Testing device and testing method for hydrogen isotope permeation parameters of materials applied to fusion reactors

Abstract

The application discloses a testing device and testing method for hydrogen isotope permeation parameters of fusion reactor application materials, relates to material testing technology in the hydrogen field, and belongs to the field of material testing technology in the hydrogen field. The testing device for hydrogen isotope permeation parameters of fusion reactor application materials comprises the following: a membrane sample is installed in a membrane testing cavity to divide the membrane testing cavity into a gas inlet sub-cavity and a permeation sub-cavity; a gas inlet tank is selectively communicated with the gas inlet sub-cavity to supply testing gas; a collecting tank is selectively communicated with the permeation sub-cavity to collect outflowing gas; a vacuum pumping structure is used for pumping the gas inlet sub-cavity and the permeation sub-cavity; a heating structure is used for heating the gas inlet sub-cavity and the permeation sub-cavity; a high-resolution mass spectrometer is selectively communicated with the permeation sub-cavity, and gas selectively flows into the high-resolution mass spectrometer. The testing device for hydrogen isotope permeation parameters of fusion reactor application materials can control the gas pressure and temperature in the two sub-cavities respectively, thereby accurately determining the hydrogen isotope permeation parameters of the materials, and the precision is high, and the data resolution is excellent.

Description

Technical Field

[0001] This invention relates to materials testing technology in the field of hydrogen, and more particularly to a testing device and method for testing hydrogen isotope permeation parameters of materials used in fusion reactors. Background Technology

[0002] The separation and purification of hydrogen isotopes are of great significance in the field of nuclear fusion energy. Accurately testing the permeation parameters of various materials in fusion reactor applications is a key technical requirement in the development of fusion engineering systems. These parameters include the hydrogen isotope separation factor, diffusion coefficient, permeation coefficient, and pressure index. In related technologies, experimental setups built by research institutions based on their own conditions typically consist of a high-pressure hydrogen isotope supply system, a vacuum chamber, and a residual gas analyzer. However, these setups lack precise analysis and dynamic control of mixed isotope components, making it impossible to directly derive accurate isotope separation factors. Commercial quadrupole mass spectrometers exhibit varying sensitivity in quantifying H2, HD, and D2 mass spectral peaks, requiring calibration. Device schemes for testing hydrogen-helium separation materials are primarily designed for hydrogen-helium separation scenarios. Summary of the Invention

[0003] This invention aims to at least solve one of the technical problems existing in the prior art. To this end, this invention proposes a testing device for hydrogen isotope permeation parameters of materials used in fusion reactors. The device can control the gas pressure and temperature in two sub-cavities separately, thereby accurately measuring the hydrogen isotope permeation parameters of the material, including the measurement of hydrogen isotope separation factor, diffusion coefficient, permeation coefficient, and pressure index, with high accuracy and excellent data resolution.

[0004] A testing device for hydrogen isotope permeation parameters of fusion reactor application materials according to an embodiment of the present invention includes: a membrane testing chamber, wherein a membrane sample is installed in the membrane testing chamber, and the membrane sample divides the inner cavity of the membrane testing chamber into an inlet sub-cavity and a permeation sub-cavity; an inlet tank and a collection tank, wherein the inlet tank is selectively connected to the inlet sub-cavity to supply test gas to the inlet sub-cavity, and the collection tank is selectively connected to the permeation sub-cavity to collect gas flowing out of the permeation sub-cavity; a vacuuming structure and a heating structure, wherein the vacuuming structure is used to evacuate the inlet sub-cavity and the permeation sub-cavity, and the heating structure is used to heat the inlet sub-cavity and the permeation sub-cavity; and a high-resolution mass spectrometer, wherein the high-resolution mass spectrometer is selectively connected to the permeation sub-cavity, and the gas in the permeation sub-cavity selectively flows into the high-resolution mass spectrometer.

[0005] The device for testing hydrogen isotope permeation parameters of fusion reactor materials according to embodiments of the present invention divides the inner cavity of the membrane test chamber into an inlet sub-cavity and a permeation sub-cavity by using a membrane sample. The gas pressure and gas composition in each sub-cavity can be controlled independently, thereby accurately measuring the hydrogen isotope permeation parameters of the material with high precision and excellent data resolution. Furthermore, independent control of the two sub-cavities allows the same testing device to simulate various experimental conditions, measure the transport parameters of each gas component under different pressures, and enable the evaluation of competitive permeation effects and separation performance between isotopes.

[0006] According to some embodiments of the present invention, a testing device for hydrogen isotope permeation parameters of fusion reactor application materials is provided, wherein the vacuuming structure includes a mechanical pump and a molecular pump group, both of which are configured to selectively communicate with the inlet sub-cavity and the permeation sub-cavity, and the mechanical pump and the molecular pump group are configured to simultaneously evacuate the inlet sub-cavity and the permeation sub-cavity in sequence.

[0007] According to some embodiments of the present invention, a testing device for hydrogen isotope permeation parameters of fusion reactor application materials is provided, wherein the gas inlet tank and the gas inlet sub-cavity are connected by a gas inlet pipeline, and the gas inlet pipeline is provided with two first gas inlet valves, and the inlet of the mechanical pump is connected to the two first gas inlet valves.

[0008] And / or, the collection tank and the permeation chamber are connected by an outlet pipe, the outlet pipe being provided with two first outlet valves, and the inlet of the molecular pump assembly being connected to the two first outlet valves.

