An automatic sampling system for mass spectrometers in the electronic specialty gas industry

Abstract

The present invention discloses an automatic sampling system for mass spectrometers in the electronic specialty gas industry, comprising a displacement and purge airway system, a sampling system, a pressure control system, a vacuum venting system, and a PLC control system, wherein the PLC control system is electrically connected to the displacement and purge airway system, the sampling system, the pressure control system, and the vacuum venting system. The automatic sampling system for mass spectrometers in the electronic specialty gas industry described in the present invention establishes automatic functional modules such as helium detection, displacement, sampling, and purging, realizing one-button operation; the system is subjected to sampling control tests under different pressure conditions, and can simultaneously meet the requirements of stable sampling of ultra-high and ultra-low pressure electronic specialty gas spectrometers at 1-10 torr pressure, and a mass spectrometer cavity pressure of 3E ‑6 to 8E ‑5 Torr stable analysis realizes stable output control of high-pressure, ultra-low-pressure samples, purge gas and other gases with different pressures, ensures sample outflow stability, meets the needs of high-end mass spectrometry analysis and detection, and brings better usage prospects.

Description

Technical Field

[0001] The present invention relates to the field of high-purity electronic special gases, and in particular to an automatic sampling system for a mass spectrometer in the electronic special gas industry. Background Art

[0002] In recent years, with the development of high-purity electronic specialty gases in China, the purity and production capacity of these gases, commonly used in the integrated circuit and panel industries, have significantly improved, contributing to the improvement of the domestic electronic specialty gas industry chain. With the increasing integration of integrated circuits and their application in a wide range of fields, such as aerospace, cloud computing, high-speed trains, communications, and networking, the requirements for the operating speed, stability, reliability, and safety of electronic equipment are constantly increasing. The requirements for key process materials in manufacturing-related facilities are no longer limited to general purity requirements, but have risen to the level of full-spectrum mass spectrometry analysis and comprehensive quality monitoring.

[0003] The delivery of high-purity electronic gases generally relies on pressure devices such as stainless steel pipes and cylinders. Gases such as germanium tetrafluoride and boron trifluoride are often highly toxic, corrosive, highly adhesive, and highly reactive with water. Extremely low-pressure samples are also present during the isotope centrifugation process. These properties, when used in the analysis and testing process, require not only clean, leak-free replacement of connecting pipes but also prolonged purging of the analytical pipelines and instruments. Our earlier patent, CN208688755U, "A High-Purity Specialty Gas Replacement Panel," addresses the flammable, explosive, and highly toxic properties of high-purity phosphine and arsine, providing a high-purity specialty gas replacement panel that ensures the airtightness of the entire system. This panel enables the delivery of high-pressure gas samples without introducing new impurities during operation, ensuring product purity and the safety of the working environment. However, this patent does not meet the requirements for stable, low-pressure input from mass spectrometers in high-end analytical testing instruments. In addition, in view of the characteristics of remote monitoring and analysis of the highly toxic gas generation process, targeted programming of pneumatic valves, pressure signal units, pressure controllers and PLCs is used to ultimately achieve stable output control of high-pressure, ultra-low-pressure samples, purge gases and other gases at different pressures, ensuring sample outflow stability and meeting the needs of high-end mass spectrometry analysis and detection.

[0004] Mass spectrometers are widely used in the electronic specialty gas industry, especially for fluorine-containing gases such as germanium tetrafluoride and boron trifluoride. They can achieve direct sampling, full spectrum scanning over a wide mass range, accurate quantification of common impurities in helium standard gas, and abundance calculation based on the response of different mass-to-charge ratios of isotopes. Conventional chromatography and Fourier transform infrared cannot meet these requirements at the same time. However, if a mass spectrometer is to achieve the analysis and detection of impurities, the injection pressure must be constant and the injection port pressure must be within 5E. -5 to 5E - 6torr, and in order to protect the internal quadrupole, purge gas is required to be purged in real time, and the purge mode needs to be below 1E -4 torr vacuum pressure.

