Gas permeation measuring device and method

Abstract

The application relates to a gas permeation measuring device and method. When a sample is detected and processed, the sample is fixed by a first fixing member, a first vacuum pumping assembly is used to pump the first cavity, a second vacuum pumping assembly is used to pump the second cavity, then a gas inlet module inputs reaction gas into the first cavity, a plasma generator generates plasma, a first high-temperature heating member heats the sample at high temperature, and the gas inlet module adjusts the pressure of the input reaction gas, so that the actual working condition environment of a reactor is simulated, in-situ measurement of the reaction gas permeability under the simulated working condition is realized, and the barrier property of the material under the working condition of high temperature and high energy can be evaluated.

Description

Technical Field

[0001] This application relates to the field of gas detection technology, and in particular to a gas permeation measurement device and method. Background Technology

[0002] Trace gas permeation behavior in high-barrier systems is a physicochemical process with wide-ranging applications, and systematic and in-depth research on this behavior is of great significance in various fields such as energy conservation and environmental protection, flexible electronics, medical health, and aerospace. In the field of flexible displays, blocking the permeation of trace water vapor and oxygen can significantly improve the lifespan and reliability of display devices, and is a key technology driving the development of the flexible display industry. In the fields of hydrogen and nuclear energy, high-pressure hydrogen storage tanks need to be effectively leak-proof, and hydrogen isotopes such as deuterium and tritium in nuclear fusion reactors also need to be effectively blocked to prevent leakage. Therefore, trace gas permeation measurement systems, especially permeation measurement systems that simulate actual working conditions for corresponding application scenarios, have broad demand and application prospects.

[0003] In related technologies, high-temperature gas-phase deuterium permeation experimental systems heat the sample chamber to a temperature of 450℃–600℃, introduce deuterium gas above the sample, and maintain a high vacuum below the sample with a mass spectrometer and vacuum pump assembly. The mass spectrometer measures the amount of deuterium permeating into the sample to evaluate the material's deuterium permeation performance. However, these technologies fail to consider the impact of high-temperature, high-energy operating conditions on the material's barrier properties, and they also cannot simulate the high-temperature, high-energy operating conditions of actual stockpile sites, thus making it impossible to evaluate the material's barrier properties. Summary of the Invention

[0004] Therefore, it is necessary to overcome the shortcomings of existing technologies and provide a gas permeation measurement device and method that can evaluate the barrier performance of materials under high temperature and high energy conditions.

[0005] A gas permeation measuring device, the gas permeation measuring device comprising:

[0006] An intake module is used to provide reaction gases;

[0007] A first chamber has a first fixing member for fixing a sample and a first high-temperature heating member for heating the sample on its inner wall. The first fixing member and the sample can separate the first chamber into a first split chamber located above the first fixing member and a second split chamber located below the first fixing member. The first split chamber is connected to the air intake module and is equipped with a first plasma generator for applying high-energy particles to the surface of the sample.

[0008] A first vacuum pumping assembly is connected to the first split chamber and is used to control the vacuum level of the first split chamber.

[0009] A second vacuum pumping assembly, connected to the second split chamber, is used to control the vacuum level of the second split chamber; and

[0010] A detection component, which is connected to the second split chamber, is used to detect the permeability of the reaction gas.

[0011] In one embodiment, at least two first chambers are provided, and at least two first chambers are connected in parallel.

[0012] In one embodiment, the gas permeation measuring device further includes a second chamber and a flow guiding device located inside the second chamber. The inner wall of the second chamber is provided with a second fixing member and a second high-temperature heating member for heating the flow guiding device. The second fixing member and the flow guiding device divide the second chamber into a third split chamber located above the second fixing member and a fourth split chamber located below the second fixing member. The third split chamber is connected to the air inlet module, and the fourth split chamber is connected to the detection component. The flow guiding device is provided with an air inlet and an air outlet. The air inlet is connected to the third split chamber, and the air outlet is connected to the fourth split chamber.

[0013] In one embodiment, the gas permeation measuring device further includes a third chamber. The inner wall of the third chamber is provided with a third fixing member for fixing the sample and a third high-temperature heating member for heating the sample. The third fixing member and the installed sample can separate the third chamber into a fifth split chamber located above the third fixing member and a sixth split chamber located below the third fixing member. The fifth split chamber is connected to the gas inlet module, and the sixth split chamber is connected to the detection component. The fifth split chamber is provided with an infrared light emitting device and an infrared light receiving device. The infrared light emitting device is used to emit infrared detection light onto the sample surface, and the infrared light receiving device is used to receive the infrared detection light reflected from the sample surface.

