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CN-117288902-B - Analysis method of fluorine-containing gas

CN117288902BCN 117288902 BCN117288902 BCN 117288902BCN-117288902-B

Abstract

The scheme belongs to the technical field of gas analysis, and particularly relates to an analysis method of fluorine-containing gas. The method for analyzing the pure fluorine gas comprises the following steps of S10-S80, S10, namely closing a first valve, a second valve, a third valve, a fourth valve, a fifth valve and an eighth valve, opening the first pressure reducing valve, the second pressure reducing valve and the third pressure reducing valve, S20, namely slowly opening the sixth valve and the second valve in sequence, venting for 10min, and closing the sixth valve and the second valve, and K10-SK90, wherein the method comprises the steps of K10, namely closing the fifth valve, the second valve, the eighth valve, the sixth valve, the third valve, the fourth valve and the first valve, and opening the first pressure reducing valve, the second pressure reducing valve, the third pressure reducing valve and the seventh valve. The method is simple and convenient to operate, high in operability and safety performance, air in the pipeline is sucked through the injection port of the venturi tube, then the air is discharged from the outlet of the venturi tube, efficient and thorough replacement of the air in the pipeline is realized, and the analysis result is more accurate and real.

Inventors

  • LEI HAIPING
  • LIU JIANLAN
  • RAN FANG

Assignees

  • 欧中电子材料（重庆）有限公司

Dates

Publication Date
20260508
Application Date
20231014

Claims (9)