[0005] To this end, we propose an automatic sampling system for mass spectrometers in the electronic specialty gas industry. Summary of the Invention

[0006] The main purpose of the present invention is to provide an automatic sampling system for mass spectrometers in the electronic specialty gas industry, which can effectively solve the problems in the background technology.

[0007] To achieve the above object, the technical solution adopted by the present invention is:

[0008] An automatic sampling system for mass spectrometers in the electronic specialty gas industry, comprising a displacement purge gas system, a sampling system, a pressure control system, a vacuum venting system, and a PLC control system, wherein the PLC control system is electrically connected to the displacement purge gas system, the sampling system, the pressure control system, and the vacuum venting system, and the sampling system, the displacement purge gas system, and the vacuum venting system are all connected to the pressure control system;

[0009] The displacement purge gas system is used to adjust the output pressure of the gas;

[0010] The sample injection system is used to guide the high-pressure sample into the automatic sample injection system or the low-pressure sample into the automatic sample injection system;

[0011] The pressure control system is used to adjust and obtain the pressure data of the gas in the automatic sampling system;

[0012] The vacuum venting system is used to complete the venting, evacuation, and replacement of high and low pressure gases and the replacement and purging of the sampling pipeline;

[0013] The PLC control system is used to control the operation of the entire automatic sampling system.

[0014] Preferably, the replacement purge air path system comprises two groups of replacement purge air paths, and the replacement purge air paths are sequentially provided with a one-way valve, a first pressure gauge, a pressure reducing gauge and a first diaphragm valve.

[0015] Preferably, the pressure control system includes a primary pressure reducing device and a secondary pressure reducing device, and both the primary pressure reducing device and the secondary pressure reducing device are connected to two sets of replacement purge air paths.

[0016] Preferably, the first-stage pressure reducing device includes a pressure reducing valve and a first pressure transmitter, and the pressure reducing valve is connected to the first pressure transmitter.

[0017] Preferably, the secondary pressure reducing device includes a pressure controller, a second pressure transmitter and several groups of second diaphragm valves.

[0018] Preferably, the injection system includes two groups of high-pressure injection ports and two groups of low-pressure injection ports, and a third diaphragm valve is provided on the pipelines of the two groups of high-pressure injection ports and the two groups of low-pressure injection ports. The high-pressure injection ports are connected to the pipeline between the first-level pressure reducing device and the replacement purge gas system, and the low-pressure injection ports are connected to the pipeline between the first-level pressure reducing device and the second-level pressure reducing device.

[0019] Preferably, the vacuum venting system includes a vacuum outlet connected to the vacuum equipment and a venting outlet connected to the tail gas treatment equipment, and a fourth diaphragm valve and a second pressure gauge are provided on the pipelines of the vacuum outlet and the venting outlet.

[0020] Preferably, the PLC control system includes a pneumatic valve, a pressure sensor, a PLC control box and an automatic control touch screen.

[0021] Compared with the prior art, the present invention provides an automatic sampling system for mass spectrometers in the electronic specialty gas industry, which has the following beneficial effects:

[0022] 1. The present invention provides an automatic sampling system for mass spectrometers in the electronic specialty gas industry to establish automatic functional modules such as helium detection, replacement, sampling, and purging, realizing one-button operation; the system is tested for sampling control under different pressure conditions, and can simultaneously meet the requirements of ultra-high pressure and ultra-low pressure electronic specialty gas spectrometers with a pressure of 1-10 torr and a mass spectrometer cavity pressure of 3E -6 to 8E -5 torr stability analysis;

[0023] 2. The automatic sampling system for mass spectrometers in the electronic special gas industry of the present invention realizes stable output control of high-pressure, ultra-low-pressure samples, purge gas and other gases of different pressures, ensures sample outflow stability, meets the needs of high-end mass spectrometry analysis and detection, and has better use effect than traditional methods, meets people's use requirements, and is more practical.

