Method for analyzing a fluorine-containing gas

Abstract

The scheme belongs to the technical field of gas analysis, and particularly relates to an analysis method of fluorine-containing gas. For pure fluorine gas analysis, the method comprises the following steps S10-S80: step S10: closing first valve, second valve, third valve, fourth valve, fifth valve and eighth valve, and opening first pressure reducing valve, second pressure reducing valve and third pressure reducing valve; step S20: slowly opening sixth valve and second valve in sequence, and closing sixth valve and second valve after 10 min of emptying; comprising the following steps K10-SK90: step K10: closing fifth valve, second valve, eighth valve, sixth valve, third valve, fourth valve and first valve, and opening first pressure reducing valve, second pressure reducing valve, third pressure reducing valve and seventh valve. The method is simple and convenient to operate, has high controllability and safety performance, air in the pipeline is sucked into the injection port of the Venturi tube, and then the air is discharged from the outlet of the Venturi tube, so that the air in the pipeline is efficiently and completely replaced, and the analysis result is more accurate and real.

Description

Technical Field

[0001] This solution belongs to the field of gas analysis technology, specifically involving an analytical method for fluorine-containing gases. Background Technology

[0002] Fluorine is the most electronegative and chemically reactive nonmetallic element, reacting with almost all elements. Fluorine gas (F2) is used in the semiconductor industry as an etching or cleaning gas in the manufacture of photovoltaic cells and TFTs (thin-film transistors) for liquid crystal displays due to its reactive properties. As a cleaning agent in CVD reaction chambers, F2 has stronger reactivity than NF3 and does not contribute to the greenhouse effect. The metallic fluorides formed by the reaction of fluorine gas with metals such as tungsten or germanium can be used as vapor deposition gases or doping gases in semiconductor manufacturing. High-purity fluorine gas can be mixed with inert gases such as nitrogen, helium, neon, and argon in any concentration to create a mixture for use as a laser gas. Therefore, fluorine gas has great application potential in the semiconductor field, but the industry's requirements for fluorine purity are increasingly stringent, gradually increasing from 99.7% (volume ratio) to over 99.99% (volume ratio). However, the analysis of various impurities in fluorine gas is challenging, especially the analysis of HF, for which the industry has yet to find a suitable analytical method.

[0003] Patent CN216747582U discloses a device for detecting the HF content in fluorine gas, including a constant volume sampling tube, a conversion column system and a vacuum pump connected in sequence by pipelines. A vacuum valve is connected in series between the conversion column system and the vacuum pump through pipelines. An absorption bottle system is connected in parallel to the two ends of the vacuum valve through pipelines. The absorption bottle system contains an absorption liquid. The conversion column system is filled with a fluorine gas conversion agent. The constant volume sampling tube is equipped with a fluorine gas sampling valve and an inert gas purging valve.

[0004] This method involves first collecting a specific volume of fluorine gas to be detected using a constant-volume sampling tube. Then, high-purity nitrogen or inert gases such as helium, argon, or radon are used to drive and displace the fluorine gas into a conversion column. The column is filled with a fluorine conversion agent, which converts the fluorine gas into a substance that does not interfere with HF detection. However, this method only converts the fluorine gas into a non-interfering substance; it does not replace the air in the pipeline. Air contains various gases that can affect the analytical results, leading to inaccurate or unreliable results. Summary of the Invention

[0005] This solution provides an analytical method for fluorine-containing gases that yields accurate and reliable results.

[0006] To achieve the above objectives, this solution provides an analytical method for fluorine-containing gases.

[0007] Includes steps S1-S7: replacing the pipeline,

[0008] Step S1: With all valves closed, adjust the first pressure reducing valve to 5-8 barg, open the first, fifth, and seventh valves, and lower the second pressure gauge to negative pressure. After 1-2 minutes, when the second pressure gauge pointer does not change, close the fifth and seventh valves.

[0009] Step S2: Adjust the third pressure reducing valve to 2-5 barg, and open the third, fourth and seventh valves in sequence. Adjust the second pressure reducing valve to 1-5 psig to allow high-purity nitrogen to enter the analyzer to the specified pressure.

[0010] Step S3: Close the third valve, open the fifth valve, and the second pressure gauge drops to negative pressure;

[0011] Step S4: Open the second valve. When the pointer of the second pressure gauge does not change after 1-2 minutes, close the fifth valve and the second valve.

[0012] Step S5: Open the third valve and adjust the second pressure gauge to the specified pressure.

[0013] Step S6: Repeat steps S3-S5 a total of 60 times to complete the replacement.

[0014] Step S7: After replacement, press the analyzer to the specified pressure and inject the sample to check if the replacement is complete. If not, repeat steps S1-S6 above to continue replacement until it is qualified.