[0014] In one embodiment, the detection assembly includes a mass spectrometer, a detection chamber, a first switch K1, and a second switch K2; the detection chamber is connected to the mass spectrometer, the detection chamber is also connected to the second split chamber, and the detection chamber is also connected to the second vacuum assembly; the first switch K1 is used to control the connection or disconnection between the detection chamber and the second split chamber, and the second switch K2 is used to control the connection or disconnection between the detection chamber and the second vacuum assembly.

[0015] In one embodiment, the air intake module includes a main pipe, a first branch pipe, and a second branch pipe; the main pipe is connected to the first branch pipe and the second branch pipe respectively, and the main pipe is also connected to the first split chamber; the first branch pipe is connected to a plurality of air intake pipes respectively, and a gas flow controller is provided on the air intake pipe; the second branch pipe is provided with a water storage container and a buffer container arranged sequentially along the airflow direction.

[0016] In one embodiment, the first vacuum pumping assembly includes a first turbomolecular pump and a first vortex pump connected sequentially along the pumping direction; and / or,

[0017] The second vacuum pumping assembly includes a second turbomolecular pump and a second vortex pump connected sequentially along the pumping direction.

[0018] In one embodiment, the first high-temperature heating element includes a high-temperature resistant heating plate; the high-temperature resistant heating plate abuts against the bottom surface of the sample, and the heating plate is provided with a plurality of vent holes.

[0019] In one embodiment, the first chamber further includes a first pressure detection device P1 and a second pressure detection device P2; the first pressure detection device P1 is disposed in the first split chamber and is used to detect the vacuum degree of the first split chamber; the second pressure detection device P2 is disposed in the second split chamber and is used to detect the vacuum degree of the second split chamber.

[0020] A gas permeation measurement method, employing the aforementioned gas permeation measurement device, includes the following steps:

[0021] Step S210: The sample is sent into the first chamber and fixed in place by the first fixing member;

[0022] Step S220: Vacuum the first split chamber using the first vacuum pumping assembly, and vacuum the second split chamber using the second vacuum pumping assembly.

[0023] Step S230: The gas inlet module inputs the reaction gas into the interior of the first split chamber, generates plasma through the plasma generator, heats the sample at high temperature through the first high-temperature heating element, and adjusts the pressure of the input reaction gas through the gas inlet module.

[0024] Step S240: Detect the permeability of the reaction gas using a detection component.

[0025] In one embodiment, the detection assembly includes a mass spectrometer, a detection chamber, a first switch K1, and a second switch K2; the detection chamber is connected to the mass spectrometer, the detection chamber is also connected to a second split chamber, and the detection chamber is also connected to a second vacuum assembly; the first switch K1 is used to control the connection or disconnection between the detection chamber and the second split chamber, and the second switch K2 is used to control the connection or disconnection between the detection chamber and the second vacuum assembly;

[0026] The step of detecting the permeability of the reaction gas using a detection component includes:

[0027] Step S241: Close the first switch K1 to accumulate the reaction gas in the second split chamber;

[0028] Step S242: After the first switch K1 is closed and held for a preset time, the first switch K1 is opened and the second switch K2 is closed, so that the reaction gas in the second split chamber enters the detection chamber and the reaction gas inside the detection chamber is detected by a mass spectrometer.

[0029] Step S243: Turn on the second switch K2, and the second vacuum assembly will work to evacuate the detection chamber and the second split chamber.

[0030] Step S244, repeat steps S241 to S243.

[0031] In one embodiment, the gas permeation measurement method further includes: step S222, after the vacuum degree of the first split chamber and the vacuum degree of the second split chamber each reach the required level, the first chamber is baked at a temperature of 150°C to 200°C for 6 to 10 hours to remove water vapor adsorbed on the inner wall of the first chamber.

[0032] The aforementioned gas permeation measurement device and method, when processing a sample, fixes the sample with a first fixing member, evacuates the first chamber using a first vacuum assembly, and evacuates the second chamber using a second vacuum assembly. Then, the gas inlet module introduces the reactive gas into the interior of the first split chamber, generates plasma through a plasma generator, heats the sample at high temperature using a first high-temperature heating element, and adjusts the pressure of the input reactive gas through the gas inlet module. This simulates the actual operating environment of a reactor (a barrier sample from a nuclear reactor such as tritium), enabling in-situ measurement of the reactive gas permeability under simulated operating conditions. This allows for the evaluation of the barrier performance of materials under high-temperature and high-energy operating conditions. Attached Figure Description

[0033] Figure 1 This is a schematic diagram of the structure of a gas permeation measuring device according to an embodiment of this application.

