Electronic-grade mixed gas distribution device and operation method thereof

Abstract

The invention provides an electronic-grade mixed gas distribution device and an operation method thereof. The method sequentially comprises the steps of pipeline replacement, quantitative filling of component gas, quantitative filling of balance gas, mixed gas detection and raw material recovery. According to the invention, the mixing efficiency of the mixed gas and the safety coefficient in the mixing process can be effectively improved; according to the invention, the quality of the electronic-grade mixed gas can be improved. The recovery gas cylinder in the gas distribution device can serve as a buffer device, safe recovery of gas can be guaranteed after liquid nitrogen is cooled, recovery of flammable and explosive gas is particularly facilitated, and production cost is saved.

Description

Technical Field

[0001] The invention relates to the field of gas preparation, and in particular to an electronic-grade mixed gas preparation device and an operation method thereof. Background Art

[0002] Electronic-grade mixed gas is a mixture of several gases prepared in a certain proportion to meet the needs of specific processes or applications. It is mainly used in high-precision fields such as semiconductor manufacturing, optoelectronic device production, and scientific research. Electronic-grade mixed gas has extremely high requirements for gas purity. Any trace impurities may have a serious impact on the performance of the product. For example, in semiconductor manufacturing, even trace amounts of dust or metal ions can cause the chip to short-circuit or fail. When existing devices use electronic-grade gas distribution, the error is above 0.1%. The proportion of each component in the electronic-grade mixed gas must be precisely controlled, and a slight deviation in the proportion will cause product performance to deteriorate or fail. Especially for electronic-grade gas distribution in the chip field, when the error is greater than 0.1%, it will directly lead to the scrapping of subsequent gas distribution products.

[0003] Patent CN 213253833 U cannot accurately control the proportion of each component. Patent CN 206064194 U uses a gas distribution cabinet, component gas cylinders and mixed gas cylinders to perform gas preparation procedures, and uses the pressure value of the reference gas cylinder to measure the mass of the trace components to complete the configuration of the mixed gas. However, relying solely on pressure value measurement cannot accurately control the proportion of each component.

[0004] Patent CN 108745010 A proposes a highly toxic electronic mixed gas configuration process, which includes component pre-configuration calculation, pipeline replacement before configuration, highly toxic component gas quantitative control, and balance gas one-way quantitative control. However, this method has high requirements on the pressure threshold of the raw gas cylinder. High-value raw materials in the raw gas cylinder that are below the pressure threshold cannot be filled into the mixed gas cylinder. At the same time, there may be a safety risk that the mixed gas may flow back into the raw gas cylinder.

[0005] When the gas distribution device in the prior art CN108176324A adopts a two-stage vacuum pump, the pumping time is relatively long. Due to the lack of an anti-backflow valve, the nitrogen in the phosphine and hydrogen mixture exceeds the standard, resulting in poisoning of the phosphine and hydrogen mixture; there is only one replacement and vacuum point and vacuum gauge, and the intersection points of the pipeline and each branch pipe are all concentrated on the terminal pipeline of the phosphine delivery pipe. There is no protective adjustment buffer device. In the event of unqualified product filling, pipeline leakage, and pipeline blockage, the replacement and purging of the system will be affected; not only does it reduce the life of the vacuum gauge and the finishing control valve, but the gas distribution device also has the problem that when the gas cylinder is insufficiently supplied with gas, the flammable and explosive gas cannot be recovered; when an abnormality occurs in the gas distribution system, a purifier needs to be installed separately to clean the entire gas distribution device, resulting in a long cleaning cycle, waste of raw gas, and low production efficiency of the production line.

[0006] Therefore, in view of the problems of insufficient purity, inaccurate proportion, waste of raw materials and filling safety in the traditional mixed gas configuration method, an electronic grade mixed gas distribution device and its operation method are proposed. Summary of the invention

[0007] The purpose of the present invention is to provide an electronic-grade mixed gas distribution device and an operating method thereof, so as to solve the problems of insufficient purity, inaccurate proportions, inability to recover raw materials resulting in waste of raw gas and filling safety existing in the mixed gas configuration method of the prior art.

[0008] In order to solve the above problems, the present application is implemented through the following technical solutions: An electronic grade mixed gas distribution device comprises a nitrogen container, wherein an outlet pipe of the nitrogen container is connected to an inlet pipe of a displacement pipeline through a nitrogen valve; and the inlet pipe of the displacement pipeline is also connected to an outlet pipe of a helium container through a helium valve. The branch pipe 1 of the displacement pipeline is connected to the inlet of the balancing gas pipeline through the first displacement valve; The branch pipe 2 of the replacement pipe is connected to the inlet of the component gas pipeline through the second replacement valve; The branch pipe 3 of the displacement pipe is connected to the middle part of the gas distribution main pipe through the third displacement valve; The outlet valve inlet of the main gas distribution pipeline is connected in parallel with the outlets of the balance gas pipeline and the component gas pipeline; The main gas distribution pipeline is also connected to the vacuum main pipeline through a No. 1 vacuum valve and a No. 2 vacuum valve connected in parallel.

[0009] The inlet of the balancing gas pipeline is also connected in series with a second one-way valve and a balancing gas valve, and the balancing gas valve is connected to the gas outlet pipe of the balancing gas container.

[0010] The inlet of the component gas pipeline is also connected in series with the first one-way valve and the component gas valve in sequence, and the component gas valve is connected to the gas outlet pipe of the component gas container.