[0009] According to some embodiments of the present invention, a testing device for hydrogen isotope permeation parameters of fusion reactor application materials is provided, wherein the air inlet pipeline is connected to a first pressure detector, the first pressure detector is connected between two first air inlet valves, and a first detection control valve is provided between the first pressure detector and the air inlet pipeline.

[0010] And / or, the outlet pipeline is connected to a second pressure detector, the second pressure detector is connected between the two first outlet valves, and a second detection control valve is provided between the second pressure detector and the outlet pipeline.

[0011] According to some embodiments of the present invention, a testing device for hydrogen isotope permeation parameters of fusion reactor application materials is provided, wherein an intermediate pipeline is connected between the inlet pipeline and the outlet pipeline, and an intermediate control valve is provided in the intermediate pipeline.

[0012] Specifically, when the mechanical pump is connected to the inlet sub-cavity through the inlet pipe, it is connected to the permeate sub-cavity through the intermediate pipe and the outlet pipe. When the molecular pump assembly is connected to the permeate sub-cavity through the outlet pipe, it is connected to the inlet sub-cavity through the intermediate pipe and the inlet pipe.

[0013] According to some embodiments of the present invention, a testing device for hydrogen isotope permeation parameters of fusion reactor application materials is provided, wherein the high-resolution mass spectrometer is connected to the gas outlet pipeline through a detection pipeline, and a detection control valve is provided in the detection pipeline.

[0014] According to some embodiments of the present invention, a testing device for hydrogen isotope permeation parameters of fusion reactor application materials is provided, wherein there are multiple gas inlet tanks, and the multiple gas inlet tanks are configured to be selectively connected to the gas inlet sub-cavity, and at least two of the gas inlet tanks have different gas compositions.

[0015] This invention also proposes a method for testing the hydrogen isotope permeation parameters of materials used in fusion reactors.

[0016] The method for testing hydrogen isotope permeation parameters of fusion reactor application materials according to embodiments of the present invention employs the testing apparatus for hydrogen isotope permeation parameters of fusion reactor application materials described in any one of the above claims, and the testing method includes:

[0017] The membrane sample is installed in the membrane test chamber, and the inner cavity of the membrane test chamber is divided into an inlet sub-cavity and a permeate sub-cavity.

[0018] The air inlet chamber and the permeation chamber are evacuated.

[0019] The air inlet chamber and the permeation chamber are heated to the target temperature;

[0020] Test gas is introduced into the air inlet sub-cavity, and the air pressure in the air inlet sub-cavity is maintained at a set pressure value;

[0021] The permeate gas within the permeate chamber is sampled and analyzed.

[0022] According to some embodiments of the present invention, a method for testing hydrogen isotope permeation parameters of fusion reactor application materials, wherein evacuating the inlet sub-cavity and the permeation sub-cavity includes:

[0023] First, a vacuum is created in the air inlet chamber and the permeation chamber using a mechanical pump;

[0024] Then, a secondary vacuum is applied to the inlet sub-cavity and the permeate sub-cavity using a molecular pump assembly.

[0025] The method for testing hydrogen isotope permeation parameters of fusion reactor application materials according to some embodiments of the present invention further includes:

[0026] After evacuating the air intake sub-cavity and the permeation sub-cavity, the air intake sub-cavity is purged of gas and leaks are detected.

[0027] According to some embodiments of the present invention, a method for testing hydrogen isotope permeation parameters of fusion reactor application materials, wherein the gas purging of the inlet sub-cavity includes:

[0028] High-purity inert gas is introduced into the air inlet chamber to flush it, and then the vacuum is re-evacuated. This process is repeated several times to remove any residual adsorbed gas from the pipeline and the chamber.

[0029] According to some embodiments of the present invention, a method for testing hydrogen isotope permeation parameters of fusion reactor application materials, wherein leak detection of the inlet sub-cavity includes:

[0030] A high-purity inert gas at a certain pressure is introduced into the air inlet chamber;

[0031] Mass spectrometry was used to detect the gas in the permeation chamber.

[0032] If no significant signal of the mass-to-charge ratio of the high-purity inert gas is detected in the gas from the permeation sub-cavity, it is determined that there is no leakage in the inlet sub-cavity;

[0033] Furthermore, when a significant signal of the mass-to-charge ratio of the high-purity inert gas is detected from the gas in the permeation sub-cavity, it is determined that the inlet sub-cavity is leaking.

[0034] According to some embodiments of the present invention, a method for testing hydrogen isotope permeation parameters of fusion reactor application materials, wherein installing the membrane sample into the membrane testing chamber includes:

[0035] The membrane sample is fixed to the membrane test chamber using a VCR connector or flange, and the inlet chamber and the permeate chamber are sealed and isolated.

[0036] The testing device and method for the hydrogen isotope permeation parameters of the fusion reactor application materials have the same advantages as the existing technology, and will not be repeated here.