[0034] Figure 2 In one embodiment of this application, the intake gas in the second chamber is nitrogen and C6F. 12 Pressure data curves of the two gases over time.

[0035] 10. Intake module; 11. Main pipeline; 12. First branch pipeline; 121. Gas flow controller; 13. Second branch pipeline; 131. Water storage container; 132. Buffer container; 20. First chamber; 21. First fixing component; 22. First high-temperature heating component; 23. First split chamber; 24. Second split chamber; 25. First plasma generator; 26. First lifting mechanism; 30. First vacuum assembly; 31. First turbomolecular pump; 32. First vortex pump; 40. Second vacuum assembly; 41. Second turbomolecular pump; 42. Second vortex pump; 50. Detection assembly; 51. Mass spectrometer; 52. Detection chamber; 60. Sample; 70. Second chamber; 71. Flow guiding device; 80. Third chamber; 81. Infrared light emitting device; 82. Infrared light receiving device. Detailed Implementation

[0036] To make the above-mentioned objectives, features, and advantages of this application more apparent and understandable, the specific embodiments of this application are described in detail below with reference to the accompanying drawings. Many specific details are set forth in the following description to provide a thorough understanding of this application. However, this application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of this application. Therefore, this application is not limited to the specific embodiments disclosed below.

[0037] See Figure 1 , Figure 1A schematic diagram of a gas permeation measuring device according to an embodiment of this application is shown. The gas permeation measuring device includes: an inlet module 10, a first chamber 20, a first vacuum assembly 30, a second vacuum assembly 40, and a detection assembly 50. The inlet module 10 provides the reaction gas. The inner wall of the first chamber 20 is provided with a first fixing member 21 for fixing a sample 60 and a first high-temperature heating member 22 for heating the sample 60. The first fixing member 21 and the mounted sample 60 can separate the first chamber 20 to form a first split chamber 23 above the first fixing member 21 and a second split chamber 24 below the first fixing member 21. The first split chamber 23 is connected to the inlet module 10 and is provided with a first plasma generator 25. The first plasma generator 25 is used to apply high-energy particles to the surface of the sample 60. The first vacuum assembly 30 is connected to the first split chamber 23 and is used to control the vacuum level of the first split chamber 23. The second vacuum pumping assembly 40 is connected to the second split chamber 24 and is used to control the vacuum level of the second split chamber 24. The detection assembly 50 is connected to the second split chamber 24 and is used to detect the permeability of the reaction gas.

[0038] It should be noted that the reactant gas is, but is not limited to, a single gas, such as hydrogen, protium, deuterium, tritium, nitrogen, carbon dioxide, methane, or C6F. 12 It can also be a mixture of gases, such as a mixture of hydrogen and nitrogen.

[0039] The gas permeation measurement device described above, when testing and processing sample 60, fixes sample 60 with first fixing member 21, uses first vacuum assembly 30 to evacuate first chamber 20, and uses second vacuum assembly 40 to evacuate second chamber 70. Then, gas inlet module 10 inputs reactive gas into the interior of first split chamber 23, plasma is generated by plasma generator, first high-temperature heating element 22 heats sample 60 at high temperature, and gas inlet module 10 adjusts the pressure of input reactive gas, thereby simulating the actual working environment of a reactor (barrier sample 60 of nuclear reactors such as tritium), realizing in-situ measurement of reactive gas permeability under simulated working conditions, and can evaluate the barrier performance of materials under high temperature and high energy working conditions.

[0040] It should be noted that, in addition to simulating high-energy and high-temperature environments, the device can also simulate the application scenarios of conventional OLED encapsulation films. Specifically, by turning off the first plasma generator 25 and adjusting conditions such as temperature and water vapor pressure, different environmental conditions can be simulated, and the water vapor barrier performance of the OLED encapsulation film under different conditions, i.e., permeability, can be measured. Therefore, the gas permeation measurement device of this embodiment can also simulate the application scenarios of most barrier materials by changing the inlet pressure, inlet gas type, temperature, and whether or not a high-energy environment exists, and is not limited to barrier samples from nuclear reactors.

[0041] In one embodiment, the first plasma generator 25 stops working, and by adjusting the temperature of the first high-temperature heating element 22 and adjusting the inlet pressure, the actual working conditions under different temperature and humidity conditions are simulated (such as flexible thin film samples 60 commonly used in food, flexible displays, etc.), thereby realizing in-situ measurement of the permeability of various reactive gases under simulated working conditions.