[0015] Then, the pure fluorine gas is analyzed, including the following steps S10-S80:

[0016] Step S10: Close the first valve, the second valve, the third valve, the fourth valve, the fifth valve and the eighth valve, and open the first pressure reducing valve, the second pressure reducing valve and the third pressure reducing valve;

[0017] Step S20: Slowly open the sixth valve and the second valve in sequence, and vent for 10 minutes; then close the sixth valve and the second valve.

[0018] Step S30: Open the first valve, the fifth valve and the seventh valve in sequence, and the second pressure gauge drops to negative pressure;

[0019] Step S40: Open the second valve and the fourth valve. If the pointer of the second pressure gauge does not change for 1-2 minutes, close the fifth valve, the second valve, the fourth valve and the first valve in sequence.

[0020] Step S80: Slowly open the sixth valve and the fourth valve in sequence. When the second pressure gauge reaches the specified pressure, close the sixth valve.

[0021] Step S60: Open the first valve and the fifth valve in sequence. The second pressure gauge will drop to negative pressure. Open the second valve again. When the pointer of the second pressure gauge does not change for 1-2 minutes, close the fifth valve, the second valve, the fourth valve, and the first valve in sequence.

[0022] Step S70: Slowly open the sixth valve and the fourth valve in sequence. When the second pressure gauge reaches the specified pressure, close the fourth valve and the sixth valve. The analyzer then analyzes the pure fluorine gas.

[0023] Step S80: After the analysis is completed, open the first valve, the fifth valve, the second valve and the fourth valve in sequence. The second pressure gauge drops to negative pressure. When the pointer of the second pressure gauge does not change for 1-2 minutes, close the fifth valve, the second valve, the fourth valve and the first valve in sequence.

[0024] Analysis of fluorine-containing gas mixtures includes the following steps K10-SK90:

[0025] Step K10: Close valves 5, 2, 8, 6, 3, 4, and 1; open valves 1, 2, 3, and 7.

[0026] Step K20: Open the third valve and the eighth valve in sequence, close the third valve until the airflow weakens, open the third valve again, and repeat the opening and closing of the third valve at least 30 times.

[0027] Step K30: Adjust the eighth valve until the airflow decreases, connect the gas cylinder valve to the fluorine-containing mixed gas cylinder with the gas and tighten it; open the eighth valve and confirm that there is no leakage at the gas cylinder connection.

[0028] Step K40: Close the third valve, open the first and second valves until there is no airflow sound, and close the second, eighth, and first valves;

[0029] Step K50: Slowly open the valve of the fluorine-containing mixed gas cylinder and then close it. Open the eighth valve and the fourth valve in sequence. The third pressure gauge shows pressure. Ensure that there is no leakage at the cylinder valve connection.

[0030] Step K60: Slowly open the valve of the fluorine-containing mixed gas cylinder; press the second pressure gauge to the specified pressure, and close the fourth and eighth valves;

[0031] Step K70: Open the first valve, the fifth valve, the second valve, and the fourth valve in sequence. The second pressure gauge drops to negative pressure. When the pointer of the second pressure gauge does not change for 1-2 minutes, close the fifth valve, the second valve, and the first valve in sequence.

[0032] Step K80: Open the eighth valve, adjust the second pressure gauge II to the specified pressure, and close the fourth valve, the eighth valve, and the fluorine mixture cylinder valve; analyze the fluorine-containing gas mixture using the analyzer.

[0033] Step K90: Analysis complete. Open the first valve, the fifth valve, the second valve, the eighth valve, and the fourth valve in sequence. The second pressure gauge will drop to negative pressure. When the pointer of the second pressure gauge does not change for 1-2 minutes, close the fifth valve, the second valve, the eighth valve, the fourth valve, and the first valve in sequence.

[0034] The beneficial effects of this method are: It is simple and convenient to operate, highly controllable and safe. Air is drawn into the pipeline through the injection port of the Venturi tube and then discharged from the outlet of the Venturi tube, achieving efficient and thorough replacement of the air in the pipeline. This enables efficient, accurate, stable and safe analysis of the content of impurity components in fluorine-containing mixed gases in subsequent analysis work, which is of great significance in practical applications. In addition, it can also analyze the concentration in pure fluorine gas, and the analysis results are more accurate and true.

[0035] Furthermore, for the analysis of pure fluorine gas, step S100 is also included: if the analyzer is not used for a long time, the third valve, fourth valve, and fifth valve can be opened sequentially for flow purging. This flow purging removes dust from the analyzer.

[0036] Furthermore, when analyzing fluorine-containing mixed gases, step K100 is also included. If the analyzer is not used for a long time, the third valve, the fourth valve, and the fifth valve can be opened in sequence for flow purging.