[0037] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0038] The above and / or additional aspects and advantages of the present invention will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which:

[0039] Figure 1 This is a schematic diagram of the structure of the testing device for hydrogen isotope permeation parameters of fusion reactor application materials according to an embodiment of the present invention;

[0040] Figure 2 This is a flowchart illustrating the method for testing hydrogen isotope permeation parameters of fusion reactor application materials according to an embodiment of the present invention. Figure 1 ;

[0041] Figure 3 This is a schematic diagram of the process of evacuating the air inlet chamber and the permeation chamber according to an embodiment of the present invention;

[0042] Figure 4 This is a flowchart illustrating the method for testing hydrogen isotope permeation parameters of fusion reactor application materials according to an embodiment of the present invention. Figure 2 ;

[0043] Figure 5 This is a schematic diagram of the process for gas removal from the intake chamber according to an embodiment of the present invention;

[0044] Figure 6 This is a schematic flowchart of the intake chamber leakage detection process according to an embodiment of the present invention;

[0045] Figure 7 This is a schematic diagram illustrating the process of installing a membrane sample into a membrane testing chamber according to an embodiment of the present invention.

[0046] Figure label:

[0047] A testing device 100 for hydrogen isotope permeation parameters of materials used in fusion reactors.

[0048] Membrane testing chamber 1, membrane sample 11, inlet sub-chamber 12, permeate sub-chamber 13

[0049] Intake tank 2, Collection tank 3

[0050] Mechanical pump 41, molecular pump assembly 42,

[0051] Heating structure 5,

[0052] High-resolution mass spectrometer 6, detection tubing 61, detection control valve 62,

[0053] Intake pipe 7, first intake valve 71, first pressure detector 72, first detection control valve 73

[0054] Air outlet line 8, first air outlet valve 81, second pressure detector 82, second detection control valve 83.

[0055] Intermediate pipeline 9, intermediate control valve 91. Detailed Implementation

[0056] Embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0057] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential," etc., indicating orientation or positional relationships, are based on the orientation or positional relationships shown in the accompanying drawings and are only for the convenience of describing the invention 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 the invention. Furthermore, features defined with "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0058] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; 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; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0059] The following is for reference. Figure 1 The apparatus 100 described in this embodiment of the invention is a test device for hydrogen isotope permeation parameters of fusion reactor application materials. It can control the gas pressure and temperature in two sub-cavities respectively, thereby accurately measuring the hydrogen isotope permeation parameters of the materials, including the measurement of hydrogen isotope separation factor, diffusion coefficient, permeation coefficient and pressure index, with high accuracy and excellent data resolution.

[0060] like Figure 1 As shown, the testing device 100 for hydrogen isotope permeation parameters of fusion reactor application materials according to an embodiment of the present invention includes: a membrane testing chamber 1, an inlet tank 2, a collection tank 3, a vacuum structure, a heating structure 5, and a high-resolution mass spectrometer 6.

[0061] A membrane sample 11 is installed inside the membrane testing chamber 1. This means that the hydrogen isotope permeation parameter of the membrane sample 11 can be measured within the membrane testing chamber 1. The membrane sample 11 can be a palladium membrane or a membrane made of other materials. The membrane sample 11 divides the inner cavity of the membrane testing chamber 1 into an inlet sub-cavity 12 and a permeation sub-cavity 13. The inlet sub-cavity 12 holds the gas before testing, while the permeation sub-cavity 13 holds the gas after testing. During actual testing, gas is introduced into the inlet sub-cavity 12. The gas entering the inlet sub-cavity 12 contacts the membrane sample 11 and permeates through the membrane sample 11 into the permeation sub-cavity 13, which is opposite to the inlet sub-cavity 12. Therefore, by analyzing the composition of the gas in the two sub-cavities, and combining this with test data such as gas pressure, and performing calculations, the hydrogen isotope permeation parameter of the material can be determined. The connection between the membrane sample 11 and the membrane test chamber 1 has good sealing performance. That is, no tiny gaps that allow gas to pass through will be generated at the contact position between the edge of the membrane sample 11 and the membrane test chamber 1. In this way, gas will not enter the permeate chamber 13 from the inlet chamber 12 through the contact gap, thereby avoiding any impact on the test results. Moreover, the membrane test chamber 1 can withstand a large range of temperature and pressure differences, such as operating safely within a temperature range of room temperature to 723K and a pressure difference range of vacuum to 0.3MPa, so as to realize the testing of hydrogen isotope permeation parameters of the membrane sample 11.

[0062] The membrane sample 11 can be mounted on the membrane test chamber 1 using a sealing clamp, and can be fixed to the sealing clamp using a VCR connector or flange connection. A sealing ring can be installed at the gap between the membrane sample 11 and the membrane test chamber 1 to prevent gas from entering the permeate chamber 13 from the inlet chamber 12 or vice versa. This ensures a sealed isolation between the two chambers, guaranteeing the accuracy of the test results.

[0063] The inlet tank 2 is the gas storage location before the test begins, and the collection tank 3 collects the gas after the test for analysis of its composition. The inlet tank 2 is selectively connected to the inlet sub-chamber 12 to supply test gas to it. That is, when gas needs to be supplied to the inlet sub-chamber 12, the inlet tank 2 can be connected to it to input the test gas; when gas is not needed, the inlet tank 2 can be disconnected. Similarly, the collection tank 3 is selectively connected to the permeation sub-chamber 13 to collect the gas flowing out of it. That is, when gas needs to be collected from the permeation sub-chamber 13, the collection tank 3 can be connected to it, allowing the permeation sub-chamber 13 to discharge its internal gas into the collection tank 3; when gas is not needed, the collection tank 3 can be disconnected.

[0064] The gas inlet tank 2 can be set as one or multiple. When multiple gas inlet tanks 2 are set, multiple gas inlet tanks 2 can store different hydrogen isotope gases and mixed gases, thereby enabling the testing of membrane samples 11 under different conditions.