[0042] Please see Figure 1 In one embodiment, at least two first chambers 20 are provided, and the at least two first chambers 20 are connected in parallel. Thus, one first chamber 20 is equivalent to one permeation measurement channel, and the at least two first chambers 20 connected in parallel are at least two permeation measurement channels, realizing dual-channel measurement, which can greatly improve the measurement efficiency of sample 60, and at the same time, differential measurement can be used to realize quantitative evaluation of the modification of sample 60.

[0043] It should be noted that the steps for differential measurement and dual-channel measurement are the same; the main difference lies in data processing. Dual-channel measurement focuses on measuring two samples 60 simultaneously, without seeking correlation between the samples 60 or the data. Differential measurement, on the other hand, targets two related samples 60, such as one sample 60 being a substrate sample 60, and the other sample 60 having a barrier film coated on the substrate sample 60 as the substrate material. Differential measurement measures the permeation signals of the two channels to calculate the permeation performance parameters of the corresponding sample 60. Comparing and analyzing these parameters provides a quantitative assessment of surface modification of the sample 60, thereby guiding the development and research of new coatings and materials.

[0044] Please see Figure 1In one embodiment, the gas permeation measuring device further includes a second chamber 70 and a flow guiding device 71 located inside the second chamber 70. A second fixing member and a second high-temperature heating member for heating the flow guiding device 71 are provided on the inner wall of the second chamber 70. The second fixing member and the flow guiding device 71 divide the second chamber 70 into a third split chamber located above the second fixing member and a fourth split chamber located below the second fixing member. The third split chamber is connected to the air inlet module 10, and the fourth split chamber is connected to the detection component 50. The flow guiding device 71 has an air inlet and an air outlet; the air inlet is connected to the third split chamber, and the air outlet is connected to the fourth split chamber. Thus, the reactant gas enters the third split chamber through the air inlet module 10 and is then transported to the fourth split chamber through the flow guiding device 71, achieving the calibration function of the system signal and ensuring the accuracy of the measurement.

[0045] In one embodiment, the first vacuum pumping assembly 30 is also connected to the third split chamber for controlling the vacuum level of the third split chamber. The second vacuum pumping assembly 40 is also connected to the fourth split chamber for controlling the vacuum level of the fourth split chamber.

[0046] It should be noted that the standard conductance element (SCE) 71 is a micro-nano porous plug structure made of sintered stainless steel, with an average pore diameter of less than 1 micrometer, capable of operating at 1e 4 Under conditions below Pa pressure, a molecular flow effect is generated and a constant conductance is maintained. At this time, the gas flow rate through the SCE is only a linear function of the upper inlet pressure. Using this characteristic, users can introduce optional test gas and known flow rate gas into the target vacuum chamber and thereby calibrate the gas signal of the vacuum metering equipment.

[0047] In one embodiment, the calibration steps include:

[0048] Step S110: Heat and bake the outer wall of the entire equipment pipeline. The temperature is set to, for example, 150℃-200℃, and the baking time is set to, for example, 6 hours-10 hours. The purpose is to remove the residual gas adsorbed on the inner side of the equipment wall.

[0049] Step S120: The reaction gas to be tested is injected into the third split chamber and kept stable for a period of time. As the reaction gas flows through the SCE and the fourth split chamber into the detection chamber 52 of the detection component 50 and gradually reaches a stable flow state, the gas pressure in the detection chamber 52 will also gradually reach a stable value. The detection component 50, specifically, such as the mass spectrometer 51, will record the inlet pressure of the reaction gas entering the third split chamber and the detection pressure in the detection chamber 52 at this time.

[0050] Please refer to Figure 2 , Figure 2The intake gases are shown to be nitrogen and C6F. 12 The pressure curves of the two gases over time show that the final shape is a "stepped shape".

[0051] Step S130: Since the conductance of the SCE is known, the actual gas flow rate through the SCE can be obtained by multiplying the upper inlet pressure and the conductance value. This flow rate signal is used to calibrate the obtained detection chamber pressure signal, which is the QMS (mass spectrometer) signal.

[0052] Step S140: Adjust the intake chamber pressure, and repeat steps S120 to S130 until the QMS full-range data is overwritten (generally 1e). -13 torr~1e -7 (torr), and finally the calibration curve is obtained.

[0053] Step S150: Change the data monitoring mode to dynamic detection using time integration. Similarly, use SCE to perform dynamic method signal calibration. The process is the same as the static method. Finally, obtain the dynamic method calibration curve.

