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Gas chromatography valve path system for analyzing multiple high-purity fluorine-containing electronic gases and using method of system

An electronic gas and gas chromatography technology, applied in the field of multi-dimensional gas chromatography valve circuit system, can solve the problems of single gas circuit, cumbersome operation, low analysis efficiency, etc., to reduce corrosion and influence, avoid pollution and damage, and reduce residual time. Effect

Active Publication Date: 2012-08-15
洛阳昊华气体科技有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the national standards and foreign standards (such as IEC, SEMI, ASTM, etc.) related to the detection of the above-mentioned high-purity fluorine-containing electronic gases, corresponding regulations have been made on the analysis methods of gas impurities, and some of them have clearly given the valve system. For example, "Industrial Sulfur Hexafluoride" (GB / T 12022-2006), "Gas Sulfur Hexafluoride for Electronic Industry" (GB / T 18867-2002), ASTM D2472-00 (SF 6 ), SEMI C3.24-0301 (SF 6 ), IEC 60376-2005 (SF 6 ), "Gas Nitrogen Trifluoride for Electronic Industry" (GB / T 21287-2007), SEMIC3.39-0999 (NF 3 ), SEMI C3.40-1000 (CF 4 ), SEMI C3.21-90 (CF 4 ), SEMIC3.37-0701 (C 2 f 6 ), SEMI C3.52-0200 (WF 6 ), SEMI C3.58-0303 (C 4 f 8 ), etc., but the gas path in the analysis methods listed in these standards is relatively single. To complete the analysis of a gas impurity, multiple instruments or multiple injections are required. The analysis efficiency is low, the operation is cumbersome, and the analysis cost is high. It is not suitable for industrial production. Analysis and detection of
[0004] US 20100154511A1 introduces a device and method for multidimensional gas chromatography, which uses a single-valve, three-column, and two-detector valve system, and focuses on the working principles of different types of switching valves. If there are many types of impurities in the main component , can’t meet the needs of analysis; CN102053129A introduces a chromatographic process that adopts two valves and two columns to analyze electronic grade carbon tetrafluoride. 2 , O 2 and CO separation and analysis; CN201780285U and CN101915811A introduce a device and method for analyzing and detecting impurities in high-purity non-corrosive gases, using four valves and five columns to analyze high-purity oxygen and other non-corrosive gases. Gas, introduces its working principle, through the valve circuit switching to analyze the large molecular weight and small molecular weight impurity components in the main component, only the rough separation of the components can be achieved

Method used

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  • Gas chromatography valve path system for analyzing multiple high-purity fluorine-containing electronic gases and using method of system
  • Gas chromatography valve path system for analyzing multiple high-purity fluorine-containing electronic gases and using method of system
  • Gas chromatography valve path system for analyzing multiple high-purity fluorine-containing electronic gases and using method of system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1: Separation and detection of gas-phase impurities in high-purity sulfur hexafluoride

[0052] Gas-phase impurities in sulfur hexafluoride with a purity of more than 99.999% mainly include: nitrogen (N 2 ), oxygen (O 2 ), carbon monoxide (CO), carbon dioxide (CO 2 ), methane (CH 4 ), carbon tetrafluoride (CF 4 ).

[0053] The pre-separation chromatographic column 6 is a silica gel chromatographic column with a length of 2 meters.

[0054] The first analytical chromatographic column 7 is a 5A molecular sieve chromatographic column with a length of 2 meters.

[0055] The second analytical chromatographic column 8 is a Hayesep Q chromatographic column with a length of 3 meters.

[0056] The third analytical chromatographic column 9 is a Hayesep Q chromatographic column with a length of 6 meters.

[0057] 1. Attached figure 1 In this state, the quantitative loop 24 is purged with the carrier gas, and the sulfur hexafluoride sample passes through the first f...

Embodiment 2

[0065] Example 2: Separation and detection of gas phase impurities in high-purity nitrogen trifluoride

[0066] Gas-phase impurities in nitrogen trifluoride with a purity of more than 99.99% mainly include: nitrogen (N 2 ), oxygen (O 2 ), carbon monoxide (CO), carbon dioxide (CO 2 ), carbon tetrafluoride (CF 4 ), nitrous oxide (N 2 O), sulfur hexafluoride (SF 6 ).

[0067] The pre-separation chromatographic column 6 is a Hayesep Q chromatographic column with a length of 2 meters.

[0068] The first analytical chromatographic column 7 is a 5A molecular sieve chromatographic column with a length of 2 meters.

[0069] The second analytical chromatographic column 8 is a Hayesep Q chromatographic column with a length of 3 meters.

[0070] The third analytical chromatographic column 9 is a Hayesep Q chromatographic column with a length of 6 meters.

[0071] 1. Attached figure 1 In this state, the quantitative loop 24 is purged with carrier gas, and the nitrogen trifluoride ...

Embodiment 3

[0079] Example 3: Separation and detection of gas phase impurities in high-purity tungsten hexafluoride

[0080] Gas-phase impurities in tungsten hexafluoride with a purity of more than 99.999% mainly include: nitrogen (N 2 ), oxygen (O 2 ), carbon monoxide (CO), carbon dioxide (CO 2 ), carbon tetrafluoride (CF 4 ), sulfur hexafluoride (SF 6 ).

[0081] The pre-separation chromatographic column 6 is a fluorine oil chromatographic column with a length of 4 meters.

[0082] The first analytical chromatographic column 7 is a 5A molecular sieve chromatographic column with a length of 2 meters.

[0083] The second analytical chromatographic column 8 is a Hayesep Q chromatographic column with a length of 3 meters.

[0084] The third analytical chromatographic column 9 is a Hayesep Q chromatographic column with a length of 6 meters.

[0085] 1. Attached figure 1 In this state, the quantitative loop 24 is purged with carrier gas, and the tungsten hexafluoride sample is collect...

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Abstract

The invention discloses a gas chromatography valve path system for analyzing multiple high-purity fluorine-containing electronic gases and a using method of the system. The system comprises 2 four-way valves, 2 ten-way valves, 1 eight-way valve, 1 quantitative ring, 4 chromatographic columns, 14 pressure balance regulation valves and 1 discharge ionization detector; and the carrier gas of the system is high-purity helium. According to the invention, a five-valve four-column valve path system is adopted, and the measurement of multiple gas-phase impurities can be finished by once sample introduction. The valve path system is convenient to operate and applicable to the industrial production in the field of high-purity fluorine-containing electronic gases.

Description

technical field [0001] The invention relates to a multidimensional gas chromatography valve circuit system, in particular to a gas chromatography valve circuit system for analyzing various high-purity fluorine-containing electronic gases. Background technique [0002] Fluorine-containing electronic gases are mainly used as cleaning agents and plasma etchant for chemical vapor deposition in electronics, semiconductor industry and photovoltaic industry. With the rapid development of related fields such as TFT-LCD panel industry, semiconductor industry and solar panel industry in recent years, the consumption of fluorine-containing electronic gases is also increasing. [0003] If impurities such as H in the high-purity fluorine-containing electron gas 2 , O 2 , N 2 、CH 4 , CO, CO 2 , N 2 If the content of O is too high, it will seriously affect its performance in cleaning and etching, so the requirements for analysis and detection are relatively high. At present, in the ...

Claims

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Application Information

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IPC IPC(8): G01N30/20G01N30/06
Inventor 黄晓磊牛学坤梁真镇张景利付梦月侯玲玲汤月贞张亚平
Owner 洛阳昊华气体科技有限公司
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