[0024] The parts not involved in the device are the same as those in the prior art or can be implemented by using the prior art. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a structural diagram of an automatic sampling system for a mass spectrometer in the electronic specialty gas industry according to the present invention. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0027] In the description of the present invention, it should be understood that the terms "upper", "lower", "front", "back", "left", "right", "top", "bottom", "inside", "outside", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore should not be understood as limiting the present invention.

[0028] Example 1

[0029] An automatic sampling system for mass spectrometers in the electronic specialty gas industry, such as Figure 1 As shown, it includes a displacement purge gas system, a sampling system, a pressure control system, a vacuum venting system and a PLC control system. The PLC control system is electrically connected to the displacement purge gas system, the sampling system, the pressure control system and the vacuum venting system. The sampling system, the displacement purge gas system and the vacuum venting system are all connected to the pressure control system.

[0030] Replacement purge gas system, used to adjust the gas output pressure;

[0031] Injection system, used to guide high-pressure samples into or low-pressure samples into the automatic injection system;

[0032] Pressure control system, used to adjust and obtain gas pressure data in the automatic sampling system;

[0033] Vacuum venting system, used to complete the venting, evacuation, replacement of high and low pressure gases and replacement and purging of the sampling pipeline;

[0034] PLC control system is used to control the operation of the entire automatic sampling system.

[0035] The replacement purge gas system includes two sets of replacement purge gas lines. The replacement purge gas lines are sequentially provided with a one-way valve, a first pressure gauge, a pressure reducing gauge and a first diaphragm valve. They can meet the maximum input of 3000psi and the maximum output of 160psi, and complete the helium inspection, disconnection and replacement of cylinders of common electronic special gases, panel injection pipeline replacement, and instrument purge functions.

[0036] The two sets of replacement purge gas lines use nitrogen and helium as cleaning gases, but are not limited to commonly used gases in the gas industry, such as compressed air.

[0037] The pressure control system comprises a primary pressure reducing device and a secondary pressure reducing device, and both the primary pressure reducing device and the secondary pressure reducing device are communicated with two groups of displacement purge air paths.

[0038] The first-stage pressure reducing device includes a pressure reducing valve and a first pressure transmitter. The pressure reducing valve is connected to the first pressure transmitter and can meet 3000psi input and a maximum output of 160psi.

[0039] The secondary pressure reducing device includes a pressure controller, a second pressure transmitter and several groups of second diaphragm valves. The minimum output pressure of the pressure controller is 1-20 torr. The pressure controller adopts a digital pressure controller.

[0040] The pressure controller and the second pressure transmitter are not limited to pressure reducing gauges and pressure gauges of related brands in the industry.

[0041] The pressure gauge has a range of (-30-160psi), and the pressure transmitter has a range of (0.1atm, 1atm). The PLC automatic control system is used to complete the corresponding pressure signal electrical acquisition and program feedback.

[0042] The injection system includes two sets of high-pressure injection ports and two sets of low-pressure injection ports. The pipelines of the two sets of high-pressure injection ports and the two sets of low-pressure injection ports are all equipped with third diaphragm valves. The pipelines between the high-pressure injection ports and the first-stage pressure reducing device and the displacement purge gas system are connected and located before the first pressure gauge input port. It is suitable for the injection of samples with an absolute pressure of 0.1-20 MPa and undergoes two-stage pressure reduction. The output pressure does not exceed 10 Torr.

[0043] The diaphragm valve in this patent adopts a pneumatic diaphragm valve.

[0044] The low-pressure inlet is connected to the pipeline between the first-level pressure reducing device and the second-level pressure reducing device, which is located after the first pressure gauge input port. Samples of 10-1000 torr need to be controlled by the second-level pressure reducing device of the pressure controller, and the output pressure does not exceed 10 torr; samples below 10 torr do not undergo pressure control and are directly bypassed and injected through the low-pressure inlet.

[0045] The vacuum venting system includes a vacuum outlet connected to the vacuum equipment and a venting outlet connected to the exhaust gas treatment equipment. The fourth diaphragm valve and the second pressure gauge are installed on the pipelines of the vacuum outlet and the venting outlet to cooperate with the replacement and purge air circuit to complete the venting, evacuation and replacement of high and low pressure gases, and the replacement and purge of the sampling pipeline.