[0037] Furthermore, it also includes an analytical apparatus for realizing the above method of fluorine-containing gas, including a first passage, a second passage, a third passage and a fourth passage;

[0038] The first passage is sequentially equipped with a standard nitrogen inlet pipe, a first pressure reducing valve, a first pressure gauge, a first valve, a check valve, and a venturi tube. The inlets of the standard nitrogen inlet pipe, the first pressure reducing valve, the first pressure gauge, the first standard valve, the check valve, and the venturi tube are all connected by pipes.

[0039] The second access path includes a fluorine gas inlet pipe, a sixth valve, a fourth valve, a second pressure reducing valve, a second pressure gauge, a seventh valve, and an analyzer, arranged sequentially. The fluorine gas inlet pipe, the sixth valve, the fourth valve, the second pressure reducing valve, the second pressure gauge, the seventh valve, and the analyzer are all connected by pipes. The fourth valve is also connected to a third pressure gauge via a pipe. The sixth valve and the injector of the venturi tube are connected by a second valve via a pipe. The exhaust end of the analyzer is connected to a fifth valve via a pipe. The fifth valve is connected to both the injector of the venturi tube and the second valve.

[0040] The third passage includes a third pressure-reducing valve, a fourth pressure gauge, and a third valve arranged sequentially. The third pressure-reducing valve, the fourth pressure gauge, and the third valve are all connected by pipes. The two ends of the third valve are connected to the second valve and the fourth valve by pipes, respectively.

[0041] The fourth passage includes a fluorine-containing mixed gas cylinder and an eighth valve. The fluorine-containing mixed gas cylinder and the eighth valve are connected by a pipeline, and the eighth valve is connected by a pipeline to the second valve and the sixth valve respectively.

[0042] Furthermore, it also includes an operation panel, in which the first pressure reducing valve, first pressure gauge, first valve, check valve, sixth valve, fourth valve, second pressure reducing valve, second pressure gauge, seventh valve, analyzer, third pressure reducing valve, fourth pressure gauge, third valve, and eighth valve are all communicatively or electrically connected. Operators can directly perform analysis work on the operation panel, which is simple, convenient, and highly efficient.

[0043] Furthermore, the first, second, and third pressure reducing valves are used to convert high-pressure gas into low-pressure gas. The pressure reducing valve consists of a valve body, a diaphragm, a valve seat, a valve stem, a valve cap, and a handle. The valve body is made of 316L stainless steel.

[0044] Furthermore, the first, second, third, and fourth pressure gauges use elastic elements as sensing elements to measure and indicate pressures higher than ambient pressure. Each of the first, second, third, and fourth pressure gauges consists of an overflow orifice, a pointer, and a glass panel.

[0045] Furthermore, the one-way valve consists of a valve body, a valve core, a spring, and a sealing ring, and the valve body is made of 316L stainless steel.

[0046] Furthermore, the material of the venturi tube is 316L.

[0047] The first step is that the valve bodies of the first to the eighth valves are all composed of a valve body, a diaphragm, a valve seat, a valve stem, a valve cap, and a handle, and the valve body material is 316L.

[0048] Furthermore, the pipe is a hollow, long, round steel bar made of 316L stainless steel. Attached Figure Description

[0049] Figure 1 This is a schematic diagram of the process of replacing the pipeline in Embodiment 1 of the present invention.

[0050] Figure 2 This is a schematic diagram of the process for analyzing pure fluorine gas according to Embodiment 1 of the present invention.

[0051] Figure 3 This is a schematic diagram of the process for analyzing a fluorine-containing mixed gas according to Embodiment 1 of the present invention.

[0052] Figure 4 This is a schematic diagram of the structure of Embodiment 1 of the present invention.

[0053] Figure 5 This is a schematic diagram of the structure of Embodiment 2 of the present invention.

[0054] Figure 6 This is a schematic diagram of the structure of the tube plug located inside the vent pipe in Embodiment 2 of the present invention.

[0055] Figure 7 This is a schematic diagram of the structure of the tube plug located in the limiting groove in Embodiment 2 of the present invention.

[0056] Figure 8 This is a schematic diagram of the left view of the air outlet of the plug in Embodiment 2 of the present invention. Detailed Implementation

[0057] The following detailed description illustrates the specific implementation method:

[0058] The markings in the accompanying drawings include: 101, First valve; 102, Second valve; 103, Third valve; 104, Fourth valve; 105, Fifth valve; 106, Sixth valve; 107, Seventh valve; 108, Eighth valve; 109, First pressure reducing valve; 110, Second pressure reducing valve; 111, Third pressure reducing valve; 112, First pressure gauge; 113, Second pressure gauge; 114, Third pressure gauge; 115, Fourth pressure gauge; 1, Bottle body; 2, Gas valve; 3, Bottle mouth; 4, Vent pipe; 5, Permanent magnet; 6, Base; 7, Electromagnet; 8, Coil; 9, Support plate; 10, Support rod; 11, Push rod; 12, Pipe plug; 13, Limiting groove; 14, Fan blade.

