dried in an oven at 160°C for 18h to obtain a metal fluoride-loaded activated carbon materia...

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Abstract

The invention relates to the field of high-purity gas purification, in particular to a preparation method and application method of an HF electronic gas deep purification material. The preparation method produces a metal fluoride-loaded activated carbon material AC / MFx-nH2O. After deeply dehydrating the material by using a carbonyl fluoride / high-purity nitrogen mixed gas flow, the HF electron gasdeep purification material AC / MFx is obtained, the material is provided with fluoride, can form crystal water and hydrated metal fluoride and has high water absorption performance, anhydrous fluorideand activated carbon cannot be corroded by HF, collapse of a framework structure and secondary pollution of reaction products to HF cannot be caused, and the method has the advantages of being high inpurity and extremely low in water content when used for efficiently removing water from HF.

Description

technical field [0001] The invention relates to the field of high-purity gas purification, in particular to a method for preparing and applying an HF electronic gas deep purification material. 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; exploring the preparation method of high-purity HF electron gas is of great significance for breaking foreign monopoly. [0003] 201811207404.2 involves a method of using a process device for preparing electronic-grade hydrogen fluoride. It is characterized in that fluorine gas is used to oxidize arsenic impurities in hydrogen fluoride to generate high boiling compound HAsF 6 , MAsF 6 , reusing the high boiler HAsF 6 , MAsF 6 Different from the volatility of HF and other components, multiple equilibrium processes are adopted to separate the mixture of multiple components into pure electronic-grade hydrogen fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/336C01B32/354C01B7/19
CPCC01B32/336C01B32/354C01B7/197Y02C20/30B01J20/027B01J20/20B01J20/3078B01J20/0237B01J20/046B01J20/3071B01J20/3085C09K13/08C01B7/191B01D53/0415B01D53/261B01D2253/102B01D2253/112B01D2253/25B01D2256/26B01D2257/80
Inventor 叶向荣周黎旸陈刚贺辉龙张学良李军周井森张云锋
Owner ZHEJIANG BRITECH CO LTD
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