[0065] The vacuum structure is used to evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13. The vacuum structure can be connected to the inlet sub-cavity 12 and the permeation sub-cavity 13 respectively. Thus, the vacuum structure can evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13 respectively, so that there is no participating gas or very little participating gas in the membrane test chamber 1 before the test starts. This reduces or avoids the influence of participating gas on the test results and ensures the accuracy of the test results of the hydrogen isotope permeation parameters of the material.

[0066] Furthermore, the heating structure 5 is used to heat the inlet sub-cavity 12 and the permeation sub-cavity 13. Specifically, the heating structure 5 can cover the membrane test chamber 1 to heat the inlet sub-cavity 12 and the permeation sub-cavity 13, thereby simulating the working environment temperature of the membrane sample 11. For example, the temperature in the two sub-cavities can be heated to a temperature range of 573-723K, thereby obtaining the permeation parameters of hydrogen isotopes of the membrane sample 11 during actual operation. A K-type thermocouple or other temperature sensor can be arranged near the membrane sample 11. The K-type thermocouple can monitor the surface temperature of the membrane sample 11 in real time to transmit the temperature information to the control unit. The control unit can further control the temperature controller to control the surface temperature of the membrane sample 11, thereby keeping the temperature of the membrane sample 11 constant and improving the accuracy of the test results. Before starting the test, the membrane test chamber 1 can be slowly heated by the heating structure 5. For example, controlling the heating temperature within the range of 50-100℃ can accelerate the detachment of gas adhering to the inner wall of the membrane test chamber 1, thereby speeding up the acquisition of a vacuum.

[0067] The high-resolution mass spectrometer 6 is selectively connected to the permeation chamber 13, allowing gas from the permeation chamber 13 to selectively flow into the high-resolution mass spectrometer 6. In other words, when the high-resolution mass spectrometer 6 is connected to the permeation chamber 13, the permeation chamber 13 can deliver gas to the high-resolution mass spectrometer 6, enabling the high-resolution mass spectrometer 6 to accurately measure the hydrogen isotope composition of the gas within the permeation chamber 13. When it is not necessary to deliver gas from the permeation chamber 13 to the high-resolution mass spectrometer 6, the high-resolution mass spectrometer 6 can be disconnected from the permeation chamber 13. Therefore, the high-resolution mass spectrometer 6 can be flexibly connected to or disconnected from the permeation chamber 13.

[0068] The fusion reactor application material hydrogen isotope permeation parameter testing device 100 according to an embodiment of the present invention divides the inner cavity of the membrane testing chamber 1 into an inlet sub-cavity 12 and a permeation sub-cavity 13 by using a membrane sample 11. The gas pressure and temperature in the two sub-cavities can be controlled separately, thereby accurately measuring the hydrogen isotope permeation parameters of the material. For example, it can accurately measure the hydrogen isotope separation factor, diffusion coefficient, permeation coefficient, and pressure index of the material, with high accuracy and excellent data resolution. Simultaneously, the independent control of the two sub-cavities allows the same testing device to simulate various experimental conditions, measure the transport parameters of each gas component under different pressures, and make it possible to evaluate the competitive permeation effect and separation performance between isotopes.

[0069] In some embodiments, the vacuuming structure includes a mechanical pump 41 and a molecular pump assembly 42. Both the mechanical pump 41 and the molecular pump assembly 42 are selectively connected to the inlet sub-cavity 12 and the permeation sub-cavity 13, and are configured to simultaneously evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13 sequentially. That is, the mechanical pump 41 and the molecular pump assembly 42 can be connected to the inlet sub-cavity 12 and the permeation sub-cavity 13 respectively, and can evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13 connected to them.

[0070] Specifically, such as Figure 1 As shown, the mechanical pump 41 is connected to the inlet sub-cavity 12, and the molecular pump group 42 is connected to the permeate sub-cavity 13. In actual operation, the mechanical pump 41 can be turned on first to extract the gas in the inlet sub-cavity 12. For example, the pressure in the inlet sub-cavity 12 and the permeate sub-cavity 13 can be reduced to below 10 Pa. Then, the molecular pump group 42 can be turned on to continue to evacuate the permeate sub-cavity 13 so that the interior of the membrane test chamber 1 reaches a high vacuum state. This ensures that no excess gas remains inside the membrane test chamber 1, thus avoiding any impact on the accuracy of the test results.

[0071] In some embodiments, the air intake tank 2 and the air intake sub-cavity 12 are connected by an air intake pipe 7. Gas can be transported from the air intake tank 2 to the air intake sub-cavity 12 through the air intake pipe 7. The air intake pipe 7 is provided with two first air intake valves 71. The inlet of the mechanical pump 41 is connected to the two first air intake valves 71. The two first air intake valves 71 can control the gas flow rate in the air intake pipe 7.

[0072] Specifically, such as Figure 1As shown, an intake tank 2 is provided on one side of the intake sub-cavity 12. The intake tank 2 can store hydrogen isotope gas or mixed gas. The intake tank 2 is connected to the intake sub-cavity 12 through the intake pipe 7. Two first intake valves 71 are provided between the intake tank 2 and the intake sub-cavity 12. At the same time, the part of the intake pipe 7 between the two first intake valves 71 is connected to the inlet of the mechanical pump 41. In practice, the first intake valve 71 near the intake tank 2 can be closed, and the first intake valve 71 near the intake sub-cavity 12 can be opened. Then, the mechanical pump 41 can be turned on to evacuate the intake sub-cavity 12. When it is necessary to introduce gas into the intake sub-cavity 12, the first intake valve 71 near the mechanical pump 41 can be closed, and the first intake valve 71 near the intake sub-cavity 12 can be opened. Thus, the gas in the intake tank 2 can enter the intake sub-cavity 12 through the intake pipe 7, and the gas will not flow out from the mechanical pump 41, thereby realizing the evacuation of the intake sub-cavity 12 and the introduction of gas.