[0011] The gas distribution main pipeline is connected to the reference gas cylinder through a pipeline and a first reference valve, and the gas distribution main pipeline is connected to the recovery gas cylinder through a pipeline and a recovery gas valve. Both the reference gas cylinder and the recovery gas cylinder are located on the outlet side of the gas outlet valve, the reference gas cylinder is installed on a precision electronic scale, and the recovery gas cylinder is installed inside a liquid nitrogen cylinder. The outlet of the gas distribution main pipeline is connected to the mixed gas container through the first mixed gas valve, and the air inlet pipe of the mixed gas container is also connected to the air inlet of the pressure reducing valve of the detection main pipeline through the first detection valve, and the air outlet of the pressure reducing valve is connected in parallel to the sampling ports of the chromatograph and the moisture meter.

[0012] The branch pipe of the vacuum main pipeline is connected to the component gas pipeline through the No. 3 vacuum valve; the branch pipe of the vacuum main pipeline is also connected to the balance gas pipeline through the No. 4 vacuum valve; the vacuum main pipeline is also connected to the vacuum pump through the third one-way valve, the exhaust pipe of the vacuum pump is connected to the exhaust buffer tank, and the buffer tank inlet pipe is also connected to the exhaust port of the exhaust main pipeline through the fourth one-way valve, and the branch pipe of the exhaust main pipeline is connected to the gas distribution main pipeline through the first exhaust valve and the second exhaust valve in parallel.

[0013] Branch pipe four of the replacement pipeline is connected to the rear side of the thermocouple vacuum gauge at the tail end of the gas distribution main pipeline through the fourth replacement valve; on the front side of the thermocouple vacuum gauge, the gas distribution main pipeline is also connected in parallel with a high-pressure valve, a medium-pressure valve and a low-pressure valve; the high-pressure valve is connected to the high-pressure gauge, the medium-pressure valve is connected to the medium-pressure gauge, and the low-pressure valve is connected to the low-pressure gauge.

[0014] The outlet of the gas distribution main pipeline is connected to the spare mixed gas container through the second mixed gas valve; the air inlet pipe of the spare mixed gas container is also connected to the air inlet of the pressure reducing valve of the detection main pipeline through the second detection valve.

[0015] The outlet pipe of the buffer tank is connected to the inlet of the tail gas absorption tower, and the tail gas absorption tower is equipped with a liquid replenishment pipe and a waste liquid pipe; a circulation pump is installed at the bottom of the tail gas absorption tower, and the output end of the circulation pump is connected to the top of the tail gas absorption tower through a circulation valve, and a vent valve is also installed on the top of the tail gas absorption tower.

[0016] The connection between the second tail gas valve and the gas distribution main pipeline is located at the rear side of the connection between the reference gas cylinder and the recovery gas cylinder and the gas distribution main pipeline, and is located at the front side of the connection between the high pressure gauge and the gas distribution main pipeline.

[0017] Further preferably, the first tail gas valve is located at the rear side of the high-pressure gauge, medium-pressure gauge, low-pressure gauge and thermocouple vacuum gauge to prevent the airflow from impacting the interface between the pressure gauge and the gas distribution main pipeline, affecting the accuracy and life of the high-pressure gauge, medium-pressure gauge and low-pressure gauge.

[0018] The operation method of the electronic grade mixed gas distribution device comprises the following steps: S1. Use inert gas to purge the replacement pipeline 1901, the balance gas pipeline 1902, the component gas pipeline 1903, the gas distribution main pipeline 1904 and the exhaust gas main pipeline 1905, and then evacuate; S2, quantitatively fill the reference gas cylinder 6 with a mass of m1 balance gas, and repeat step S1; S3, quantitatively filling the reference gas cylinder 6 with component gases having a mass of m2 to obtain a mixed gas, and repeating step S1; S4, checking whether the mixed gas in step S3 is qualified; S4.1, when the detected mixed gas is qualified, the mixed gas cylinder 12 and the reference gas cylinder 6 are qualified; repeat steps S2 to S4; S4.2. When the mixed gas is detected to be unqualified, the mixed gas cylinder 12 and the reference gas cylinder 6 are first deflated and then vacuumized; and steps S1 to S4 are repeated.

[0019] Compared with the prior art, the present invention has the following beneficial effects: 1. The electronic-grade mixed gas distribution method of the present invention effectively improves the mixing efficiency of the mixed gas and the safety factor in the mixing process through pipeline replacement, quantitative filling of component gases, quantitative filling of balance gas, mixed gas detection and raw material recovery steps, which helps to improve the quality of the electronic-grade mixed gas.

[0020] 2. Check valves are installed behind the outlet valves of the component gas cylinder 4 and the balance gas cylinder 3 to prevent the mixed gas from flowing back and causing danger.

[0021] 3. A high-precision pneumatic regulating valve is installed on the gas distribution main pipeline 1904. The valve opening is interlocked with the weight of the precision electronic scale 7. After the reference gas cylinder 6 is full, a new reference gas cylinder can be replaced. The present invention can reduce the error of each electronic grade gas distribution to below 0.07%, thereby improving the accuracy of the filling quality.

[0022] 4. Tail gas pipelines, vacuum pipelines, and helium and nitrogen replacement pipelines are provided on the balance gas pipeline 1902, component gas pipeline 1903, mixed gas cylinder 12, spare mixed gas container 13, reference gas cylinder 6, and recovery gas cylinder 8 charging pipelines. The recovery gas cylinder 8 can act as a buffer device and can also ensure the safe recovery of gas after liquid nitrogen cooling, which is particularly beneficial for the recovery of flammable and explosive gases and is very beneficial for saving production costs.