[0046] The vacuum equipment is composed of an adsorption barrel and a vacuum pump, but is not limited to vacuuming methods such as cold hydrazine collection commonly used in this field.

[0047] The PLC control system includes pneumatic valves, pressure sensors, a PLC control box, and an automatic control touch screen. The pneumatic valves can be driven by compressed air or nitrogen, with a driving pressure of 4-5 bar. The pressure transmitter has a range of 0.1 bar and 1 bar, and cooperates with the completion of vacuuming and valve opening under different conditions. The PLC control box is a circuit and gas circuit module. The automatic control touch screen has built-in automatic control programs such as helium detection, replacement, injection, and purge, and controls the corresponding modules through the touch screen.

[0048] The PLC control system includes high and low pressure injection function modules and high and low pressure helium detection and purge modules, but is not limited to the program design of the above function modules. It includes but is not limited to adding function modules such as pressure signal alarm settings and related emergency operations based on application extensions.

[0049] The components of the automatic sampling system are connected by EP-grade stainless steel piping with VCR-type interfaces. After the sample bottle is connected to the automatic sampling system, it undergoes leak testing, replacement, injection, and post-replacement to complete the sampling and analysis operation.

[0050] Example 2

[0051] right Figure 1 Further number descriptions are added, where the first pressure gauge and the second pressure gauge are both numbered PI101, the two sets of first diaphragm valves are numbered PCV103 and PCV10104, and the several sets of second diaphragm valves are numbered PCV207, PCV206, and PCV205 respectively; the third diaphragm valves are numbered PCV201, PCV202, PCV203, and PCV204 respectively, and the fourth diaphragm valves are numbered PCV101 and PCV102 respectively;

[0052] The first pressure transmitter is numbered WIKA-2, and the second pressure transmitter is numbered WIKA-1;

[0053] The two groups of high-pressure inlets are numbered as inlet 1 and inlet 2, and the two groups of low-pressure inlets are numbered as inlet 3 and inlet 4.

[0054] The high-pressure sample helium detection and replacement workflow of the automatic sampling panel in this embodiment is automatically controlled and will automatically stop in the event of an abnormality. The automatic program flow is as follows: taking sampling port 1 as an example, open PCV101 and PCV202, pump to the WIKA-1 reading of -14.7psi, maintain for 120s, close PCV101, and the WIKA-1 reading of -14.7psi within 60s indicates that the low-pressure holding test has passed, and then proceed to the next step of high-pressure holding test.

[0055] Open PCV104, and the WIKA-2 reading will remain at 20psi for 15 seconds. Then close PCV104, and the WIKA-2 reading will be 15psi within 60 seconds, indicating that the high-pressure holding test has passed. Then proceed to the next replacement operation.

[0056] Open PCV101, PCV205, and PCV206, pump until the WIKA-1 reading reaches -14.7 psi, hold for 30 seconds, close PCV101, and then enter the replacement procedure.

[0057] Open PCV104, hold for 15 seconds, then close PCV104, open PCV101, pump until the WIKA-1 reading reaches -14.7 psi, hold for 30 seconds, then close PCV101 after 30 seconds, and repeat 10 times; then reset all valves.

[0058] Example 3

[0059] right Figure 1 Further number descriptions are added, where the first pressure gauge and the second pressure gauge are both numbered PI101, the two sets of first diaphragm valves are numbered PCV103 and PCV10104, and the several sets of second diaphragm valves are numbered PCV207, PCV206, and PCV205 respectively; the third diaphragm valves are numbered PCV201, PCV202, PCV203, and PCV204 respectively, and the fourth diaphragm valves are numbered PCV101 and PCV102 respectively;

[0060] The first pressure transmitter is numbered WIKA-2, and the second pressure transmitter is numbered WIKA-1;

[0061] The two groups of high-pressure inlets are numbered as inlet 1 and inlet 2, and the two groups of low-pressure inlets are numbered as inlet 3 and inlet 4.