[0073] And / or, in some other embodiments, the collection tank 3 and the permeation chamber 13 are connected by an outlet pipe 8. Gas can enter the collection tank 3 from the permeation chamber 13 through the outlet pipe 8. The outlet pipe 8 is provided with two first outlet valves 81. The inlet of the molecular pump group 42 is connected to the two first outlet valves 81. The two first outlet valves 81 can control the gas flow rate in the outlet pipe 8.

[0074] For example, a collection tank 3 and a molecular pump assembly 42 are provided on one side of the permeate chamber 13. Two first gas outlet valves 81 are provided between the collection tank 3 and the permeate chamber 13. At the same time, the portion of the gas outlet pipeline 8 located between the two first gas outlet valves 81 is connected to the inlet of the molecular pump assembly 42. In actual operation, the first gas outlet valve 81 near the collection tank 3 can be closed, and the first gas outlet valve 81 near the molecular pump assembly 42 can be opened. Then, the molecular pump assembly 42 can be opened to evacuate the permeate chamber 13. When it is necessary to collect gas in the collection tank 3, the first gas outlet valve 81 near the molecular pump assembly 42 can be closed, and the first gas outlet valve 81 near the collection tank 3 can be opened. Thus, the gas in the permeate chamber 13 can enter the collection tank 3 through the gas outlet pipeline 8 to facilitate the analysis of gas components.

[0075] In some embodiments, the intake pipe 7 is connected to a first pressure detector 72, which is connected between two first intake valves 71. A first detection control valve 73 is provided between the first pressure detector 72 and the intake pipe 7. The first pressure detector 72 can detect the gas pressure on one side of the intake tank 2 to facilitate the control of the gas pressure on the intake side; the first detection control valve 73 can control the connection between the first pressure detector 72 and the intake pipe 7.

[0076] And / or, in other embodiments, the gas outlet pipe 8 is connected to a second pressure detector 82, which is connected between the two first gas outlet valves 81. A second detection control valve 83 is provided between the second pressure detector 82 and the gas outlet pipe 8. The second pressure detector 82 can detect the gas pressure on one side of the collection tank 3 to facilitate the control of the gas pressure on the permeation side; the second detection control valve 83 can control the connection between the second pressure detector 82 and the gas outlet pipe 8.

[0077] Specifically, such as Figure 1 As shown, a first detection control valve 73 and a first pressure detector 72 are sequentially connected in the air inlet pipe 7 between the air inlet sub-chamber 12 and the air inlet tank 2. A second detection control valve 83 and a second pressure detector 82 are sequentially connected in the air outlet pipe 8 between the permeation sub-chamber 13 and the collection tank 3. In actual operation, the first detection control valve 73 and the second detection control valve 83 can be opened simultaneously. In this way, the first pressure detector 72 and the second pressure detector 82 can simultaneously detect the gas pressure on the air inlet side and the permeation side, thereby ensuring the pressure conditions during the test and improving the accuracy of the test.

[0078] Among them, the first pressure detector 72 and the second pressure detector 82 can be high-precision pressure transmitters to achieve the measurement of pressure in the range of high vacuum to hundreds of kilopascals, so as to meet the requirements of measuring the small permeation of the membrane sample 11 and the high pressure on the inlet side.

[0079] In some embodiments, an intermediate pipe 9 connects the intake pipe 7 and the exhaust pipe 8, and an intermediate control valve 91 is provided in the intermediate pipe 9; that is, the intake pipe 7 and the exhaust pipe 8 can be connected through the intermediate pipe 9, wherein the intermediate control valve 91 can control the connection and disconnection of the intake pipe 7 and the exhaust pipe 8.

[0080] Specifically, when the mechanical pump 41 is connected to the inlet sub-cavity 12 via the inlet pipe 7, it is connected to the permeation sub-cavity 13 via the intermediate pipe 9 and the outlet pipe 8. Similarly, when the molecular pump assembly 42 is connected to the permeation sub-cavity 13 via the outlet pipe 8, it is connected to the inlet sub-cavity 12 via the intermediate pipe 9 and the inlet pipe 7. For example... Figure 1As shown, when the mechanical pump 41, the first inlet valve 71, and the intermediate control valve 91 are opened, the mechanical pump 41 can simultaneously evacuate the inlet sub-cavity 12 and the permeate sub-cavity 13. That is, the mechanical pump 41 can evacuate the permeate sub-cavity 13 through the intermediate pipeline 9. When the molecular pump group 42, the first outlet valve 81, and the intermediate control valve 91 are opened, the molecular pump group 42 can simultaneously evacuate the permeate sub-cavity 13 and the inlet sub-cavity 12. That is, the molecular pump group 42 can evacuate the inlet sub-cavity 12 through the intermediate pipeline 9. Thus, both the mechanical pump 41 and the molecular pump group 42 can evacuate the inlet sub-cavity 12 and the permeate sub-cavity 13, which can minimize the gas in the membrane test chamber 1 to achieve a vacuum state, thereby improving the accuracy of the test results.