  1. 1. An analysis method of fluorine-containing gas, characterized by comprising: comprises the steps of S1-S7, replacing the pipeline, Step S1, all valves are in a closed state, the first pressure reducing valve (109) is adjusted to 5-8barg, the first valve (101), the fifth valve (105) and the seventh valve (107) are opened, the second pressure gauge (113) is reduced to negative pressure, when the pointer of the second pressure gauge (113) is unchanged for 1-2min, the fifth valve (105) and the seventh valve (107) are closed, Step S2, a third pressure reducing valve (111) is adjusted to 2-5barg, a third valve (103), a fourth valve (104) and a seventh valve (107) are sequentially opened, the second pressure reducing valve (110) is adjusted to 1-5psig, and high-purity nitrogen enters the analyzer to the specified pressure; step S3, closing the third valve (103), opening the fifth valve (105), and reducing the second pressure gauge (113) to negative pressure; step S4, opening the second valve (102), and closing the fifth valve (105) and the second valve (102) when the pointer of the second pressure gauge (113) is unchanged for 1-2 min; step S5, opening a valve third valve (103), and enabling a second pressure gauge (113) to reach a specified pressure; Step S6, repeating the operation steps S3-S5 for 60 times to finish replacement; Step S7, after replacement, sampling analysis can be performed until the pressure reaches the specified pressure in the analyzer, and if the replacement is thorough, repeating the steps S1-S6 until the replacement is qualified; comprising the steps of S10-S80 of analyzing pure fluorine gas, Step S10, closing a first valve (101), a second valve (102), a third valve (103), a fourth valve (104), a fifth valve (105) and an eighth valve (108), and opening a first pressure reducing valve (109), a second pressure reducing valve (110) and a third pressure reducing valve (111); Step S20, sequentially and slowly opening a sixth valve (106) and a second valve (102), and after emptying for 10min, closing the sixth valve (106) and the second valve (102); Step S30, sequentially opening a first valve (101), a fifth valve (105) and a seventh valve (107), and reducing the second pressure gauge (113) to negative pressure; Step S40, when the second valve (102) and the fourth valve (104) are opened and the pointer of the second pressure gauge (113) is unchanged for 1-2min, sequentially closing the fifth valve (105), the second valve (102), the fourth valve (104) and the first valve (101); Step S50, sequentially and slowly opening a sixth valve (106) and a fourth valve (104), and closing the sixth valve (106) when the second pressure gauge (113) reaches a specified pressure; Step S60, sequentially opening the first valve (101) and the fifth valve (105), reducing the second pressure gauge (113) to negative pressure, opening the second valve (102), sequentially closing the fifth valve (105), the second valve (102), the fourth valve (104) and the first valve (101) when the pointer of the second pressure gauge (113) is unchanged for 1-2min, Step S70, the sixth valve (106) and the fourth valve (104) are opened slowly, when the second pressure gauge (113) reaches the specified pressure, the fourth valve (104) and the sixth valve (106) are closed, the analyzer analyzes the pure fluorine gas, Step 80, after analysis is finished, sequentially opening a first valve (101), a fifth valve (105), a second valve (102) and a fourth valve (104), and sequentially closing the fifth valve (105), the second valve (102), the fourth valve (104) and the first valve (101) when the second pressure gauge (113) drops to negative pressure and the pointer of the second pressure gauge (113) is unchanged for 1-2 min; Comprises the following steps of K10-SK90, analyzing fluorine-containing mixed gas, Step K10, closing a fifth valve (105), a second valve (102), an eighth valve (108), a sixth valve (106), a third valve (103), a fourth valve (104) and a first valve (101), opening a first pressure reducing valve (109), a second pressure reducing valve (110), a third pressure reducing valve (111) and a seventh valve (107), Step K20, sequentially opening the third valve (103) and the eighth valve (108), closing the third valve (103) until the air flow becomes weak, opening the third valve (103), continuously closing and opening the third valve (103) for at least 30 times, Step K30, adjusting the eighth valve (108) until the air flow is small, and screwing the joint of the fluorine-containing mixed gas bottle valve on the belt air; step K40, closing the third valve (103), opening the first valve (101) and the second valve (102) until no airflow sound exists, and closing the second valve (102), the eighth valve (108) and the first valve (101); step K50, after the fluorine-containing mixed gas bottle valve is slowly opened, the eighth valve (108) and the fourth valve (104) are sequentially opened, and the third pressure gauge (114) has pressure, so that no leakage is ensured at the joint of the bottle valve; Step K60, slowly opening a fluorine-containing mixed gas bottle valve, closing a fourth valve (104) and an eighth valve (108) by a second pressure gauge (113) to a specified pressure; Step K70, sequentially opening the first valve (101), the fifth valve (105), the second valve (102) and the fourth valve (104), and sequentially closing the fifth valve (105), the second valve (102) and the first valve (101) when the second pressure gauge (113) is reduced to negative pressure and the pointer of the second pressure gauge (113) is unchanged for 1-2 min; Step K80, opening an eighth valve (108), closing a fourth valve (104), the eighth valve (108) and a fluorine-containing mixed gas bottle valve when the second pressure gauge (113) II reaches a specified pressure, analyzing the fluorine-containing mixed gas by an analyzer, Step K90, after analysis is finished, sequentially opening a first valve (101), a fifth valve (105), a second valve (102), an eighth valve (108) and a fourth valve (104), wherein the second pressure gauge (113) is reduced to negative pressure, and when the pointer of the second pressure gauge (113) is unchanged for 1-2min, sequentially closing the fifth valve (105), the second valve (102), the eighth valve (108), the fourth valve (104) and the first valve (101); The analysis device for the fluorine-containing gas for realizing the method comprises a first passage, a second passage, a third passage and a fourth passage; The first passage