[0054] Please see Figure 1 In one embodiment, the gas permeation measurement device further includes a third chamber 80. The inner wall of the third chamber 80 is provided with a third fixing member for fixing the sample 60 and a third high-temperature heating member for heating the sample 60. The third fixing member and the mounted sample 60 can divide the third chamber 80 into a fifth separate chamber located above the third fixing member and a sixth separate chamber located below the third fixing member. The fifth separate chamber is connected to the gas inlet module 10, and the sixth separate chamber is connected to the detection component 50. The fifth separate chamber is provided with an infrared light emitting device 81 and an infrared light receiving device 82. The infrared light emitting device 81 emits infrared detection light onto the surface of the sample 60, and the infrared light receiving device 82 receives the infrared detection light reflected from the surface of the sample 60. Thus, during the permeation of the reactive gas, the permeation behavior between the reactive gas and the surface of the sample 60 can be characterized in real time and in situ based on the optical signal received by the infrared light receiving device 82, which helps to understand the surface mechanism and principle of hydrogen permeation in materials.

[0055] In one embodiment, the first vacuum pumping assembly 30 is also connected to the fifth split chamber for controlling the vacuum level of the fifth split chamber, and the second vacuum pumping assembly 40 is also connected to the sixth split chamber for controlling the vacuum level of the sixth split chamber.

[0056] Please see Figure 1In one embodiment, the detection assembly 50 includes a mass spectrometer 51, a detection chamber 52, a first switch K1, and a second switch K2. The detection chamber 52 is connected to the mass spectrometer 51, a second split chamber 24, and a second vacuum assembly 40. The first switch K1 controls the connection or disconnection between the detection chamber 52 and the second split chamber 24, and the second switch K2 controls the connection or disconnection between the detection chamber 52 and the second vacuum assembly 40. Thus, when it is necessary to evacuate the second split chamber 24, both the first switch K1 and the second switch K2 are turned on, and the second vacuum assembly 40 provides negative pressure, allowing the gas inside the second split chamber 24 to enter the detection chamber 52 and then be discharged outward through the second vacuum assembly 40; when the vacuum level inside the second split chamber 24 meets the requirements, the first switch K1 and the second switch K2 are turned off, and the second vacuum assembly 40 stops working.

[0057] In addition, both dynamic and static detection methods can be used. Dynamic detection mainly involves setting appropriate time intervals and controlling the opening and closing of the circulating valves to achieve a dynamic cycle of "vacuuming-accumulation-detection." Static detection, on the other hand, involves keeping the first switch K1 and the second switch K2 open throughout the measurement process. The reactant gas inside the second compartment 24 enters the detection chamber 52, where it is detected by the mass spectrometer 51 and subsequently removed by the vacuum pump unit.

[0058] Optionally, the mass spectrometer 51 is specifically, for example, a quadrupole mass spectrometer 51. The detection of the permeation signal is achieved using the quadrupole mass spectrometer 51, which can detect elements within a certain mass number range. This allows the gas permeation measurement device of this embodiment to not only measure hydrogen isotopes but also to perform permeation measurements under simulated operating conditions for other types of gases, thereby broadening the applicability of this device.

[0059] In one embodiment, when the second chamber 70 is provided, the first switch K1 can also control the connection or disconnection between the detection chamber 52 and the fourth split chamber. When the third chamber 80 is provided, the first switch K1 can also control the connection or disconnection between the detection chamber 52 and the sixth split chamber.

[0060] Optionally, the first switching element K1 may be, for example, a three-position four-way control valve, a four-position five-way control valve, etc., which can connect the air outlet pipes of the second split chamber 24, the fourth split chamber, and the sixth split chamber to the air inlet pipe of the detection chamber 52.

[0061] Please see Figure 1In one embodiment, the air intake module 10 includes a main pipe 11, a first branch pipe 12, and a second branch pipe 13. The main pipe 11 is connected to the first branch pipe 12 and the second branch pipe 13, and is also connected to the first split chamber 23. The first branch pipe 12 is connected to multiple air intake pipes, and a gas flow controller 121 is installed on the air intake pipes. The second branch pipe 13 is provided with a water storage container 131 and a buffer container 132 arranged sequentially along the airflow direction.

[0062] Please see Figure 1 In one embodiment, the intake module 10 is provided with a metering valve F, which is used to control the opening degree of the valve body to regulate the gas flow rate. Specifically, the metering valve F is located on the main pipeline 11.