[0023] 5. Check valves are installed behind the outlet valves of the vacuum main pipeline 1906 and the exhaust main pipeline 1905 to prevent air from flowing back into the system and affecting the quality of the mixed gas product and causing explosion hazard.

[0024] 6. The air intake pipes of the mixed gas container 12 and the spare mixed gas container 13 are connected to the analytical instrument to analyze the quality of the product after filling, realize seamless connection between filling and testing, save time and improve efficiency. The pressure reducing valve 16, the first test valve 1202 and the second test valve 1204 are installed on the analysis and testing connecting pipes. The first test valve 1202 and the second test valve 1204 are one-way valves.

[0025] 7. The mixed gas cylinders are divided into two groups, a mixed gas container 12 and a spare mixed gas container 13, which share a filling system. When one group is filled, tested and disassembled, the other group of spare mixed gas containers can be filled to save time and improve filling efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 The present invention is a schematic diagram of the structure of an electronic-grade mixed gas distribution device.

[0027] Reference numerals: nitrogen container 1; nitrogen valve 101; helium container 2; helium valve 201; first replacement valve 202; second replacement valve 203; third replacement valve 204; fourth replacement valve 205; balance gas container 3; balance gas valve 301; component gas container 4; component gas valve 401; first non-return valve 5; second non-return valve 501; reference gas cylinder 6; first reference valve 601; main pipeline outlet valve 602; precision electronic scale 7; recovery gas cylinder 8; recovery gas valve 801; liquid nitrogen cylinder 9; high-pressure valve 10; high-pressure gauge 1001; medium-pressure gauge 1002; low-pressure gauge 1003; thermocouple vacuum gauge 11; mixed gas container 12; first mixed gas valve 1201; first detection valve 1202; second mixed gas valve 1203; The second detection valve 1204; the spare mixed gas container 13; the vacuum pump 14; the third non-return valve 1301; the first vacuum valve 1302; the second vacuum valve 1303; the third vacuum valve 1304; the fourth vacuum valve 1305; the tail gas buffer tank 15; the fourth non-return valve 1401; the first tail gas valve 1402; the second tail gas valve 1403; the pressure reducing valve 16; the chromatograph 17; the moisture meter 18; the circulation valve 1801; the circulation pump 19; the replacement pipeline 1901; the balance gas pipeline 1902: the component gas pipeline 1903: the gas distribution main pipeline 1904; the tail gas main pipeline 1905; the vacuum main pipeline 1906; the liquid replenishment pipe 1907; the waste liquid pipe 1908; the detection main pipeline 1909, the tail gas absorption tower 20; the vent valve 2001. DETAILED DESCRIPTION

[0028] The directions or positional relationships indicated by the terms "interior, tail, middle, one side, rear side, front side" and the like in the present invention are based on the directions or positional relationships shown in the drawings, and are only for the convenience of description, and do not indicate or imply that the devices or elements referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as limiting the present invention. The present invention is further described in detail below in conjunction with the drawings and specific embodiments. For the convenience of the attached drawings, Figure 1 The description of the replacement pipeline 1901, the balance gas pipeline 1902, the component gas pipeline 1903, the gas distribution main pipeline 1904, the tail gas main pipeline 1905, and the detection main pipeline 1909 are bold black lines. Multiple reference gas cylinders 6 and recovery gas cylinders 8 can also be connected in parallel. The instrument selection and gas selection of the present invention are for the convenience of explanation and do not limit the application to use this type of instrument. The device can also be used for other flammable and explosive gases.

[0029] The precision electronic scale 7, the vacuum pump 14, the chromatograph 17, the moisture meter 18 and the circulation pump 19 are powered by an external power supply, and the liquid nitrogen cylinder 9 is filled with liquid nitrogen.

[0030] The first reference valve 601 and the recovery gas valve 801 were purchased from Rotarex Valve (Shanghai) Co., Ltd., model M4SIVHM2V1KMM; the precision electronic scale 7 was purchased from Sartorius, model GL8201i-1SCN electronic balance; the chromatograph 17 was a helium ion chromatograph, model GC-9560-PDD purchased from Shanghai Huaai Chromatography Analysis Technology Co., Ltd.; The moisture meter 18 was purchased from Inner Mongolia Light Energy Technology Co., Ltd. High-sensitivity trace water analyzer (model: Pure n-BH2O in PH3, applicable to gases N2, He, Ar, PH3); The gas in the nitrogen container 1 is nitrogen; the gas in the helium container 2 is helium; the gas in the balance gas container 3 is hydrogen. The component gas in the component gas container 4 is phosphine (PH3). The absorbent in the tail gas absorption tower 20 is sodium hydroxide.

[0031] Attached Figure 1 The oval dotted line A on one side of the pipeline of the second valve 203 represents that it crosses other pipelines but is not connected; Attached Figure 1 The oval dotted line B on one side of the pipeline of the second buffer valve 1403 represents that it crosses other pipelines but is not connected; The liquid replenishing pipe 1907 replenishes the absorbent; the waste liquid pipe 1908 discharges the waste liquid; and the vent valve 2001 is used to discharge the tail gas after absorption.

[0032] The balancing gas cylinders in the balancing gas container 3, the component gas cylinders in the component gas container 4 and the mixed gas cylinders in the mixed gas container 12 can be connected in parallel in multiples, at least two, to achieve the purpose of one for backup and one for use.