is sequentially provided with a common nitrogen inlet pipeline, a first pressure reducing valve (109), a first pressure gauge (112), a first valve (101), a one-way valve and a venturi tube, wherein the common nitrogen inlet pipeline, the first pressure reducing valve (109), the first pressure gauge (112), the first common valve, the one-way valve and the inlet of the venturi tube are communicated through pipelines, The second passage comprises a fluorine gas inlet pipeline, a sixth valve (106), a fourth valve (104), a second pressure reducing valve (110), a second pressure gauge (113), a seventh valve (107) and an analyzer which are sequentially arranged, wherein the fluorine gas inlet pipeline, the sixth valve (106), the fourth valve (104), the second pressure reducing valve (110), the second pressure gauge (113), the seventh valve (107) and the analyzer are communicated through pipelines, the fourth valve (104) is also communicated with a third pressure gauge (114) through a pipeline, a second valve (102) is communicated between the sixth valve (106) and an injection port of a venturi tube through a pipeline, an exhaust end of the analyzer is communicated with a fifth valve (105) through a pipeline, the fifth valve (105) is respectively communicated with an injection port of the venturi tube and the second valve (102), The third passage comprises a third pressure reducing valve (111), a fourth pressure gauge (115) and a third valve (103) which are sequentially arranged, the third pressure reducing valve (111), the fourth pressure gauge (115) and the third valve (103) are communicated through pipelines, two ends of the third valve (103) are respectively communicated with the second valve (102) and the fourth valve (104) through pipelines, The fourth passage comprises a fluorine-containing mixed gas bottle body (1) and an eighth valve (108), wherein the fluorine-containing mixed gas bottle body (1) is communicated with the eighth valve (108) through a pipeline, and the eighth valve (108) is respectively communicated with the second valve (102) and the sixth valve (106) through pipelines; The fluorine-containing mixed gas bottle body (1) is hollow cylindrical, the air valve (2) is arranged at the top of the bottle body (1), the bottle mouth (3) is arranged at the top of the bottle body (1), the air valve (2) is used for closing the bottle mouth (3), the air valve (2) is detachably connected with the bottle body (1), the vent pipe (4) is arranged in the bottle body (1), the vent pipe (4) is communicated with the bottle mouth (3), the vent pipe (4) is a spring, the vent pipe (4) is hollow, the permanent magnet (5) is arranged on the vent pipe (4), the base (6) is provided with the base (6) which is provided with the electromagnet (7) corresponding to the permanent magnet (5), the permanent magnet (5) and the electromagnet (7) are in homopolar repulsion, the coil (8) is wound around the bottle body (1), the coil (8) is connected with the input wire and the output wire, a closed loop is formed between the output wire and the input wire, the electromagnet (7) is arranged on the closed loop, the bottom end of the vent pipe (4) is provided with the closing mechanism which comprises the supporting plate (9), the supporting rod (10), the sucking disc and the pipe plug (12) is used for fixing the vent pipe (4) with the end of the vent pipe (9), the upper end of the supporting rod (10) is hinged on the supporting plate (9), the lower end of the supporting rod (10) is fixedly connected with the pipe plug (12), a chute used for rotating the supporting rod (10) is arranged on the supporting plate (9), a limiting groove (13) matched with the supporting rod (10) is arranged on the supporting plate (9), the limiting groove (13) is used for preventing the supporting rod (10) from moving downwards, and a push rod (11) used for pushing the bottle plug downwards is arranged at the top in the bottle body (1).
  2. 2. The method for analyzing fluorine-containing gas according to claim 1, further comprising step S100 of sequentially opening the third valve (103), the fourth valve (104) and the fifth valve (105) for flow purging if the analyzer is not used for a long time.
  3. 3. The method of analyzing a fluorine-containing gas according to claim 1, further comprising a step K100 of sequentially opening the third valve (103), the fourth valve (104) and the fifth valve (105) to purge the flow if the analyzer is not used for a long time.
  4. 4. The method according to claim 1, further comprising an operation panel, wherein the first pressure reducing valve (109), the first pressure gauge (112), the first valve (101), the check valve, the sixth valve (106), the fourth valve (104), the second pressure reducing valve (110), the second pressure gauge (113), the seventh valve (107), the analyzer, the third pressure reducing valve (111), the fourth pressure gauge (115), the third valve (103) and the eighth valve (108) are all in communication connection or electrically connected with the operation panel.
  5. 5. The method for analyzing fluorine-containing gas according to claim 1, wherein the first pressure reducing valve (109), the second pressure reducing valve (110) and the third pressure reducing valve (111) are used for converting high-pressure gas into low pressure, the pressure reducing valves are composed of a valve body, a diaphragm, a valve seat, a valve rod, a valve cap and a handle, and the valve body is 316L.
  6. 6. The method according to claim 1, wherein the first pressure gauge (112), the second pressure gauge (113), the third pressure gauge (114) and the fourth pressure gauge (115) are elastic elements and are used as sensing elements for measuring and indicating the pressure higher than the ambient pressure, and the first pressure gauge (112), the second pressure gauge (113), the third pressure gauge (114) and the fourth pressure gauge (115) are composed of overflow holes, pointers and glass panels.
  7. 7. The method of claim 1, wherein the check valve comprises a valve body, a valve core, a spring and a sealing ring, and the valve body is 316L.
  8. 8. The method for analyzing a fluorine-containing gas according to claim 1, wherein the venturi is 316L.
  9. 9. The method of analyzing fluorine-containing gas according to claim 1, wherein the valve bodies of the first to eighth valves (101) to (108) are each composed of a valve body, a diaphragm, a valve seat, a valve stem, a bonnet, and a handle, and the valve body is 316L.