[0063] Optionally, at least one of the first branch pipe 12, the second branch pipe 13, and the main pipe 11 is provided with at least one third switch K3.

[0064] Optionally, main road 11 is also connected to the third and fifth sub-rooms respectively.

[0065] Of course, as some alternative solutions, the first branch pipe 12 or the second branch pipe 13 in the above embodiments can be omitted.

[0066] Please see Figure 1 In one embodiment, the first vacuum pumping assembly 30 includes a first turbomolecular pump 31 and a first vortex pump 32 connected sequentially along the pumping direction. Furthermore, the second vacuum pumping assembly 40 includes a second turbomolecular pump 41 and a second vortex pump 42 connected sequentially along the pumping direction. Thus, the turbomolecular pump and the vortex pump work together to achieve an ultra-high vacuum level in the corresponding split chamber, ensuring that the vacuum level meets the requirements.

[0067] Please see Figure 1 In one embodiment, the first high-temperature heating element 22 includes a high-temperature resistant heating plate. The high-temperature resistant heating plate abuts against the bottom surface of the sample 60, and the heating plate is provided with multiple vent holes. Specifically, the high-temperature resistant heating plate includes, but is not limited to, a ceramic heating plate. Thus, the high-temperature resistant heating plate can heat the sample 60 to a preset temperature range, such as 900°C, thereby enabling testing of the barrier properties of materials under high-temperature operating conditions. Furthermore, the reactive gas inside the first split chamber 23 can diffuse into the second split chamber 24 through the vent holes on the heating plate, without obstructing the measurement of the permeability of the reactive gas.

[0068] Please see Figure 1In one embodiment, the first chamber 20 further includes a first lifting mechanism 26 connected to the first high-temperature heating element 22. The first lifting mechanism 26 and the first high-temperature heating element 22 are arranged inside the second split chamber 24. The first lifting mechanism 26 is used to drive the first high-temperature heating element 22 to move up and down. Thus, when heating of the sample 60 is not required, the first lifting mechanism 26 drives the first high-temperature heating element 22 to lower its height. When heating of the sample 60 is required, the first lifting mechanism 26 drives the first high-temperature heating element 22 to rise and abut against the bottom surface of the sample 60.

[0069] In one embodiment, the first chamber 20 further includes a first pressure detection device P1 and a second pressure detection device P2. Furthermore, the first pressure detection device P1 is disposed in the first split chamber 23 and is used to detect the vacuum level of the first split chamber 23; the second pressure detection device P2 is disposed in the second split chamber 24 and is used to detect the vacuum level of the second split chamber 24.

[0070] Specifically, the first pressure sensing device P1 is, for example, a full-scale vacuum gauge. Furthermore, the second pressure sensing device P2 is, for example, an ionization vacuum gauge.

[0071] Please see Figure 1 In one embodiment, a gas permeation measurement method employs the gas permeation measurement device of any of the above embodiments, and includes the following steps:

[0072] Step S210: Send the sample 60 into the first chamber 20 and fix the sample 60 in place by the first fixing member 21;

[0073] Step S220: Vacuum the first split chamber 23 using the first vacuum assembly 30, and vacuum the second split chamber 24 using the second vacuum assembly 40.

[0074] Specifically, the first vacuum pumping assembly 30 achieves a high vacuum level of -6 Torr for the first split chamber 23; in addition, the second vacuum pumping assembly 40 achieves an ultra-high vacuum level of less than -8 Torr for the second split chamber 24.

[0075] In step S230, the gas inlet module 10 inputs the reaction gas into the interior of the first split chamber 23, generates plasma through the plasma generator, and heats the sample 60 at high temperature through the first high-temperature heating element 22, and adjusts the pressure of the input reaction gas through the gas inlet module 10.

[0076] Specifically, a permeation gas (such as deuterium) is introduced, and after the gas flow rate stabilizes, the plasma energy is set, and a plasma generator is used to generate plasma that acts on the surface of the measurement sample 60. The energy of the plasma and the pressure of the chamber in which the plasma is located are measured and observed in real time.

[0077] Optionally, the first high-temperature heating element 22 heats the sample 60 to 850°C to 950°C, specifically for example, 880°C, 890°C, 900°C, 910°C, etc.

[0078] Step S240: The permeability of the reaction gas is detected by the detection component 50.

[0079] The gas permeation measurement method described above can simulate the actual operating environment of a reactor (barrier sample 60 of a nuclear reactor such as a tritium barrier), realize in-situ measurement of the permeability of reactive gases under simulated operating conditions, and evaluate the barrier performance of materials under high temperature and high energy operating conditions.