[0059] Example 1 is basically as shown in the appendix. Figure 4 As shown:

[0060] An analytical method for fluorine-containing gases is performed using an analytical apparatus, which includes a first passage, a second passage, a third passage, and a fourth passage.

[0061] The first passage is sequentially equipped with a common nitrogen inlet pipe, a first pressure reducing valve 109, a first pressure gauge 112, a first valve 101, a check valve, and a venturi tube. The inlets of the common nitrogen inlet pipe, the first pressure reducing valve 109, the first pressure gauge 112, the first common valve, the check valve, and the venturi tube are all connected by pipes.

[0062] The second passage includes a fluorine gas inlet pipe, 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, arranged sequentially. The fluorine gas inlet pipe, 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 all connected by pipes. The fourth valve 104 is also connected to a third pressure gauge 114 via a pipe. The sixth valve 106 and the injection port of the venturi tube are connected by a second valve 102 via a pipe. The exhaust end of the analyzer is connected to a fifth valve 105 via a pipe. The fifth valve 105 is connected to both the injection port of the venturi tube and the second valve 102.

[0063] The third passage includes a third pressure reducing valve 111, a fourth pressure gauge 115, and a third valve 103 arranged sequentially. The third pressure reducing valve 111, the fourth pressure gauge 115, and the third valve 103 are all connected by pipes. The two ends of the third valve 103 are respectively connected to the second valve 102 and the fourth valve 104 through pipes.

[0064] The fourth passage includes a fluorine-containing mixed gas cylinder and an eighth valve 108. The fluorine-containing mixed gas cylinder and the eighth valve 108 are connected by a pipeline. The eighth valve 108 is connected by a pipeline to the second valve 102 and the sixth valve 106, respectively.

[0065] It also includes an operation panel, and 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 communicatively or electrically connected to the operation panel. Operators can directly perform analysis work on the operation panel, which is simple, convenient, and highly efficient.

[0066] There may be air in the pipeline of the new analyzer. Before analysis, the air in the pipeline is replaced to make the analysis results of pure fluorine gas and fluorine-containing mixed gas more accurate.

[0067] As attached Figure 1 As shown: The following steps are used to replace the air in the pipeline.

[0068] Step S1: With all valves closed, adjust the first pressure reducing valve 109 to 5-8 barg, open the first valve 101, the fifth valve 105, and the seventh valve 107. The second pressure gauge 113 will drop to negative pressure. When the pointer of the second pressure gauge 113 does not change for 1-2 minutes, close the fifth valve 105 and the seventh valve 107.

[0069] Step S2: Adjust the third pressure reducing valve 111 to 2-5 barg, and open the third valve 103, the fourth valve 104 and the seventh valve 107 in sequence. Adjust the second pressure reducing valve 110 to 1-5 psig to allow high-purity nitrogen to enter the analyzer to the specified pressure.

[0070] Step S3: Close the third valve 103, open the fifth valve 105, and the second pressure gauge 113 drops to negative pressure;

[0071] Step S4: Open the second valve 102. When the pointer of the second pressure gauge 113 does not change after 1-2 minutes, close the fifth valve 105 and the second valve 102.

[0072] Step S5: Open valve 103 (third valve) and pressure gauge 113 (second pressure gauge) to the specified pressure.

[0073] Step S6: Repeat steps S3-S5 a total of 60 times to complete the replacement.

[0074] Step S7: After replacement, press the analyzer to the specified pressure and inject the sample to check if the replacement is complete. If not, repeat steps S1-S6 above to continue replacement until it is qualified.

[0075] Then, the pure fluorine gas is analyzed using an analytical apparatus, including the following steps S10-S80: as shown in the attached diagram. Figure 2 As shown:

[0076] Step S10: Close the first valve 101, the second valve 102, the third valve 103, the fourth valve 104, the fifth valve 105 and the eighth valve 108, and open the first pressure reducing valve 109, the second pressure reducing valve 110 and the third pressure reducing valve 111;

[0077] Step S20: Slowly open the sixth valve 106 and the second valve 102 in sequence, and vent for 10 minutes; then close the sixth valve 106 and the second valve 102.