[0033] Example 1 like Figure 1 As shown, a method for distributing electronic grade mixed gas is provided, and the specific implementation steps are as follows: Determine the ratio of the balance gas and the component gas in the mixed gas, and calculate the masses m1 and m2 of the balance gas and the component gas.

[0034] An electronic grade mixed gas distribution device comprises a nitrogen container 1, wherein the outlet pipe of the nitrogen container 1 is connected to the inlet pipe of a displacement pipeline 1901 through a nitrogen valve 101; the inlet pipe of the displacement pipeline 1901 is also connected to the outlet pipe of a helium container 2 through a helium valve 201. The branch pipe 1 of the replacement pipe 1901 is connected to the inlet of the balance gas pipe 1902 through the first replacement valve 202; The branch pipe 2 of the replacement pipe 1901 is connected to the inlet of the component gas pipe 1903 through the second replacement valve 203; The branch pipe 3 of the displacement pipe 1901 is connected to the middle part of the gas distribution main pipe 1904 through the third displacement valve 204; The inlet of the gas outlet valve 602 of the gas distribution main pipeline 1904 is connected in parallel to the outlets of the balance gas pipeline 1902 and the component gas pipeline 1903; The gas distribution main pipeline 1904 is also connected to the vacuum main pipeline 1906 through the parallel vacuum valve No. 1 1302 and the vacuum valve No. 2 1303.

[0035] The inlet of the balancing gas pipeline 1902 is also connected in series with the second one-way valve 501 and the balancing gas valve 301, and the balancing gas valve 301 is connected to the gas outlet pipe of the balancing gas container 3.

[0036] The inlet of the component gas pipeline 1903 is also connected in series with the first one-way valve 5 and the component gas valve 401 in sequence, and the component gas valve 401 is connected to the gas outlet pipe of the component gas collection grid 4.

[0037] The gas distribution main pipeline 1904 is connected to the reference gas cylinder 6 through a pipeline and the first reference valve 601. The gas distribution main pipeline 1904 is connected to the recovery gas cylinder 8 through a pipeline and the recovery gas valve 801. The reference gas cylinder 6 and the recovery gas cylinder 8 are both located on the outlet side of the gas outlet valve 602. The reference gas cylinder 6 is installed on the precision electronic scale 7, and the recovery gas cylinder 8 is installed inside the liquid nitrogen cylinder 9. The outlet of the gas distribution main pipeline 1904 is connected to the mixed gas container 12 through the first mixed gas valve 1201. The air inlet pipe of the mixed gas container 12 is also connected to the air inlet of the pressure reducing valve 16 of the detection main pipeline 1909 through the first detection valve 1202. The air outlet of the pressure reducing valve 16 is connected in parallel to the sampling ports of the chromatograph 17 and the moisture meter 18.

[0038] The branch pipe of the vacuum main pipeline 1906 is connected to the component gas pipeline 1903 through the No. 3 vacuum valve 1304; the branch pipe of the vacuum main pipeline 1906 is also connected to the balance gas pipeline 1902 through the No. 4 vacuum valve 1305; the vacuum main pipeline 1906 is also connected to the vacuum pump 14 through the third one-way valve 1301, the exhaust pipe of the vacuum pump 14 is connected to the exhaust gas buffer tank 15, and the inlet pipe of the buffer tank 15 is also connected to the exhaust port of the exhaust main pipeline 1905 through the fourth one-way valve 1401, and the branch pipe of the exhaust main pipeline 1905 is connected to the gas distribution main pipeline 1904 through the first exhaust valve 1402 and the second exhaust valve 1403 connected in parallel.

[0039] Branch pipe four of the replacement pipe 1901 is connected to the rear side of the thermocouple vacuum gauge 11 at the tail end of the gas distribution main pipe 1904 through the fourth replacement valve 205; on the front side of the thermocouple vacuum gauge 11, the gas distribution main pipe 1904 is also connected in parallel with a high-pressure valve 10, a medium-pressure valve and a low-pressure valve; the high-pressure valve 10 is connected to the high-pressure gauge 1001, the medium-pressure valve is connected to the medium-pressure gauge 1002, and the low-pressure valve is connected to the low-pressure gauge 1003.

[0040] The outlet of the gas distribution main pipeline 1904 is connected to the spare mixed gas container 13 through the second mixed gas valve 1203; the air inlet pipe of the spare mixed gas container 13 is also connected to the air inlet of the pressure reducing valve 16 of the detection main pipeline 1909 through the second detection valve 1204.

[0041] The outlet pipe of the buffer tank 15 is connected to the inlet of the tail gas absorption tower 20, and the tail gas absorption tower 20 is equipped with a liquid replenishment pipe 1907 and a waste liquid pipe 1908; a circulation pump 19 is installed at the bottom of the tail gas absorption tower 20, and the output end of the circulation pump 19 is connected to the top of the tail gas absorption tower 20 through a circulation valve 1801, and a vent valve 2001 is also installed at the top of the tail gas absorption tower 20.

[0042] The connection between the second tail gas valve 1403 and the gas distribution main pipeline 1904 is located at the rear side of the connection between the reference gas cylinder 6 and the recovery gas cylinder 8 and the gas distribution main pipeline 1904, and is located at the front side of the connection between the high pressure gauge 1001 and the gas distribution main pipeline 1904.

[0043] Further preferably, the first tail gas valve 1402 is located at the rear side of the high-pressure gauge 1001, the medium-pressure gauge 1002, the low-pressure gauge 1003 and the thermocouple vacuum gauge 11 to prevent the airflow from impacting the interface between the pressure gauge and the gas distribution main pipeline 1904, affecting the accuracy and life of the high-pressure gauge 1001, the medium-pressure gauge 1002 and the low-pressure gauge 1003.