[0080] Please see Figure 1 In some embodiments, the permeation signal is directly measured using a mass spectrometer 51 (referred to as the static method) or enriched and amplified using a dynamic accumulation method (described in detail later), and finally the gas permeation signal under simulated operating conditions is measured using a mass spectrometer 51. In this embodiment, the detection method of the dynamic accumulation method will be specifically described.

[0081] Please see Figure 1 In one embodiment, the step of detecting the permeability of the reactant gas using the detection component 50 includes:

[0082] Step S241: Close the first switch K1 and accumulate the reaction gas in the second split chamber 24;

[0083] Step S242: After the first switch K1 is closed and held for a preset time, the first switch K1 is opened and the second switch K2 is closed, so that the reaction gas in the second split chamber 24 enters the detection chamber 52, and the reaction gas inside the detection chamber 52 is detected by the mass spectrometer 51.

[0084] Step S243: Open the second switch K2, and the second vacuum assembly 40 will work to evacuate the detection chamber 52 and the second split chamber 24.

[0085] Step S244, repeat steps S241 to S243.

[0086] Thus, the dynamic accumulation method achieves signal enrichment and amplification. By utilizing the dynamic accumulation method, the weak signals from penetration can be enriched and amplified, improving detection sensitivity and broadening the detection limit.

[0087] In one embodiment, the gas permeation measurement method further includes: step S222, after the vacuum degree of the first split chamber 23 and the vacuum degree of the second split chamber 24 each reach the required level, the first chamber 20 is baked at a temperature of 150°C to 200°C for a time of 6 to 10 hours to remove water vapor adsorbed on the inner wall of the first chamber 20.

[0088] In the description of this application, it should be understood that if terms such as "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" appear, these terms indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application.

[0089] Furthermore, where the terms "first" and "second" appear, these terms are for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined with "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this application, where the term "multiple" appears, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0090] In this application, unless otherwise expressly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise expressly limited. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0091] In this application, unless otherwise expressly specified and limited, the use of descriptions such as "above" or "below" the second feature indicates that the first and second features are in direct contact or indirect contact via an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. Similarly, "below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0092] It should be noted that if an element is referred to as being "fixed to" or "set on" another element, it can be directly on the other element or there may be an intervening element. If an element is considered to be "connected to" another element, it can be directly connected to the other element or there may be an intervening element. If so, the terms "vertical," "horizontal," "upper," "lower," "left," "right," and similar expressions used in this application are for illustrative purposes only and do not represent the only possible implementation.

[0093] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0094] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this patent application should be determined by the appended claims.

Claims

1. A gas permeation measuring device, characterized in that, The gas permeation measurement device includes: An intake module is used to provide reaction gases; A first chamber has a first fixing member for fixing a sample and a first high-temperature heating member for heating the sample on its inner wall. The first fixing member and the sample can separate the first chamber into a first split chamber located above the first fixing member and a second split chamber located below the first fixing member. The first split chamber is connected to the air intake module and is equipped with a first plasma generator for applying high-energy particles to the surface of the sample. A first vacuum pumping assembly is connected to the first split chamber and is used to control the vacuum level of the first split chamber. A second vacuum pumping assembly, connected to the second split chamber, is used to control the vacuum level of the second split chamber; and A detection component, which is connected to the second split chamber, is used to detect the permeability of the reaction gas; The detection component is configured to perform a dynamic accumulation method, which includes periodically closing and opening the connection between the second split chamber and the detection chamber to accumulate the reaction gas in the second split chamber, and then instantaneously releasing the accumulated gas into the detection chamber for detection, thereby achieving enrichment and amplification of weak permeation signals.

2. The gas permeation measuring device according to claim 1, characterized in that, The first chamber is configured as at least two, and the at least two first chambers are connected in parallel.

3. The gas permeation measuring device according to claim 1, characterized in that, The gas permeation measuring device further includes a second chamber and a flow guiding device located inside the second chamber. The inner wall of the second chamber is provided with a second fixing member and a second high-temperature heating member for heating the flow guiding device. The second fixing member and the flow guiding device divide the second chamber into a third split chamber located above the second fixing member and a fourth split chamber located below the second fixing member. The third split chamber is connected to the air inlet module, and the fourth split chamber is connected to the detection component. The flow guiding device is provided with an air inlet and an air outlet. The air inlet is connected to the third split chamber, and the air outlet is connected to the fourth split chamber.