Description

Analysis method of fluorine-containing gas Technical Field The scheme belongs to the technical field of gas analysis, and particularly relates to an analysis method of fluorine-containing gas. Background Fluorine is a nonmetallic element with the strongest electronegativity and the most active chemical property, and can almost act with all elements. Fluorine (F2) is used in the semiconductor industry as an etching gas or cleaning gas for the manufacture of photovoltaic cells and TFTs (thin film transistors) for liquid crystal displays because of its reactive properties. F 2 is used as a cleaning agent of a CVD reaction chamber, has stronger reactivity compared with NF 3 and does not cause greenhouse effect, and metal fluoride generated by the reaction of fluorine gas, metal tungsten or germanium and the like can be used as vapor deposition gas or doping gas in the field of semiconductor manufacturing, and high-purity fluorine gas can be mixed with inert gases such as nitrogen, helium, neon, argon and the like in any concentration ratio to prepare mixed gas which is used as laser gas. Therefore, in the field of semiconductors, fluorine gas has great application potential, but the purity requirement of the industry on the fluorine gas is higher and higher, and the purity of the fluorine gas is gradually increased from 99.7 percent (volume ratio) to more than 99.99 percent (volume ratio). However, analysis of each impurity in fluorine gas is difficult, and particularly, analysis of HF has not been suitable in the industry. The patent of CN216747582U discloses a device for detecting the HF content in fluorine gas, which comprises a constant volume sampling pipe, a conversion column system and a vacuum pump which are sequentially connected by pipelines, wherein a vacuumizing valve is connected between the conversion column system and the vacuum pump in series through the pipelines, two ends of the vacuum valve are connected with an absorption bottle system in parallel through the pipelines, absorption liquid is arranged in the absorption bottle system, a fluorine gas conversion agent is filled in the conversion column system, and a fluorine gas sampling valve and an inert gas purging valve are respectively arranged on the constant volume sampling pipe. In the analysis process, a constant volume sampling tube is used for collecting fluorine gas to be detected in a certain volume, then inert gases such as high-purity nitrogen or helium, argon, radon and the like are used for driving and replacing the fluorine gas into a conversion column, and a fluorine gas conversion agent is filled in the conversion column, so that the fluorine gas can be converted into substances which do not interfere with HF detection. However, the solution can only convert fluorine gas into substances which do not interfere with HF detection, but can not replace air in a pipeline, and the air contains various gases, so that the analysis result is affected to a certain extent, and the analysis result is not truly accurate. Disclosure of Invention The scheme provides the method for analyzing the fluorine-containing gas, which has the advantages of true and accurate analysis results. In order to achieve the above object, the present invention provides a method for analyzing fluorine-containing gas, Comprises the steps of S1-S7, replacing the pipeline, Step S1, all valves are in a closed state, the first pressure reducing valve is regulated to 5-8barg, the first valve, the fifth valve and the seventh valve are opened, the second pressure gauge is reduced to negative pressure, when the pointer of the second pressure gauge is unchanged for 1-2min, the fifth valve and the seventh valve are closed, Step S2, a third pressure reducing valve is regulated to 2-5barg, a third valve, a fourth valve and a seventh valve are sequentially opened, the second pressure reducing valve is regulated to 1-5psig, and high-purity nitrogen enters the analyzer to the specified pressure; s3, closing the third valve, opening the fifth valve, and reducing the second pressure gauge to negative pressure; s4, opening a second valve, and closing a fifth valve and the second valve when the pointer of the second pressure gauge is unchanged for 1-2 min; And S5, opening a third valve of the valve, and enabling the second pressure gauge to reach the specified pressure. And S6, repeating the operation steps S3-S5 for 60 times to finish replacement. Step S7, after replacement, sampling analysis can be performed until the pressure reaches the specified pressure in the analyzer, and if the replacement is thorough, repeating the steps S1-S6 until the replacement is qualified; Then, the pure fluorine gas is analyzed, including the following steps S10-S80: Step S10, closing a first valve, a second valve, a third valve, a fourth valve, a fifth valve and an eighth valve, and opening the first pressure reducing valve, the second pressure reducing valve and the third pressure reducing valve;