[0062] The high-pressure sample automatic injection and post-displacement workflow of the automatic injection panel in this embodiment is automatically controlled and will automatically stop in the event of an abnormality. The automatic program flow is as follows: Taking injection port 1 as an example, all valves are initially closed. PCV101, PCV202, PCV205, PCV206, and PCV207 are opened. Then, they are held for 120 seconds, and PCV101, PCV205, and PCV206 are closed. The cylinder valve is then manually opened. When the WIKA-1 reading reaches 0 psi, PCV205 is opened, and injection analysis begins.

[0063] After the analysis is complete, initially close all valves and manually close the cylinder valve. Open PCV101 and PCV202, pump to a WIKA-1 reading of -14.7 psi, and hold for 30 seconds. After 30 seconds, close PCV101 and open PCV104 until the WIKA-1 reading is 0 psi. Repeat this 10 times. After the tenth cycle, the WIKA-1 reading will be 0 psi. Reset all valves and remove the high-pressure cylinder.

[0064] Example 4

[0065] right Figure 1Further number descriptions are added, where the first pressure gauge and the second pressure gauge are both numbered PI101, the two sets of first diaphragm valves are numbered PCV103 and PCV10104, and the several sets of second diaphragm valves are numbered PCV207, PCV206, and PCV205 respectively; the third diaphragm valves are numbered PCV201, PCV202, PCV203, and PCV204 respectively, and the fourth diaphragm valves are numbered PCV101 and PCV102 respectively;

[0066] The first pressure transmitter is numbered WIKA-2, and the second pressure transmitter is numbered WIKA-1;

[0067] The two groups of high-pressure inlets are numbered as inlet 1 and inlet 2, and the two groups of low-pressure inlets are numbered as inlet 3 and inlet 4.

[0068] The low-pressure sample helium test and replacement workflow of the automated sampling panel in this embodiment is automatically controlled and will automatically stop if an abnormality occurs. The automated process, using sampling port 3 as an example, begins with all valves closed. PCV101 and PCV203 are opened, pumping to a WIKA-1 reading of -14.7 psi and maintaining this reading for 120 seconds. PCV101 is then closed, and within 60 seconds, the WIKA-1 reading will be -14.7 psi, indicating a low-pressure hold test has passed. The replacement process then proceeds to the next step.

[0069] Open PCV101, PCV205, and PCV206, pump until the WIKA-1 reading reaches -14.7 psi, hold for 30 seconds, close PCV101, and then enter the replacement procedure.

[0070] Open PCV104, hold for 15 seconds, then close PCV104, open PCV101, pump until the WIKA-1 reading reaches -14.7 psi, hold for 30 seconds, then close PCV101 after 30 seconds, and repeat 10 times; then reset all valves.

[0071] Example 5

[0072] right Figure 1 Further number descriptions are added, where the first pressure gauge and the second pressure gauge are both numbered PI101, the two sets of first diaphragm valves are numbered PCV103 and PCV10104, and the several sets of second diaphragm valves are numbered PCV207, PCV206, and PCV205 respectively; the third diaphragm valves are numbered PCV201, PCV202, PCV203, and PCV204 respectively, and the fourth diaphragm valves are numbered PCV101 and PCV102 respectively;

[0073] The first pressure transmitter is numbered WIKA-2, and the second pressure transmitter is numbered WIKA-1;

[0074] The two groups of high-pressure inlets are numbered as inlet 1 and inlet 2, and the two groups of low-pressure inlets are numbered as inlet 3 and inlet 4.

[0075] The low-pressure sample automatic injection and post-displacement workflow of the automatic injection panel in this embodiment is automatically controlled and will automatically stop if an abnormality occurs. The automatic program flow is as follows: Taking injection port 3 as an example, PCV101, PCV203, PCV205, PCV206, and PCV207 are opened, then maintained for 120 seconds, and PCV101 is closed. If the sample pressure exceeds 10 torr, PCV206 is closed and the sample is analyzed through secondary decompression injection. If the sample pressure is below 10 torr, the sample is directly injected and analyzed.