[0078] Step S30: Open the first valve 101, the fifth valve 105 and the seventh valve 107 in sequence, and the second pressure gauge 113 drops to negative pressure;

[0079] Step S40: Open the second valve 102 and the fourth valve 104. When the pointer of the second pressure gauge 113 does not change for 1-2 minutes, close the fifth valve 105, the second valve 102, the fourth valve 104 and the first valve 101 in sequence.

[0080] Step S50: Slowly open the sixth valve 106 and the fourth valve 104 in sequence. When the second pressure gauge 113 reaches the specified pressure, close the sixth valve 106.

[0081] Step S60: Open the first valve 101 and the fifth valve 105 in sequence. The second pressure gauge 113 will decrease to negative pressure. Open the second valve 102. When the pointer of the second pressure gauge 113 does not change for 1-2 minutes, close the fifth valve 105, the second valve 102, the fourth valve 104, and the first valve 101 in sequence.

[0082] Step S70: Slowly open the sixth valve 106 and the fourth valve 104 sequentially. When the second pressure gauge 113 reaches the specified pressure, close the fourth valve 104 and the sixth valve 106. The analyzer then analyzes the pure fluorine gas.

[0083] Step S80: After the analysis is completed, open the first valve 101, the fifth valve 105, the second valve 102 and the fourth valve 104 in sequence. The second pressure gauge 113 drops to negative pressure. When the pointer of the second pressure gauge 113 does not change for 1-2 minutes, close the fifth valve 105, the second valve 102, the fourth valve 104 and the first valve 101 in sequence.

[0084] The analysis of the fluorine-containing gas mixture using an analytical apparatus includes the following steps K10-SK90: (see attached) Figure 3 As shown:

[0085] Step K10: Close the fifth valve 105, the second valve 102, the eighth valve 108, the sixth valve 106, the third valve 103, the fourth valve 104, and the first valve 101; open the first pressure reducing valve 109, the second pressure reducing valve 110, the third pressure reducing valve 111, and the seventh valve 107.

[0086] Step K20: Open the third valve 103 and the eighth valve 108 in sequence, close the third valve 103 until the airflow weakens, open the third valve 103 again, and repeat the opening and closing of the third valve 103 at least 30 times.

[0087] Step K30: Adjust the eighth valve 108 until the airflow decreases, connect the gas cylinder valve connector with the gas and tighten it; open the eighth valve 108 and confirm that there is no leakage at the gas cylinder connector;

[0088] Step K40: Close the third valve 103, open the first valve 101 and the second valve 102 until there is no airflow sound, and close the second valve 102, the eighth valve 108 and the first valve 101;

[0089] Step K50: Slowly open the valve of the fluorine-containing mixed gas cylinder and then close it. Open the eighth valve 108 and the fourth valve 104 in sequence. The third pressure gauge 114 has pressure. Ensure that there is no leakage at the cylinder valve connection.

[0090] Step K60: Slowly open the valve of the fluorine-containing mixed gas cylinder; press the second pressure gauge 113 to the specified pressure, and close the fourth valve 104 and the eighth valve 108;

[0091] Step K70: Open the first valve 101, the fifth valve 105, the second valve 102, and the fourth valve 104 in sequence. The second pressure gauge 113 drops to negative pressure. When the pointer of the second pressure gauge 113 does not change for 1-2 minutes, close the fifth valve 105, the second valve 102, and the first valve 101 in sequence.

[0092] Step K80: Open the eighth valve 108, adjust the second pressure gauge 113II to the specified pressure, and close the fourth valve 104, the eighth valve 108, and the fluorine mixed gas cylinder valve; analyze the fluorine-containing mixed gas using the analyzer.

[0093] Step K90: Analysis complete. Open valves 101, 105, 102, 108, and 104 in sequence. The pressure gauge 113 will drop to negative pressure. When the pointer of the pressure gauge 113 does not change for 1-2 minutes, close valves 105, 102, 108, 104, and 101 in sequence.

[0094] Example 2,

[0095] The difference between this embodiment and Embodiment 1 is as follows: (See attached...) Figure 5-8 As shown:

