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Purification method and purification system of chlorine trifluoride

A technology of chlorine trifluoride and purification method, which is applied in the direction of interhalogen compounds, etc., and can solve the problems that the removal of light impurity components cannot be carried out at the same time, continuous rectification cannot be performed, and the content of metal ions is difficult to control.

Pending Publication Date: 2021-02-23
SUZHOU JINHONG GAS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process equipment has low investment and simple operation, continuous rectification cannot be carried out, and the removal of light impurity components (oxygen, nitrogen) and heavy components (hydrogen fluoride) cannot be carried out at the same time, and the content of metal ions in the product is difficult to control

Method used

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  • Purification method and purification system of chlorine trifluoride
  • Purification method and purification system of chlorine trifluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Use high-purity nitrogen to purge and replace the entire system, and use a vacuum pump to evacuate the system to a negative pressure of 0.5Pa.

[0058] Carry out helium leak detection on the system, because the chlorine trifluoride active agent is extremely toxic, it is necessary to ensure that the system is leak-free, and the system leak rate is lower than 1.0×10 -9 mbarL / s;

[0059] The liquid chlorine trifluoride crude product (its composition is shown in Table 2) from the chlorine trifluoride raw material storage tank is pressurized to 2.2 barg by the booster pump, and after passing through the vaporizer gasification, the outlet gas pressure is controlled to 2.2 barg, and the flow control is 5kg / h ;

[0060] The pressurized chlorine trifluoride gas enters the DN50mm×2000mm adsorption tower to absorb hydrogen fluoride (the adsorbent is sodium fluoride, potassium fluoride and calcium fluoride, the mass ratio is 5:3:2; the adsorbent is spherical and the particle size ...

Embodiment 2

[0065] Use high-purity nitrogen to purge and replace the entire system, and use a vacuum pump to evacuate the system to a negative pressure of 1pa.

[0066] Carry out helium leak detection on the system, because the chlorine trifluoride active agent is extremely toxic, it is necessary to ensure that the system is leak-free, and the system leak rate is lower than 1.0×10 -9 mbarL / s;

[0067] The liquid chlorine trifluoride crude product from the chlorine trifluoride raw material storage tank is pressurized to 2.2 barg by the booster pump, and the outlet gas pressure is controlled to be 2.2 barg after being vaporized by the vaporizer, and the flow rate is controlled to be 5kg / h;

[0068] The pressurized chlorine trifluoride gas enters the DN50mm×2000mm adsorption tower to absorb hydrogen fluoride (the mass ratio of the adsorbent is sodium fluoride, potassium fluoride and calcium fluoride is 6:2:2, the spherical particle size is 4-5mm, the average Pore ​​size 0.4nm; specific surf...

Embodiment 3

[0073] Use high-purity nitrogen to purge and replace the entire system, and use a vacuum pump to evacuate the system to a negative pressure of 1Pa.

[0074] Carry out helium leak detection on the system, because the chlorine trifluoride active agent is extremely toxic, it is necessary to ensure that the system is leak-free, and the system leak rate is lower than 1.0×10 -9 mbarL / s;

[0075] The liquid chlorine trifluoride crude product from the chlorine trifluoride raw material storage tank is pressurized to 2.2 barg by the booster pump, and the outlet gas pressure is controlled to be 2.2 barg after being vaporized by the vaporizer, and the flow rate is controlled to be 5kg / h;

[0076] The pressurized chlorine trifluoride gas enters the DN50mm×2000mm adsorption tower to absorb hydrogen fluoride (the mass ratio of the adsorbent is sodium fluoride, potassium fluoride and calcium fluoride is 3:2:2, the spherical particle size is 4-5mm, the average Pore ​​size 0.4nm; specific surf...

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Abstract

The invention provides a purification method of chlorine trifluoride, which comprises the following steps: S1) pressurizing and vaporizing a chlorine trifluoride crude product, and adsorbing with an adsorbent to obtain chlorine trifluoride gas without hydrogen fluoride, wherein the adsorbent is fluoride salt, S2) condensing the chlorine trifluoride gas from which hydrogen fluoride is removed to obtain condensed chlorine trifluoride liquid, and S3) carrying out two-stage rectification on the condensed chlorine trifluoride liquid to obtain high-purity chlorine trifluoride. Compared with the prior art, the method has the advantages that adsorption condensation and two-stage rectification are combined, the chlorine trifluoride crude product is firstly subjected to adsorption to remove part ofhydrogen fluoride and then is subjected to two-stage continuous rectification, hydrogen fluoride, oxygen, nitrogen and metal ions can be removed to reach very high purity, and the removal control of metal ion impurities can be further increased, so that the purity of the chlorine trifluoride crude product is improved. The method can be continuously carried out, the operation is stable, and the 3N-purity chlorine trifluoride product used in the semiconductor industry is obtained.

Description

technical field [0001] The invention belongs to the technical field of electronic materials, and in particular relates to a method and system for purifying chlorine trifluoride. Background technique [0002] Chlorine trifluoride (ClF 3 ) As a cleaning gas for semiconductor production, it has been used in low-pressure chemical vapor deposition (LPCVD) of polysilicon and SiN and plasma chemical vapor deposition (PCVD) of non-crystalline alloy silicon. [0003] The chemical vapor deposition (CVD) process in semiconductor manufacturing uses heat or plasma as the energy source to decompose the source gas on the silicon substrate. The film-forming reactions in low-pressure chemical vapor deposition (LPCVD) processes are driven by heat from a silicon wafer (cold-wall reactor) or a furnace (hot-wall reactor). The cold-wall LPCVD reactor is a typical single silicon wafer production device, while the LPCVD heating furnace can process silicon wafers in batches. [0004] During plasm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/24
CPCC01B7/24
Inventor 金向华温海涛王新喜孙猛汪民霞
Owner SUZHOU JINHONG GAS CO LTD
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