4. The gas permeation measuring device according to claim 1, characterized in that, The gas permeation measurement device further includes a third chamber. The inner wall of the third chamber is provided with a third fixing member for fixing the sample and a third high-temperature heating member for heating the sample. The third fixing member and the installed sample can separate the third chamber into a fifth split chamber located above the third fixing member and a sixth split chamber located below the third fixing member. The fifth split chamber is connected to the gas inlet module, and the sixth split chamber is connected to the detection component. The fifth split chamber is provided with an infrared light emitting device and an infrared light receiving device. The infrared light emitting device is used to emit infrared detection light onto the sample surface, and the infrared light receiving device is used to receive the infrared detection light reflected from the sample surface.

5. The gas permeation measuring device according to claim 1, characterized in that, The detection assembly includes a mass spectrometer, a detection chamber, a first switch K1, and a second switch K2; the detection chamber is connected to the mass spectrometer, the detection chamber is also connected to the second split chamber, and the detection chamber is also connected to the second vacuum assembly; the first switch K1 is used to control the connection or disconnection between the detection chamber and the second split chamber, and the second switch K2 is used to control the connection or disconnection between the detection chamber and the second vacuum assembly.

6. The gas permeation measuring device according to claim 1, characterized in that, The air intake module includes a main pipe, a first branch pipe, and a second branch pipe; the main pipe is connected to the first branch pipe and the second branch pipe respectively, and the main pipe is also connected to the first split chamber; the first branch pipe is connected to multiple air intake pipes respectively, and a gas flow controller is provided on the air intake pipe; the second branch pipe is provided with a water storage container and a buffer container arranged sequentially along the airflow direction.

7. The gas permeation measuring device according to claim 1, characterized in that, The first vacuum pumping assembly includes a first turbomolecular pump and a first vortex pump connected sequentially along the pumping direction; and / or, The second vacuum pumping assembly includes a second turbomolecular pump and a second vortex pump connected sequentially along the pumping direction.

8. The gas permeation measuring device according to claim 1, characterized in that, The first high-temperature heating element includes a high-temperature resistant heating plate; the high-temperature resistant heating plate is in contact with the bottom surface of the sample, and the heating plate is provided with multiple vent holes.

9. The gas permeation measuring device according to any one of claims 1 to 8, characterized in that, The first chamber further includes a first pressure detection device P1 and a second pressure detection device P2; the first pressure detection device P1 is disposed in the first split chamber and is used to detect the vacuum degree of the first split chamber; The second pressure detection device P2 is disposed in the second split chamber and is used to detect the vacuum degree of the second split chamber.

10. A method for measuring gas permeation, characterized in that, The gas permeation measuring device as described in any one of claims 1 to 9 includes the following steps: Step S210: The sample is sent into the first chamber and fixed in place by the first fixing member; Step S220: Vacuum the first split chamber using the first vacuum pumping assembly, and vacuum the second split chamber using the second vacuum pumping assembly. Step S230: The gas inlet module inputs the reaction gas into the interior of the first split chamber, generates plasma through the plasma generator, heats the sample at high temperature through the first high-temperature heating element, and adjusts the pressure of the input reaction gas through the gas inlet module. Step S240: Detect the permeability of the reaction gas using a detection component.

11. The gas permeation measurement method according to claim 10, characterized in that, The detection assembly includes a mass spectrometer, a detection chamber, a first switch K1, and a second switch K2; the detection chamber is connected to the mass spectrometer, the detection chamber is also connected to the second split chamber, and the detection chamber is also connected to the second vacuum assembly; the first switch K1 is used to control the connection or disconnection between the detection chamber and the second split chamber, and the second switch K2 is used to control the connection or disconnection between the detection chamber and the second vacuum assembly; The step of detecting the permeability of the reaction gas using a detection component includes: Step S241: Close the first switch K1 to accumulate the reaction gas in the second split chamber; Step S242: After the first switch K1 is closed and held for a preset time, the first switch K1 is opened and the second switch K2 is closed, so that the reaction gas in the second split chamber enters the detection chamber and the reaction gas inside the detection chamber is detected by a mass spectrometer. Step S243: Turn on the second switch K2, and the second vacuum assembly will work to evacuate the detection chamber and the second split chamber. Step S244, repeat steps S241 to S243.

12. The gas permeation measurement method according to claim 10, characterized in that, The gas permeation measurement method further includes step S222: after the vacuum degree of the first split chamber and the vacuum degree of the second split chamber each reach the required level, the first chamber is baked at a temperature of 150°C to 200°C for 6 to 10 hours to remove water vapor adsorbed on the inner wall of the first chamber.

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