[0096] A fluorine-containing mixed gas cylinder includes a cylinder body 1, which is a hollow cylinder. A valve 2 is located at the top of the cylinder body 1, and a bottle opening 3 is also located at the top of the cylinder body 1. The valve 2 is used to close the bottle opening 3. The valve 2 is detachably connected to the cylinder body 1. A vent pipe 4 is installed inside the cylinder body 1, communicating with the bottle opening 3. The vent pipe 4 is a spring and is hollow. A permanent magnet 5 is mounted on the vent pipe 4. A base 6 is located at the bottom of the cylinder body 1, and an electromagnet 7 corresponding to the permanent magnet 5 is mounted on the base 6. The permanent magnet 5 and the electromagnet 7 repel each other due to their similar poles. A coil 8 is wound around the cylinder body 1, and an input wire and an output wire are connected to the coil 8. The wires form a closed loop, and the electromagnet 7 is located on the closed loop. The bottom end of the vent pipe 4 is provided with a sealing mechanism, which includes a support plate 9, a support rod 10, a suction cup, and a pipe plug 12. The pipe plug 12 is used to block the vent pipe 4. The support plate 9 is fixedly connected to the upper end of the vent pipe 4. The upper end of the support rod 10 is hinged to the support plate 9, and the lower end of the support rod 10 is fixedly connected to the pipe plug 12. The support plate 9 is provided with a sliding groove for the support rod 10 to rotate. The support plate 9 is provided with a limiting groove 13 that matches the support rod 10. The limiting groove 13 is used to prevent the support rod 10 from moving downward. The top of the bottle body 1 is provided with a push rod 11 for pushing the bottle stopper downward.

[0097] Because the different gases in the fluorinated gas mixture have significant density differences, the mixed gas that has just been filled from valve 2 into cylinder 1 needs at least one hour of shaking before the components can mix in a short time. If it is not shaken, it will take at least a week to mix naturally. This results in a waste of manpower, resources and time when filling the mixed gas cylinder with fluorinated gas, and the utilization efficiency of the mixed gas cylinder is low.

[0098] When it is necessary to fill the bottle 1 with a fluorine-containing mixed gas, the gas valve 2 is opened, and the fluorine-containing mixed gas is injected into the vent pipe 4 through the bottle mouth 3. The continuous gas injection causes the vent pipe 4 to stretch from its initial state. After the vent pipe 4 is stretched, the outlet of the vent pipe 4 is nearly perpendicular to the ground. The continuously injected fluorine-containing mixed gas pushes open the pipe plug 12, causing the airflow in the vent pipe 4 to rush out. The vent pipe 4 then moves upward due to the reaction force of the airflow. Because the vent pipe 4 is a spring, it moves up and down repeatedly due to the reaction force of the airflow, which in turn drives the permanent magnet 5 to move up and down. The permanent magnet 5 cuts the magnetic field lines, generating an electric current. The electromagnet 7 then becomes charged and repels the permanent magnet 5, causing the permanent magnet 5 to move upward due to the repulsive force. Meanwhile, the continuous input of gas from the outside causes the bottom of the vent pipe 4 to move downward, and the vent pipe 4 continues to move up and down repeatedly. The vent pipe 4 stirs the gas injected into the bottle 1, making the mixed gas more uniform and the mixing effect better.

[0099] In addition, a fan blade 14 is provided on the side of the vent pipe 4 away from the bottle stopper. During the up and down movement of the vent pipe 4, the fan blade 14 plays a stirring and mixing role on the gas in the bottle, which improves the gas mixing efficiency of the fluorine-containing mixed gas bottle.

[0100] When the gas in the vent tube 4 pushes open the bottle stopper, the bottle stopper rotates clockwise and then is located in the limiting groove 13 with the support rod 10, so as to prevent the bottle stopper from rotating back and blocking the air outlet of the vent tube 4.

[0101] Then, when it is necessary to remove the gas from the fluorine-containing mixed gas cylinder for use, open the gas valve 2 and discharge the mixed gas from the cylinder through the vent pipe 4. As the gas in the cylinder slowly disappears, the vent pipe 4 contracts and moves upward. Then, the support rod at the top of the cylinder body 1 pushes the tube plug 12 out of the limiting groove 13. Then, the tube plug 12 moves downward due to its own weight and is subjected to the force given by the support rod. Then, the tube plug 12 moves counterclockwise into the vent pipe 4, thereby blocking the gas outlet of the vent pipe 4 for the next use.

[0102] The above descriptions are merely embodiments of the present invention, and common knowledge regarding specific structures and characteristics is not elaborated upon here. It should be noted that those skilled in the art can make various modifications and improvements without departing from the structure of the present invention, and these should also be considered within the scope of protection of the present invention. These modifications and improvements will not affect the effectiveness of the present invention or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.