[0081] In other words, by setting the intermediate pipeline 9, the connection state between the inlet pipeline 7 and the outlet pipeline 8 can be flexibly switched, which makes it easier for the mechanical pump 41 and the molecular pump group 42 to simultaneously evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13, respectively, reducing the need for additional vacuuming structures and reducing the cost of vacuuming setup.

[0082] In some embodiments, the high-resolution mass spectrometer 6 is connected to the gas outlet line 8 via a detection line 61, and a detection control valve 62 is provided in the detection line 61. Specifically, as shown... Figure 1 As shown, after the detection control valve 62 is opened, the gas in the collection tank 3 can enter the high-resolution mass spectrometer 6 through the gas outlet pipe 8 and the detection pipe 61. The high-resolution mass spectrometer 6 can perform component analysis on the transported gas, thereby accurately measuring the proportion of hydrogen isotopes in the gas in the permeation chamber 13, and then calculating the hydrogen isotope separation coefficient.

[0083] Therefore, by setting up the detection pipeline 61 and the detection control valve 62, the connection state between the high-resolution mass spectrometer 6 and the permeation sub-cavity 13 can be flexibly controlled, so that accurate and reliable analysis can be performed by the high-resolution mass spectrometer 6 when performing permeation gas detection and analysis.

[0084] In some embodiments, there are multiple air intake canisters 2, and each of the multiple air intake canisters 2 is configured to selectively communicate with the air intake sub-cavity 12, with at least two air intake canisters 2 containing different gas compositions. Specifically, as shown in the figure... Figure 1As shown, there are three gas inlet tanks 2, and the connection between the three gas inlet tanks 2 and the gas inlet sub-cavity 12 can be controlled by the first gas inlet valve 71. That is to say, the number of gas inlet tanks 2 connected to the gas inlet sub-cavity 12 can be one, two, three, or none of them can be connected to the gas inlet sub-cavity 12. Thus, the vacuuming of the membrane test chamber 1 and the gas delivery of the gas inlet tanks 2 to the gas inlet sub-cavity 12 can be realized. Among them, the gases in the two gas inlet tanks 2 are different, or the gases in the three gas inlet tanks 2 are all different. Thus, different gases can be used to detect the hydrogen isotope permeation parameters of the membrane sample 11, such as the determination of hydrogen isotope separation factor, diffusion coefficient, permeation coefficient and pressure index, which is faster and more convenient.

[0085] This invention also proposes a method for testing the hydrogen isotope permeation parameters of materials used in fusion reactors.

[0086] The method for testing hydrogen isotope permeation parameters of fusion reactor application materials according to embodiments of the present invention employs the testing apparatus 100 for hydrogen isotope permeation parameters of fusion reactor application materials as described above, and as follows: Figures 2-7 As shown, the test methods include:

[0087] S1. Install the membrane sample 11 inside the membrane test chamber 1, dividing the inner cavity of the membrane test chamber 1 into an inlet sub-cavity 12 and a permeation sub-cavity 13. The membrane sample 11 can be a palladium membrane or other materials, and the permeation parameters of the material can be tested using hydrogen isotope gas. Specifically, for example... Figure 1 As shown, the user can fix the membrane sample 11 in the middle of the membrane test chamber 1. In this way, the membrane test chamber 1 is divided into the permeate sub-chamber 13 on the left and the air inlet sub-chamber 12 on the right by the membrane sample 11.

[0088] S2. Evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13. Specifically, the mechanical pump 41 or the molecular pump assembly 42 can be turned on to evacuate the inlet sub-cavity 12 or the permeation sub-cavity 13, wherein the vacuum level is detected by an ion vacuum gauge.

[0089] S3. Heat the inlet sub-cavity 12 and the permeate sub-cavity 13 to the target temperature. Specifically, the user can manually activate the heating structure 5. That is, when it is necessary to heat the permeate sub-cavity 13 and the inlet sub-cavity 12, commands can be input at the operation interface or via voice. The control unit will then control the heating structure 5 to slowly heat the inlet sub-cavity 12 and the permeate sub-cavity 13. During the heating process, a temperature sensor located near the membrane sample 11 monitors the temperature of the membrane sample 11 in real time and transmits the temperature information to the control unit. This allows the control unit to constantly control the heating output of the heating structure 5 to maintain a constant temperature for the membrane sample 11.

[0090] S4. Test gas is introduced into the inlet sub-cavity 12, and the gas pressure in the inlet sub-cavity 12 is maintained at a set pressure value. The type and combination of gas can be selected according to the membrane sample 11 being measured. When testing the permeation performance of the membrane sample 11 for single hydrogen gas, pure hydrogen gas can be selected. When testing the separation coefficient of the membrane sample 11, a mixture of hydrogen and deuterium in an equimolar ratio can be selected. Specifically, the first inlet valve 71 near the inlet sub-cavity 12 in the inlet pipeline 7 can be opened, and the first inlet valve 71 near the inlet tank 2 can be opened slowly. Gas can enter the inlet sub-cavity 12 through the inlet pipeline 7. The speed at which the gas enters the inlet sub-cavity 12 can be controlled by adjusting the opening degree of the first inlet valve 71 or by setting a regulating pressure valve, thereby increasing the pressure on the inlet side to a predetermined experimental value, such as 0.1 MPa.

