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Purification method and preparation method of high-purity chlorine trifluoride

A technology of chlorine trifluoride and purification method, which is applied in the field of purification method and preparation of high-purity chlorine trifluoride, and can solve the problems of low purity of chlorine trifluoride gas, failure to meet technical indicators, and high impurity of ClF

Pending Publication Date: 2021-09-10
鹤壁德瑞科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high HF impurities in fluorine gas, the low concentration of fluorine gas, and the high impurities of ClF produced affect the yield of chlorine trifluoride products, especially HF is difficult to be processed in depth. After chlorine trifluoride gas is rectified, the current HF The content ranges from 500PPm to 700PPm, and the concentration of chlorine trifluoride is only 99.9%, which cannot meet the high-purity quality requirements of the current microelectronics industry development, especially the technical indicators of high-purity chlorine trifluoride for HF
[0011] 3N chlorine trifluoride products will also add metal ion solid residues when cleaning the process chambers of PECVD and LPCVD (cold wall), which will pollute the CVD process chambers again
The absorption rate of hydrogen fluoride has been improved, but the disadvantage of low purity of chlorine trifluoride gas can only meet the quality index of 99.9%.
[0016] "A Purification Method for Chlorine Trifluoride" (CN112723313A) discloses a purification method for chlorine trifluoride, which only provides a production method, and does not have an adsorption system. Although there is also rectification equipment, the final quality index is only Can reach 99.1%
The process of this method is relatively simple, but the product quality cannot meet the high-purity chlorine trifluoride index requirements

Method used

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  • Purification method and preparation method of high-purity chlorine trifluoride
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  • Purification method and preparation method of high-purity chlorine trifluoride

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Embodiment 1

[0075] The purpose of this embodiment is to provide a kind of reactor 5 of high-purity grade chlorine trifluoride, comprise following structure:

[0076] The reactor 5 of this high-purity chlorine trifluoride comprises a housing 55, and a partition 57 is arranged in the housing 55, and the partition 57 is specifically arranged on the middle and upper part of the reactor 5 horizontally, and the housing The environment in 55 is divided into upper and lower areas. The upper part is the feeding chamber 5100, and the lower part is the reaction chamber 5101. The height of the upper feeding chamber 5100 is better than that of the lower reaction chamber 5101. The feeding chamber 5100 is used for automatic mixing of fluorine gas and chlorine gas. storage area; the feeding chamber 5100 and the reaction chamber 5101 communicate with each other through the through holes on the partition plate 57 .

[0077] The outer wall of the reactor 5 is covered with an electric heating blanket 54 for ...

Embodiment 2

[0082] The purpose of this embodiment is to provide a kind of purification method of high-purity grade chlorine trifluoride, comprises the steps:

[0083] S1. Condensation: Lead the produced chlorine trifluoride mixed gas into condenser 6 for condensation, the temperature of the condenser is controlled at -25°C, the pressure is -0.03Mpa, the liquid obtained by condensation is crude chlorine trifluoride, non-condensable gas and The unreacted fluorine gas is vented after being treated by the exhaust gas purification system;

[0084] S2. Recovery and vaporization: the chlorine trifluoride gas purified in step S3 passes through the recovery vaporizer 7, the temperature of the recovery vaporizer is controlled at 35°C, and the pressure is -0.02Mpa to further remove trace amounts of unreacted fluorine gas and non-condensable gas, trifluorine The concentration of chlorine chloride is controlled at 96-99%, and then the recovery vaporizer is heated and vaporized to provide pressure for ...

Embodiment 3

[0091] The purpose of this embodiment is to provide a kind of purification method of high-purity grade chlorine trifluoride, comprises the steps:

[0092] S1. Condensation: The produced chlorine trifluoride mixed gas is introduced into the condenser 6 for condensation. The temperature of the condenser is controlled at -40°C and the pressure is 0Mpa. The liquid obtained by condensation is crude chlorine trifluoride, non-condensable gas and unreacted The fluorine gas is vented after being treated by the exhaust gas purification system;

[0093] S2. Recovery and vaporization: the chlorine trifluoride gas purified in step S3 passes through the recovery vaporizer 7, the temperature of the recovery vaporizer is controlled at 43°C, and the pressure is 0.3Mpa, and traces of unreacted fluorine and non-condensable gases are further removed. The chlorine concentration is controlled at 96-99%, and then the recovery vaporizer is heated and vaporized to provide pressure for the low-pressure...

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Abstract

The invention provides a purification method and a preparation method of high-purity chlorine trifluoride, and relates to the technical field of chemical engineering. According to the method, high-purity chlorine trifluoride gas with the purity of 99.995% or above is obtained through condensation, vaporization, adsorption, filtration, rectification and filling. The purification method has the advantage that the purity of the chlorine trifluoride gas prepared by the purification method reaches 99.995%. According to the preparation method, the temperature and acidity of an electrolytic bath are controlled, and a HF adsorption tower is additionally arranged, so that the prepared fluorine gas can reach the optimal concentration, the utilization rate of the fluorine gas reaches 98% or above, and more favorable conditions are provided for subsequently providing chlorine trifluoride with higher concentration.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a purification method and preparation method of high-purity chlorine trifluoride. Background technique [0002] Chlorine trifluoride is a strong oxidant with high chemical reactivity and flammability. It can react explosively with water and organic compounds. It is mainly used in the electronics industry, nuclear industry, uranium enrichment and military affairs. High-purity chlorine trifluoride is mainly used in the cleaning of CVD chambers and pipelines in the fields of semiconductors, liquid crystals, solar energy, and LEDs. It has obvious advantages in cleaning quality, efficiency, and reducing the greenhouse effect. Unlike other fluorine-containing gases used for cleaning (such as NF 3 、C 2 f 6 and CF 4 ), chlorine trifluoride can react with semiconductor materials at room temperature, and there is no need to heat the cleaning part. Therefore, the use of chlo...

Claims

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Application Information

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IPC IPC(8): C01B7/24
CPCC01B7/24
Inventor 冉康德冀勇闫乃亮
Owner 鹤壁德瑞科技有限公司
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