[0044] The operation method of the electronic grade mixed gas distribution device comprises the following steps: S1. Use inert gas to purge the replacement pipeline 1901, the balance gas pipeline 1902, the component gas pipeline 1903, the gas distribution main pipeline 1904 and the exhaust gas main pipeline 1905, and then evacuate; S2, quantitatively filling the reference gas cylinder 6 with a balance gas of mass m1, and then repeating step S1; S3, quantitatively filling the reference gas cylinder 6 with component gases of mass m2 to obtain a mixed gas, and then repeating step S1; S4, checking whether the mixed gas in step S3 is qualified; S4.1. When the detected mixed gas is qualified, the mixed gas cylinder 12 and the reference gas cylinder 6 are qualified; repeat steps S2 to S4. S4.2. When the mixed gas is detected to be unqualified, the mixed gas cylinder 12 and the reference gas cylinder 6 are first deflated and then vacuumized; and steps S1 to S4 are repeated.

[0045] When filling the mixed gas container 12 with balancing gas, open the first reference valve 601 to set the flow rate of the reference gas cylinder 6 to be the same as the flow rate of the first mixed gas valve 1201 of the mixed gas container 12. After the reference gas cylinder 6 is filled to a mass of m1, let it stand for a while and observe whether the balance reading of the precision electronic scale 7 is stable. After the mass of the reference gas cylinder 6 of the mixed gas container 12 reaches stability, the mass of the balancing gas filled in both is the same, which is m1.

[0046] When filling and discharging the mixed gas container 12, open the first reference valve 601 to set the flow rate of the reference gas cylinder 6 to be the same as the flow rate of the first mixed gas valve 1201 of the mixed gas container 12. After the mass of the reference gas cylinder 6 increases by m2, let it stand for a while and observe whether the balance reading of the precision electronic scale 7 is stable. After the masses of the mixed gas container 12 and the reference gas cylinder 6 become stable, the increased mass of both is m2.

[0047] If the mixed gas cylinder 12 passes the test, the reference gas cylinder 6 also passes; otherwise, both are judged to be unqualified; This device also has a cleaning function. When the gas supply is insufficient or the raw gas leaks or the raw gas purity is unqualified, causing the gas distribution main pipeline 1904 to be contaminated, the unqualified product gas in the mixed gas container 12 and the spare mixed gas container 13 can be released first through the first exhaust valve 1402 in the exhaust main pipeline 1905, and then the No. 1 vacuum valve 1302 can be evacuated with a vacuum pump.

[0048] Similarly, the unqualified product gas of the reference gas cylinder 6 and the recovery gas cylinder 8 is first deflated through the second buffer valve 1403, and then vacuumed through the vacuum pump No. 2 vacuum valve 1303. This arrangement can protect the thermocouple vacuum gauge 11 from the influence of gas and can also extend the service life of the pressure gauge.

[0049] The fourth one-way valve 1401 can prevent the exhaust gas from flowing back. The present invention integrates the electronic gas distribution, cleaning, ventilation and gas recovery together, and can also be applied to the precise configuration of other gases.

[0050] When the component gas container 4 and the balance gas container 3 are used to a pressure that is insufficient to fill the mixed gas container 12, multiple recovery gas cylinders 8 are connected to the component gas container 4 and the balance gas container 3 in turn, and the system is replaced three to five times with helium. Then, the recovery gas cylinder 8 is placed in a liquid nitrogen cylinder 9 with a jacket containing liquid nitrogen, and then the gas outlet valves of the component gas container 4 and the balance gas container 3 are opened respectively. The gas in the recovery gas cylinder 8 is condensed by cooling with liquid nitrogen to form a vacuum state and the gas is recovered due to the pressure difference. After the recovery is completed, the air inlet valve and the air outlet valve are closed, and the system is replaced with nitrogen three to five times before the recovery gas cylinder 8 is removed.

[0051] Example 2 See attached Figure 1 , the connection relationship of each device of the present invention is as follows: A nitrogen valve 101 is provided at the outlet of the nitrogen container 1, and a helium valve 201 is provided at the outlet of the helium container 2. The nitrogen valve 101 and the helium valve 201 are connected to the replacement pipe 1901. The replacement pipe 1901 is equipped with a first replacement valve 202, a second replacement valve 203, a third replacement valve 204, and a fourth replacement valve 205. The first replacement valve 202 is connected to the balance gas pipeline 1902 and is used for replacing the balance gas pipeline 1902 and the component gas container 3. The second replacement valve 203 is connected to the balance gas pipeline 1903 and is used for replacing the balance gas pipeline 1903 and the balance gas container 4. The third replacement valve 204 is connected to the gas distribution main pipeline 1904 and is used for replacing the recovery gas cylinder 8 and the reference gas cylinder 6. The fourth replacement valve 205 is connected to the gas distribution main pipeline 1904 and is used for replacing the mixed gas container 12 and the spare mixed gas container 13.

[0052] A balancing gas valve 301 is provided at the outlet of the balancing gas container 3, and a second one-way valve 501 is connected to the back of the balancing gas valve 301; a component gas valve 401 is provided at the outlet of the component gas container 4, and a first one-way valve 5 is connected to the back of the component gas valve 401; the exhaust pipes of the balancing gas pipeline 1902 and the component gas pipeline 1903 are connected to the gas distribution main pipeline 1904 via the main pipeline outlet valve 602; the balancing gas pipeline 1902 is connected to the vacuum main pipeline 1906 via the No. 4 vacuum valve 1305, which is used for vacuuming the balancing gas container 3 and the balancing gas pipeline 1902; the component gas pipeline 1903 is connected to the vacuum main pipeline 1906 via the No. 3 vacuum valve 1304, which is used for vacuuming the component gas container 4 and the component gas pipeline 1903.