Claims

1. A method for analyzing fluorine-containing gases, characterized in that: Includes steps S1-S7: replacing the pipeline, Step S1: With all valves closed, adjust the first pressure reducing valve (109) to 5-8 barg, open the first valve (101), the fifth valve (105) and the seventh valve (107), and the second pressure gauge (113) drops to negative pressure. When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105) and the seventh valve (107). Step S2: Adjust the third pressure reducing valve (111) to 2-5 barg, and open the third valve (103), the fourth valve (104) and the seventh valve (107) in sequence. Adjust the second pressure reducing valve (110) to 1-5 psig to allow high-purity nitrogen to enter the analyzer to the specified pressure. Step S3: Close the third valve (103), open the fifth valve (105), and the second pressure gauge (113) drops to negative pressure; Step S4: Open the second valve (102). When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105) and the second valve (102). Step S5: Open valve 3 (103) and pressure gauge 2 (113) to the specified pressure; Step S6: Repeat steps S3-S5 a total of 60 times to complete the replacement; Step S7: After replacement, press the analyzer to the specified pressure and inject the sample to check if the replacement is complete. If not, repeat steps S1-S6 above to continue replacement until it is qualified. Includes the following steps S10-S80: Analysis of pure fluorine gas, Step S10: Close the first valve (101), the second valve (102), the third valve (103), the fourth valve (104), the fifth valve (105) and the eighth valve (108), and open the first pressure reducing valve (109), the second pressure reducing valve (110) and the third pressure reducing valve (111). Step S20: Slowly open the sixth valve (106) and the second valve (102) in sequence, and vent for 10 minutes; then close the sixth valve (106) and the second valve (102). Step S30: Open the first valve (101), the fifth valve (105) and the seventh valve (107) in sequence, and the second pressure gauge (113) drops to negative pressure; Step S40: Open the second valve (102) and the fourth valve (104). When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105), the second valve (102), the fourth valve (104) and the first valve (101) in sequence. Step S50: Slowly open the sixth valve (106) and the fourth valve (104) in sequence. When the second pressure gauge (113) reaches the specified pressure, close the sixth valve (106). Step S60: Open the first valve (101) and the fifth valve (105) in sequence. The second pressure gauge (113) drops to negative pressure. Open the second valve (102). When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105), the second valve (102), the fourth valve (104), and the first valve (101) in sequence. Step S70: Slowly open the sixth valve (106) and the fourth valve (104) in sequence. When the second pressure gauge (113) reaches the specified pressure, close the fourth valve (104) and the sixth valve (106). The analyzer then analyzes the pure fluorine gas. Step S80: After the analysis is completed, open the first valve (101), the fifth valve (105), the second valve (102) and the fourth valve (104) in sequence. The second pressure gauge (113) drops to negative pressure. When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105), the second valve (102), the fourth valve (104) and the first valve (101) in sequence. The following steps are included in K10-SK90: Analysis of fluorine-containing gas mixtures. Step K10: Close the fifth valve (105), the second valve (102), the eighth valve (108), the sixth valve (106), the third valve (103), the fourth valve (104), and the first valve (101), and open the first pressure reducing valve (109), the second pressure reducing valve (110), the third pressure reducing valve (111), and the seventh valve (107). Step K20: Open the third valve (103) and the eighth valve (108) in sequence, close the third valve (103) until the airflow weakens, open the third valve (103), and continuously close and open the third valve (103) at least 30 times. Step K30: Adjust the eighth valve (108) until the airflow decreases, connect the fluorine-containing mixed gas cylinder valve connector with the gas and tighten it; open the eighth valve (108) and confirm that there is no leakage at the gas cylinder connector; Step K40: Close the third valve (103), open the first valve (101) and the second valve (102) until there is no airflow sound, and close the second valve (102), the eighth valve (108) and the first valve (101). Step K50: Slowly open the valve of the fluorine-containing mixed gas cylinder and then close it. Open the eighth valve (108) and the fourth valve (104) in sequence. The third pressure gauge (114) shows pressure. Ensure that there is no leakage at the cylinder valve connection. Step K60: Slowly open the valve of the fluorine-containing mixed gas cylinder; check the second pressure gauge (113) to the specified pressure, and close the fourth valve (104) and the eighth valve (108). Step K70: Open the first valve (101), the fifth valve (105), the second valve (102), and the fourth valve (104) in sequence. The second pressure gauge (113) drops to negative pressure. When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105), the second valve (102), and the first valve (101) in sequence. Step K80: Open the eighth valve (108), adjust the second pressure gauge (113) II to the specified pressure, and close the fourth valve (104), the eighth valve (108), and the fluorine mixture cylinder valve; the analyzer analyzes the fluorine-containing mixture. Step K90: After the analysis is completed, open the first valve (101), the fifth valve (105), the second valve (102), the eighth valve (108), and the fourth valve (104) in sequence. The second pressure gauge (113) drops to negative pressure. When the pointer of the second pressure gauge (113) does not change for 1-2 minutes, close the fifth valve (105), the second valve (102), the eighth valve (108), the fourth valve (104), and the first valve (101) in sequence. It also includes an analytical apparatus for implementing the above method for fluorine-containing gases, comprising a first passage, a second passage, a third passage, and a fourth passage; The first passage is sequentially equipped with a common nitrogen inlet pipe, a first pressure reducing valve (109), a first pressure gauge (112), a first valve (101), a check valve, and a venturi tube. The inlets of the common nitrogen inlet pipe, the first pressure reducing valve (109), the first pressure gauge (112), the first common valve, the check valve, and the venturi tube are all connected by pipes. The second passage includes a fluorine gas inlet pipe, 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, arranged sequentially. The fluorine gas inlet pipe, 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 all connected by pipes. The fourth valve (104) is also connected to a third pressure gauge (114) via a pipe. The sixth valve (106) and the injection port of the venturi tube are connected by a second valve (102) via a pipe. The exhaust end of the analyzer is connected to a fifth valve (105) via a pipe. The fifth valve (105) is connected to both the injection port of the venturi tube and the second valve (102). The third passage includes a third pressure reducing valve (111), a fourth pressure gauge (115), and a third valve (103) arranged sequentially. The third pressure reducing valve (111), the fourth pressure gauge (115), and the third valve (103) are all connected by pipes. The two ends of the third valve (103) are connected to the second valve (102) and the fourth valve (104) by pipes, respectively. The fourth passage includes a fluorine-containing mixed gas cylinder (1) and an eighth valve (108). The fluorine-containing mixed gas cylinder (1) and the eighth valve (108) are connected by a pipeline. The eighth valve (108) is connected by a pipeline to the second valve (102) and the sixth valve (106) respectively. The fluorine-containing mixed gas cylinder (1) is a hollow cylinder. A gas valve (2) is provided at the top of the cylinder (1). A bottle mouth (3) is provided at the top of the cylinder (1). The gas valve (2) is used to close the bottle mouth (3). The gas valve (2) is detachably connected to the cylinder (1). A vent pipe (4) is provided inside the cylinder (1). The vent pipe (4) is connected to the bottle mouth (3). The vent pipe (4) is a spring. The vent pipe (4) is hollow. A permanent magnet (5) is provided on the vent pipe (4). A base (6) is provided at the bottom of the cylinder (1). An electromagnet (7) corresponding to the permanent magnet (5) is provided on the base (6). The permanent magnet (5) and the electromagnet (7) are like poles and repel each other. A coil (8) is wound around the cylinder (1). An input wire and an output wire are connected to the coil (8). The output wire and the input wire are connected to the coil (8). The wires form a closed loop, the electromagnet (7) is located on the closed loop, the bottom end of the vent pipe (4) is provided with a sealing mechanism, the sealing mechanism includes a support plate (9), a support rod (10), a suction cup and a tube plug (12), the tube plug (12) is used to block the vent pipe (4), the support plate (9) is fixedly connected to the upper end of the vent pipe (4), the upper end of the support rod (10) is hinged to the support plate (9), the lower end of the support rod (10) is fixedly connected to the tube plug (12), the support plate (9) is provided with a sliding groove for the support rod (10) to rotate, the support plate (9) is provided with a limiting groove (13) that matches the support rod (10), the limiting groove (13) is used to prevent the support rod (10) from moving downward, and the top of the bottle body (1) is provided with a push rod (11) for pushing the bottle stopper downward.

2. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: When analyzing pure fluorine gas, step S100 is also included. If the analyzer is not used for a long time, the third valve (103), the fourth valve (104), and the fifth valve (105) can be opened in sequence to purge the flow.

3. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: When analyzing fluorine-containing mixed gases, step K100 is also included. If the analyzer is not used for a long time, the third valve (103), the fourth valve (104), and the fifth valve (105) can be opened in sequence for flow purging.

4. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: It also includes an operation panel, and 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 connected to the operation panel for communication or electrical connection.

5. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: The first pressure reducing valve (109), the second pressure reducing valve (110) and the third pressure reducing valve (111) are used to convert high pressure gas into low pressure. The pressure reducing valve is composed of a valve body, a diaphragm, a valve seat, a valve stem, a valve cap and a handle. The valve body is made of 316L.

6. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: The first pressure gauge (112), the second pressure gauge (113), the third pressure gauge (114) and the fourth pressure gauge (115) use elastic elements as sensitive elements to measure and indicate pressures higher than the ambient pressure. The first pressure gauge (112), the second pressure gauge (113), the third pressure gauge (114) and the fourth pressure gauge (115) are all composed of an overflow hole, a pointer and a glass panel.

7. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: The one-way valve consists of a valve body, a valve core, a spring, and a sealing ring. The valve body is made of 316L stainless steel.

8. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: The venturi tube is made of 316L stainless steel.

9. The method for analyzing fluorine-containing gases according to claim 1, characterized in that: The valve bodies of the first valve (101) to the eighth valve (108) are all composed of a valve body, a diaphragm, a valve seat, a valve stem, a valve cap, and a handle. The valve body material is 316L.

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