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Tungsten hexafluoride gas purifying device and method

A technology of tungsten hexafluoride and purification equipment, which is applied in chemical instruments and methods, specific gas purification/separation, tungsten halide, etc., can solve the problems of HF content reduction, high raw material gas purity requirements, high production cost, etc., and achieve simplified production The effect of process, low cost and high yield

Active Publication Date: 2016-03-23
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

for WF 6 The removal of HF impurities in the gas mainly adopts the fluoride adsorption method, but the adsorption method is difficult to reduce the HF content to 0.5×10 -6 the following
In addition, the purification method has high requirements on the purity of the feed gas, resulting in higher production costs

Method used

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  • Tungsten hexafluoride gas purifying device and method
  • Tungsten hexafluoride gas purifying device and method
  • Tungsten hexafluoride gas purifying device and method

Examples

Experimental program
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Effect test

Embodiment 1

[0036]In the tungsten hexafluoride purification device used in this embodiment:

[0037] The volume of the rectification kettle 2 is 100L, the volume of the condenser 4 is 5L, the diameter of the rectification column 3 is 30mm, the height is 1500mm, and the θ ring packing with an equivalent diameter of 2mm is filled, the filling height of the packing is 1200mm, and the number of theoretical plates is 80 . The raw material storage tank 1 , rectification kettle 2 , rectification column 3 , condenser 4 , crude product storage tank 5 , fine product storage tank 6 , pipelines and fillers are made of stainless steel.

[0038] A method for purifying tungsten hexafluoride, the method is purified using a purification device for tungsten hexafluoride described in this embodiment, and the steps are as follows:

[0039] 140kg of crude tungsten hexafluoride with a purity of 90% and a volume percentage of HF of 5.25% in the raw material storage tank 1 was passed as a raw material into the ...

Embodiment 2

[0049] In the tungsten hexafluoride purification device used in this embodiment:

[0050] The rectification kettle 2 has a volume of 100L, the condenser 4 has a volume of 5L, the rectification column 3 has a diameter of 40mm and a height of 2500mm, and is filled with a θ ring packing with an equivalent diameter of 4mm, the filling height of the packing is 2300mm, and the number of theoretical plates is 100 . The raw material storage tank 1 , rectification kettle 2 , rectification column 3 , condenser 4 , crude product storage tank 5 , fine product storage tank 6 , pipelines and fillers are made of nickel.

[0051] A method for purifying tungsten hexafluoride, the method is purified using a purification device for tungsten hexafluoride described in this embodiment, and the steps are as follows:

[0052] 220kg of crude tungsten hexafluoride with a purity of about 80% and a volume percentage of HF of 9.98% in the raw material storage tank 1 is passed as a raw material into the r...

Embodiment 3

[0062] In the tungsten hexafluoride purification device used in this embodiment:

[0063] The volume of the rectifying kettle 2 is 200L, the volume of the condenser 4 is 10L, the diameter of the rectifying column 3 is 100mm, the height is 3500mm, and the Raschig ring packing with an equivalent diameter of 8mm is filled, the filling height of the packing is 3300mm, and the number of theoretical plates is 150. The raw material storage tank 1, rectification kettle 2, rectification column 3, condenser 4, crude product storage tank 5, fine product storage tank 6, pipelines and fillers are made of Monel.

[0064] A method for purifying tungsten hexafluoride, the method is purified using a purification device for tungsten hexafluoride described in this embodiment, and the steps are as follows:

[0065] 600 kg of crude tungsten hexafluoride with a purity of about 90% and a volume percentage of HF of 5.03% in the raw material storage tank 1 is passed as a raw material into the rectifi...

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Abstract

The invention relates to a tungsten hexafluoride gas purifying device and method and belongs to the field of chemical engineering separation. The device is mainly composed of a rectification kettle, a rectification column and a condenser. Crude product WF6 gas with the purity smaller than or equal to 99% and the HF content being 1-10% is introduced into the rectification kettle, the temperature of the rectification kettle is controlled to be 30-60 DEG C, pressure is controlled to be 0.10-0.40 MPa, the temperature of the condenser is 20-50 DEG C, pressure is 0.05-0.35 MPa, the WF6 liquid is vaporized to rise and liquified to flow back, mass transfer separation happens to WF6 of a gas phase and a liquid phase in the rectification column, and therefore the purpose of removing N2, O2, CO, CO2, CF4, SiF4, SF6, N2O and HF impurities is achieved. The method is simple in technology and low in cost, 99.9999% high-purity WF6 gas can be obtained with gas low in purity and high in HF content as raw materials, and the HF content can be lowered to 0.5*10<-6> or below.

Description

technical field [0001] The invention relates to a purification device and method for tungsten hexafluoride gas, belonging to the field of chemical separation. Background technique [0002] Tungsten hexafluoride (WF 6 ) is the only stable and industrially produced variety of tungsten fluoride, which is mainly used in the field of electronics. In the electronics industry, it is mainly used as a raw material for metal tungsten chemical vapor deposition (CVD) process. Tungsten deposited by the CVD process has the advantages of low resistivity, high resistance to electromigration, and excellent planarity when filling small vias. The above applications often require the purity of tungsten hexafluoride to be over 99.9999%, and the HF content to be lower than 0.5×10 -6 Only then can the stability and reliability of the production products be guaranteed. [0003] High-purity tungsten hexafluoride gas is generally obtained through multiple steps such as primary tungsten hexafluori...

Claims

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Application Information

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IPC IPC(8): C01G41/04
CPCC01B2210/0009C01B2210/0042C01B2210/0043C01B2210/0056C01G41/04
Inventor 张长金彭立培柳彤王占卫郑秋艳董云海张净普
Owner PERIC SPECIAL GASES CO LTD
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