[0053] The gas distribution main pipeline 1904 is connected in sequence with the reference gas cylinder 6, the recovery gas cylinder 8, the high-pressure valve 10, the high-pressure gauge 1001; the medium-pressure gauge 1002; the low-pressure gauge 1003; the thermocouple vacuum gauge 11, the mixed gas container 12 and the spare mixed gas container 13. The reference gas cylinder 6 is connected to the gas distribution main pipeline 1904 via the first reference valve 601, and the reference gas cylinder 6 is placed on the precision electronic scale 7. The recovery gas cylinder 8 is connected to the gas distribution main pipeline 1904 via the recovery gas valve 801, and the recovery gas cylinder 8 is placed in the liquid nitrogen cylinder 9. The high-pressure valve 10 is divided into a high-pressure gauge 1001, a medium-pressure gauge 1002, and a low-pressure gauge 1003, so as to more accurately display the pressure value on the gas distribution main pipeline.

[0054] There are pipelines before and after the pressure gauge on the gas distribution main pipeline 1904, respectively, connected to the exhaust main pipeline 1905 through the second exhaust valve 1403 and the first exhaust valve 1402. The second exhaust valve 1403 is used to discharge the exhaust gas from the reference gas cylinder 6 and the recovery gas cylinder 8, and the first exhaust valve 1402 is used to discharge the exhaust gas from the mixed gas container 12. The rear end of the exhaust main pipeline 1905 is connected to a check valve 1401, and the exhaust buffer tank 15 is connected to the rear end of the check valve 1401. The rear end of the vacuum main pipe 1906 is connected to a check valve 1301, and the vacuum pump 14 is connected to the rear end of the check valve 1301. The vacuum pump 14 is connected to the exhaust buffer tank 15. The reason for installing the check valve is to prevent the exhaust gas in the exhaust buffer tank 15 and the possible air from flowing back to the gas distribution main pipeline 1904 to cause explosion or pollute the gas. The tail gas buffer tank 15 is connected to the tail gas absorption tower 20. The absorbent in the tail gas absorption tower 20 is pressurized from the bottom of the tower by the circulation pump 19 and then poured into the top of the absorption tower through the circulation valve 1801. The absorbed tail gas is discharged from the top of the absorption tower through the vent valve 2001.

[0055] The mixed gas container 12 and the spare mixed gas container 13 are connected to the detection main pipeline 1909 via the first detection valve 1202 and the second detection valve 1204 respectively, which is convenient for direct detection of the mixed gas product. The detection main pipeline 1909 is connected with a pressure reducing valve 16, and the pressure reducing valve 16 is connected with a chromatograph 17 and a moisture meter 18. The function of the pressure reducing valve 16 is to reduce the pressure of the mixed gas to 0.4MPa before entering the instrument for detection.

[0056] Determine the ratio of the balance gas and the component gas in the mixed gas, and calculate the masses m1 and m2 of the balance gas and the component gas.

[0057] Pipe replacement drainage and air removal: S-1, connect the nitrogen container 1, the helium container 2, the balance gas container 3, the component gas container 4, the reference gas cylinder 6, the mixed gas container 12, and the spare mixed gas container 13 to the filling system; S-2. Open the nitrogen valve 101 at the outlet of the nitrogen container 1, the first replacement valve 202, the second replacement valve 203, the main pipeline outlet valve 602, and the first tail gas valve 1402 in sequence. The nitrogen is pressurized to 0.2 MPa and flows out through the nitrogen container 1 through the first replacement valve 202 into the balancing gas pipeline 1902, and then enters the component gas pipeline 1903 through the second replacement valve 203. The nitrogen in the component gas pipeline 1903 and the balancing gas pipeline 1902 enters the gas distribution main pipeline 1904 through the main pipeline outlet valve 602, and is then discharged to the tail gas buffer tank 15 through the first tail gas valve 1402. The whole purge process lasts for 1 hour. The purpose is to blow away the air and moisture in the replacement pipeline 1901, the balancing gas pipeline 1902, the component gas pipeline 1903, the gas distribution main pipeline 1904, and the tail gas main pipeline 1905.

[0058] S-3. Close all valves in step S-2, start the vacuum pump 14, and then open the No. 1 vacuum valve 1302 to evacuate the system. Draw the nitrogen in the balance gas pipeline 1902, the component gas pipeline 1903, and the gas distribution main pipeline 1904 through the No. 1 vacuum valve 1302 to the vacuum pipeline 1906, and then discharge it to the tail gas buffer tank 15. After the thermocouple vacuum gauge 11 shows that the vacuum degree is 1Pa, close the No. 1 vacuum valve 1302, and then turn off the vacuum pump 14 to stop evacuating the system.

[0059] S-4. Repeat steps S-2 and S-3 five times, and finally keep the pipeline in a vacuum state.

[0060] S-5. Replace the nitrogen in steps S-2 and S-3 with helium, cycle steps S-2 and S-3 five times, and finally keep the pipeline in a vacuum state.