[0076] After analysis, initially close all valves, including the sample source valve. Open PCV101 and PCV203, pump down to a WIKA-1 reading of -14.7 psi, and hold for 30 seconds. After 30 seconds, close PCV101 and open PCV104 until the WIKA-1 reading is 0 psi. Repeat this cycle 10 times. To protect the low-pressure sample inlet, perform the tenth pumpdown without introducing air.

[0077] It should be noted that the present invention is an automatic sampling system for mass spectrometers in the electronic specialty gas industry, which establishes automatic functional modules such as helium detection, displacement, sampling, and purging, realizing one-button operation. The system has been tested for sampling control under different pressure conditions, and can simultaneously meet the requirements of stable sampling of ultra-high-pressure and ultra-low-pressure electronic specialty gas mass spectrometers at 1-10 torr pressure, and stable analysis at mass spectrometer cavity pressures of 3E-6 to 8E-5 torr.

[0078] The automatic sampling system for mass spectrometers in the electronic specialty gas industry of the present invention realizes stable output control of high-pressure, ultra-low-pressure samples, purge gas and other gases of different pressures, ensures sample outflow stability, meets the needs of high-end mass spectrometry analysis and detection, has better use effect than traditional methods, meets people's use requirements, and is more practical.

[0079] The basic principles, main features, and advantages of the present invention are shown and described above. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions are merely illustrative of the principles of the present invention. Various changes and modifications may be made to the present invention without departing from the spirit and scope of the present invention. Such changes and modifications are intended to fall within the scope of the present invention. The scope of protection claimed in the present invention is defined by the appended claims and their equivalents.

Claims

1. An automatic sampling system for mass spectrometers in the electronic specialty gas industry, characterized in that: It includes a replacement purge air system, a sampling system, a pressure control system, a vacuum venting system and a PLC control system. The PLC control system is electrically connected to the replacement purge air system, the sampling system, the pressure control system and the vacuum venting system. The sampling system, the replacement purge air system and the vacuum venting system are all connected to the pressure control system. The displacement purge gas system is used to adjust the output pressure of the gas; The sample injection system is used to guide the high-pressure sample into the automatic sample injection system or the low-pressure sample into the automatic sample injection system; The pressure control system is used to adjust and obtain the pressure data of the gas in the automatic sampling system; The vacuum venting system is used to complete the venting, evacuation, and replacement of high and low pressure gases and the replacement and purging of the sampling pipeline; The PLC control system is used to control the operation of the entire automatic sampling system; The displacement purge air path system comprises two groups of displacement purge air paths, wherein a one-way valve, a first pressure gauge, a pressure reducing gauge and a first diaphragm valve are sequentially arranged on the displacement purge air paths; The pressure control system includes a primary pressure reducing device and a secondary pressure reducing device, both of which are connected to two sets of displacement and purge air paths; The first-stage pressure reducing device includes a pressure reducing valve and a first pressure transmitter, and the pressure reducing valve is connected to the first pressure transmitter; The secondary pressure reducing device includes a pressure controller, a second pressure transmitter and several groups of second diaphragm valves; The injection system includes two groups of high-pressure injection ports and two groups of low-pressure injection ports. A third diaphragm valve is provided on the pipelines of the two groups of high-pressure injection ports and the two groups of low-pressure injection ports. The high-pressure injection ports are connected to the pipeline between the first-level pressure reducing device and the replacement purge gas system, and the low-pressure injection ports are connected to the pipeline between the first-level pressure reducing device and the second-level pressure reducing device.

2. The automatic sampling system for mass spectrometer in the electronic specialty gas industry according to claim 1, characterized in that: The vacuum venting system includes a vacuum outlet connected to the vacuum equipment and a venting outlet connected to the tail gas treatment equipment. A fourth diaphragm valve and a second pressure gauge are provided on the pipelines of the vacuum outlet and the venting outlet.

3. The automatic sampling system for mass spectrometer in the electronic specialty gas industry according to claim 1, characterized in that: The PLC control system includes a pneumatic valve, a pressure sensor, a PLC control box and an automatic control touch screen.

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