[0091] Furthermore, the first detection control valve 73 is opened, the value of the first pressure detector 72 reaches the predetermined experimental value, and the experimental value is maintained at the predetermined value by controlling the first air inlet valve 71. The gas in the air inlet sub-cavity 12 begins to slowly permeate through the membrane sample 11, and gas begins to accumulate in the permeation sub-cavity 13. The second detection control valve 83 is opened, and the second pressure detector 82 can detect that the pressure in the permeation sub-cavity 13 gradually increases. The pressure change curve in the permeation sub-cavity 13 over time can be recorded by the data acquisition system.

[0092] S5. Sampling and analysis of the permeate gas in the permeate chamber 13. Specifically, the detection control valve 62 and the first outlet valve 81 can be opened, and the gas in the collection tank 3 can enter the high-resolution mass spectrometer 6 through the detection pipeline 61. The high-resolution mass spectrometer 6 can accurately measure the hydrogen isotope composition ratio of the gas. After the gas pressure on the permeate side rises linearly and the mass spectrum composition stabilizes, the collected data can be calculated and analyzed. By using the slope of the steady-state segment in the pressure-time curve, i.e., the slope of the segment where the gas pressure rises linearly and the mass spectrum composition is stable, the steady-state flow rate of the permeate gas can be calculated using the ideal gas law. Then, combined with the effective permeate area of ​​the membrane sample 11 and the pressure on the inlet side, parameters such as the permeation coefficient of the membrane sample 11 for this gas can be further calculated. After multiple tests with varying inlet side pressure, the steady-state flow rate calculated from the multiple tests can be plotted and fitted with the corresponding pressure values ​​on a logarithmic coordinate system to obtain the relationship index between the steady-state flow rate and the pressure value. This relationship index can characterize the degree to which the membrane sample 11 is controlled by diffusion or surface reaction during the permeation process.

[0093] Furthermore, the separation coefficient of membrane sample 11 at the corresponding temperature and pressure can be obtained by measuring the ratio of each component in the permeate gas using high-resolution mass spectrometry and dividing it by the ratio of each component on the inlet side. Thus, the permeation performance of membrane sample 11 can be obtained.

[0094] In some embodiments, evacuating the inlet sub-cavity 12 and the permeation sub-cavity 13 includes:

[0095] S6. First, a vacuum is created in the inlet sub-cavity 12 and the permeation sub-cavity 13 using the mechanical pump 41. Specifically, the first inlet valve 71, the intermediate control valve 91, and the mechanical pump 41 are opened. The mechanical pump 41 can simultaneously evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13.

[0096] S7. Then, a secondary vacuum is applied to the inlet sub-cavity 12 and the permeation sub-cavity 13 by the molecular pump assembly 42. Specifically, the first outlet valve 81, the intermediate control valve 91, and the molecular pump assembly 42 are opened, and the molecular pump assembly 42 can simultaneously evacuate the inlet sub-cavity 12 and the permeation sub-cavity 13.

[0097] Therefore, both the mechanical pump 41 and the molecular pump assembly 42 can evacuate the air inlet chamber 12 and the permeate chamber 13 to minimize the amount of residual air in the membrane test chamber 1 and avoid affecting the test results.

[0098] In some embodiments, the method for testing the hydrogen isotope permeation parameters of materials used in fusion reactors further includes:

[0099] S8. After evacuating the air inlet sub-cavity 12 and the permeation sub-cavity 13, the air inlet sub-cavity 12 is purged of gas and leaks are detected.

[0100] In some embodiments, gas purging of the intake chamber 12 includes:

[0101] S9. Purge the inlet sub-cavity 12 with high-purity inert gas, then re-evacuate the vacuum, repeating this process several times to remove any remaining adsorbed gas from the pipeline and cavity. Specifically, open the first inlet valve 71 near the inlet sub-cavity 12 and close the first inlet valve 71 near the mechanical pump 41. High-purity inert gas enters the inlet sub-cavity 12 through the inlet pipeline 7. Then close the first inlet valve 71 near the inlet tank 2 and open the first inlet valve 71 near the mechanical pump 41 and the mechanical pump 41. The mechanical pump 41 begins to extract the gas from the inlet sub-cavity 12. Repeating this process several times will remove all the adsorbed gas from the inlet sub-cavity 12, preventing any impact on the test results.

[0102] In some embodiments, leak detection of the intake chamber 12 includes:

[0103] S10. Introduce a high-purity inert gas at a certain pressure into the air inlet chamber 12.

[0104] S11. Mass spectrometry is used to detect the gas in the permeation chamber 13.

[0105] S12. If no significant signal of the mass-to-charge ratio of high-purity inert gas is detected in the gas from the permeation chamber 13, it is determined that there is no leakage in the inlet chamber 12.

[0106] S13, and when a significant signal of the mass-to-charge ratio of high-purity inert gas is detected in the gas from the permeation chamber 13, it is determined that the intake chamber 12 is leaking.

[0107] Specifically, high-purity helium gas at a certain pressure, such as 300 kPa, can be introduced into the inlet sub-cavity 12. The first outlet valve 81 near the permeate sub-cavity 13 is closed, and the permeate sub-cavity 13 is kept under vacuum. The high-resolution mass spectrometer 6 is turned on to monitor the mass spectrometry signal in the permeate sub-cavity 13. If no significant signal of the mass-to-charge ratio of the high-purity inert gas is detected, there is no leakage in the membrane sample 11 and its sealing connection. If a significant signal of the mass-to-charge ratio of the high-purity inert gas is detected, there is leakage in the membrane sample 11 and its sealing connection. The detection can be stopped, the membrane sample 11 can be inspected, and it can be resealed.