[0061] Balance gas quantitative filling: (1) Open the first mixed gas valve 1201, the first reference valve 601, the main pipeline outlet valve 602, and the balancing gas valve 301 in sequence. The balancing gas enters the balancing gas pipeline 1902 from the balancing gas container 3 through the balancing gas valve 301, and then enters the gas distribution main pipeline 1904 through the main pipeline outlet valve 602. It enters the reference gas cylinder 6 through the first reference valve 601 and enters the mixed gas container 12 through the first mixed gas valve 1201. The air intake flow rate is controlled by adjusting the opening of the balancing gas valve 301 until the precision electronic scale 7 shows that the mass of the reference gas cylinder 6 reaches m1. The first mixed gas valve 1201 is cut off to stop charging the mixed gas container 12, and then the first reference valve 601, the main pipeline outlet valve 602, and the balancing gas valve 301 are closed in sequence.

[0062] (2) Use nitrogen to replace the pipeline, repeat steps S-2 and S-3 in the pipeline replacement five times, and finally keep the pipeline in a vacuum state.

[0063] (3) Replace nitrogen with helium, repeat steps S-2 and S-3 in the pipeline replacement five times, and finally keep the pipeline in a vacuum state.

[0064] Quantitative filling of component gases: (1) Open the first mixed gas valve 1201, the first reference valve 601, the main pipeline outlet valve 602, and the component gas valve 401 in sequence. The component gas enters the component gas pipeline 1903 from the component gas container 4 through the component gas valve 401, and then enters the gas distribution main pipeline 1904 through the main pipeline outlet valve 602. The gas in the gas distribution main pipeline 1904 enters the reference gas cylinder 6 through the first reference valve 601 and enters the mixed gas container 12 through the first mixed gas valve 1201. The intake flow rate is controlled by adjusting the opening of the component gas valve 401 until the precision electronic scale 7 shows that the mass of the reference gas cylinder 6 reaches m3; m3=m1+m2, and the first mixed gas valve 1201 is cut off to stop charging the mixed gas container 12, and then the first reference valve 601, the main pipeline outlet valve 602, and the component gas valve 401 are closed in sequence. The reference gas cylinder 6 is the filled electronic grade mixed gas.

[0065] (2) Use nitrogen to replace the pipeline, repeat steps S-2 and S-3 in the pipeline replacement five times, and finally keep the pipeline in a vacuum state.

[0066] (3) Replace nitrogen with helium, repeat steps S-2 and S-3 in the pipeline replacement five times, and finally keep the pipeline in a vacuum state.

[0067] Mixed gas detection: (1) Open the first detection valve 1202. The mixed gas enters the detection main pipeline 1909 from the mixed gas container 12 through the first detection valve 1202, and then enters the helium ion chromatograph 17 and the moisture meter 18 to analyze the gas component content of the mixed gas after the pressure is adjusted to 0.4 MPa by the pressure reducing valve 16. Then, the first detection valve 1202 is closed.

[0068] (2) While waiting for the test result of the mixed gas container 12, the mixed gas container 12 can be disassembled and the mixed gas container 13 can be inflated according to the above-mentioned steps of quantitative filling of component gases and quantitative filling of mixed gas.

[0069] Raw material recycling: (1) When the residual pressure in the component gas container 4 is insufficient to fill a complete mixed gas container 12, the recovery gas cylinder 8 is connected to the system and then replaced with helium. Then, steps S-2 and S-3 in the pipeline replacement are repeated five times, and finally the pipeline is kept in a vacuum state.

[0070] (2) The recovery gas cylinder 8 is placed in a liquid nitrogen cylinder 9 with a jacket containing liquid nitrogen, and then the component gas valve 401, the main pipeline outlet valve 602, and the recovery gas valve 801 are opened in sequence. The component gas enters the component gas pipeline from the component gas container through the component gas valve 401, then enters the main pipeline 1904 through the main pipeline outlet valve 602, and then enters the recovery gas cylinder 8 through the recovery gas valve 801. The remaining component gas in the component gas container 4 is recovered by the pressure difference formed by the vacuum state formed by the condensation of the gas in the recovery gas cylinder 8 by the liquid nitrogen cooling. After the recovery is completed, the component gas valve 401, the main pipeline outlet valve 602, and the recovery gas valve 801 are closed in sequence.

[0071] (3) Use nitrogen replacement and repeat steps S-2 and S-3 in the pipeline replacement five times, and finally keep the pipeline in a vacuum state.

[0072] Although the specific implementation modes of the present invention are described above, those skilled in the art should understand that the specific implementation modes described are only illustrative and are not intended to limit the scope of the present invention. Equivalent modifications and changes made by those skilled in the art in accordance with the spirit of the present invention should be included in the scope of protection of the claims of the present invention.

Claims

1. An electronic grade mixed gas distribution device, comprising a nitrogen container (1), characterized in that: The outlet pipe of the nitrogen container (1) is connected to the inlet pipe of the replacement pipeline (1901) through the nitrogen valve (101); The inlet pipe of the replacement pipeline (1901) is also connected to the outlet pipe of the helium container (2) through the helium valve (201). A branch pipe 1 of the replacement pipe (1901) is connected to the inlet of the balancing gas pipe (1902) through a first replacement valve (202); The branch pipe 2 of the replacement pipe (1901) is connected to the inlet of the component gas pipe (1903) through the second replacement valve (203); The branch pipe 3 of the displacement pipe (1901) is connected to the middle part of the gas distribution main pipe (1904) through the third displacement valve (204); The inlet of the gas outlet valve (602) of the gas distribution main pipeline (1904) is connected in parallel to the outlets of the balance gas pipeline (1902) and the component gas pipeline (1903); The main gas distribution pipeline (1904) is also connected to the vacuum main pipeline (1906) via a No. 1 vacuum valve (1302) and a No. 2 vacuum valve (1303) connected in parallel.

2. The electronic grade mixed gas distribution device according to claim 1, characterized in that: The inlet of the balancing gas pipeline (1902) is also connected in series with a second one-way valve (501) and a balancing gas valve (301), and the balancing gas valve (301) is connected to the gas outlet pipe of the balancing gas container (3).

3. The electronic grade mixed gas distribution device according to claim 1, characterized in that: The inlet of the component gas pipeline (1903) is also connected in series with the first one-way valve (5) and the component gas valve (401), and the component gas valve (401) is connected to the gas outlet pipe of the component gas container (4).

4. The electronic grade mixed gas distribution device according to claim 1, characterized in that: The gas distribution main pipeline (1904) is connected to the reference gas cylinder (6) through a pipeline and a first reference valve (601), and the gas distribution main pipeline (1904) is connected to the recovery gas cylinder (8) through a pipeline and a recovery gas valve (801). The reference gas cylinder (6) and the recovery gas cylinder (8) are both located on the outlet side of the gas outlet valve (602). The reference gas cylinder (6) is installed on a precision electronic scale (7), and the recovery gas cylinder (8) is installed inside a liquid nitrogen cylinder (9). The outlet of the gas distribution main pipeline (1904) is connected to the mixed gas container (12) through the first mixed gas valve (1201). The gas inlet pipe of the mixed gas container (12) is also connected to the gas inlet of the pressure reducing valve (16) of the detection main pipeline (1909) through the first detection valve (1202). The gas outlet of the pressure reducing valve (16) is connected in parallel to the sampling ports of the chromatograph (17) and the moisture meter (18).

5. The electronic grade mixed gas distribution device according to claim 1, characterized in that: The branch pipe of the vacuum main pipeline (1906) is connected to the component gas pipeline (1903) through the third vacuum valve (1304); the branch pipe of the vacuum main pipeline (1906) is also connected to the balance gas pipeline (1902) through the fourth vacuum valve (1305); the vacuum main pipeline (1906) is also connected to the vacuum pump (14) through the third one-way valve (1301), the exhaust pipe of the vacuum pump (14) is connected to the exhaust buffer tank (15), and the inlet pipe of the buffer tank (15) is also connected to the exhaust port of the exhaust main pipeline (1905) through the fourth one-way valve (1401), and the branch pipe of the exhaust main pipeline (1905) is connected to the gas distribution main pipeline (1904) through the first exhaust valve (1402) and the second exhaust valve (1403) connected in parallel.

6. The electronic grade mixed gas distribution device according to claim 1, characterized in that: The branch pipe 4 of the displacement pipe (1901) is connected to the rear side of the thermocouple vacuum gauge (11) at the tail end of the gas distribution main pipe (1904) through the fourth displacement valve (205); on the front side of the thermocouple vacuum gauge (11), the gas distribution main pipe (1904) is also connected in parallel with a high-pressure valve (10), a medium-pressure valve and a low-pressure valve; the high-pressure valve (10) is connected to the high-pressure gauge (1001), the medium-pressure valve is connected to the medium-pressure gauge (1002), and the low-pressure valve is connected to the low-pressure gauge (1003).

7. The electronic grade mixed gas distribution device according to claim 1, characterized in that: The outlet of the gas distribution main pipeline (1904) is connected to the spare mixed gas container (13) through the second mixed gas valve (1203); the air inlet pipe of the spare mixed gas container (13) is also connected to the air inlet of the pressure reducing valve (16) of the detection main pipeline (1909) through the second detection valve (1204).

8. The electronic grade mixed gas distribution device according to claim 5, characterized in that: The outlet pipe of the buffer tank (15) is connected to the inlet of the tail gas absorption tower (20), and the tail gas absorption tower (20) is equipped with a liquid replenishment pipe (1907) and a waste liquid pipe (1908); a circulation pump (19) is installed at the bottom of the tail gas absorption tower (20), and the output end of the circulation pump (19) is connected to the top of the tail gas absorption tower (20) through a circulation valve (1801), and the top of the tail gas absorption tower (20) is also equipped with a vent valve (2001).

9. The electronic grade mixed gas distribution device according to claim 5, characterized in that: The connection between the second tail gas valve (1403) and the gas distribution main pipeline (1904) is located at the rear side of the connection between the reference gas cylinder (6) and the recovery gas cylinder (8) and the gas distribution main pipeline (1904), and is located at the front side of the connection between the high pressure gauge (1001) and the gas distribution main pipeline (1904).

10. The method for operating the electronic grade mixed gas distribution device according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. Use inert gas to purge the replacement pipeline 1901, the balance gas pipeline 1902, the component gas pipeline 1903, the gas distribution main pipeline 1904 and the exhaust gas main pipeline 1905, and then evacuate; S2, quantitatively fill the reference gas cylinder 6 with a mass of m1 balance gas, and repeat step S1; S3, quantitatively filling the reference gas cylinder 6 with component gases having a mass of m2 to obtain a mixed gas, and repeating step S1; S4. Check whether the mixed gas is qualified; S4.1, when the detected mixed gas is qualified, the mixed gas cylinder 12 and the reference gas cylinder 6 are qualified; repeat steps S2 to S4; S4.

2. When the mixed gas is detected to be unqualified, the mixed gas cylinder 12 and the reference gas cylinder 6 are first deflated and then vacuumized; and steps S1 to S4 are repeated.

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