[0108] In some embodiments, mounting the membrane sample 11 inside the membrane test chamber 1 includes:

[0109] S14. Fix the membrane sample 11 inside the membrane test chamber 1 using a VCR connector or flange, and seal and isolate the inlet sub-chamber 12 and the permeate sub-chamber 13. Specifically, the membrane sample 11 can be installed on the sealing fixture of the membrane test chamber 1, and the membrane sample 11 is fixed to the sealing fixture using a VCR connector or flange. In this way, the membrane sample 11 can completely isolate the inlet sub-chamber 12 and the permeate sub-chamber 13. At the same time, check the sealing ring, connecting joints, etc. to ensure that the membrane sample 11 is completely sealed to ensure that the membrane test chamber 1 is leak-free under vacuum and high pressure conditions.

[0110] Therefore, by adopting effective gas path purification measures and a high-vacuum sealed membrane test chamber 1, the cross-interference of residual gases between different test experiments can be significantly reduced, so that the surface state of the membrane sample 11 and the system background are consistent, thereby making the test data have good reproducibility and making the permeation performance obtained under different pressures and temperatures more consistent.

[0111] Furthermore, the cooperation between the first pressure detector 72, the second pressure detector 82, and the high-resolution mass spectrometer 6 enables highly sensitive monitoring of the permeation process. The first pressure detector 72 and the second pressure detector 82 can capture minute pressure changes and promptly reflect the initial permeation dynamics. At the same time, the high-resolution mass spectrometer 6 can distinguish gas components in real time. Thus, the device can obtain richer and more detailed hydrogen isotope transport information.

[0112] Furthermore, the second pressure detector 82 can record the constant rate of pressure rise to accurately calculate the steady-state permeation flux, pressure index, and separation coefficient. Multiple sets of experiments can be conducted by changing the inlet side pressure to plot the relationship curve between steady-state permeation flux and pressure and obtain the pressure index to determine the permeation mechanism. At the same time, the separation coefficient can be obtained by analyzing the gas components through the high-resolution mass spectrometer 6. Thus, various parameters can be obtained quickly and accurately to evaluate the hydrogen isotope permeation parameters of the membrane sample 11 under different conditions.

[0113] The valves in this device can be solenoid valves controlled by a programmable logic controller (PLC) or a computer to achieve automated gas control, improving the controllability and repeatability of the experiment and reducing errors. Simultaneously, the connection between the membrane test chamber 1 and the membrane sample 11 can be adjusted according to different membrane samples 11. When the membrane sample 11 being tested is a hollow fiber membrane or a tubular membrane, the clamping assembly can be replaced to ensure the sealing performance of the membrane test chamber 1. Furthermore, when the membrane sample 11 being tested is a composite membrane or a coated membrane, carrier support structures can be added to both sides of the membrane sample 11 or the sealing method can be adjusted, thus enabling the device to adapt to membrane samples 11 of different shapes and sizes to ensure good sealing performance.

[0114] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0115] Although embodiments of the invention have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.

Claims

1. A testing device for hydrogen isotope permeation parameters of materials used in fusion reactors, characterized in that, include: A membrane test chamber (1) is provided, in which a membrane sample (11) is installed. The membrane sample (11) divides the inner cavity of the membrane test chamber (1) into an inlet sub-cavity (12) and a permeate sub-cavity (13). The gas inlet (2) and the gas collection tank (3) are selectively connected to the gas inlet sub-cavity (12) to supply test gas to the gas inlet sub-cavity (12), and the gas collection tank (3) is selectively connected to the permeation sub-cavity (13) to collect the gas flowing out of the permeation sub-cavity (13). The vacuuming structure and the heating structure (5) are used to evacuate the air inlet sub-cavity (12) and the permeation sub-cavity (13), and the heating structure (5) is used to heat the air inlet sub-cavity (12) and the permeation sub-cavity (13). A high-resolution mass spectrometer (6) is selectively connected to the permeation sub-cavity (13), and the gas in the permeation sub-cavity (13) selectively flows into the high-resolution mass spectrometer (6). The vacuuming structure includes a mechanical pump (41) and a molecular pump group (42). Both the mechanical pump (41) and the molecular pump group (42) are configured to selectively communicate with the inlet sub-cavity (12) and the permeation sub-cavity (13), and the mechanical pump (41) and the molecular pump group (42) are configured to simultaneously evacuate the inlet sub-cavity (12) and the permeation sub-cavity (13) in sequence. The air inlet tank (2) and the air inlet sub-chamber (12) are connected by an air inlet pipe (7). The air inlet pipe (7) is provided with two first air inlet valves (71). The inlet of the mechanical pump (41) is connected to the two first air inlet valves (71). The collection tank (3) and the permeation chamber (13) are connected by an outlet pipe (8), and the outlet pipe (8) is provided with two first outlet valves (81). The inlet of the molecular pump group (42) is connected to the two first outlet valves (81). An intermediate pipe (9) is connected between the air intake pipe (7) and the air outlet pipe (8), and an intermediate control valve (91) is provided in the intermediate pipe (9). When the mechanical pump (41) is connected to the inlet sub-cavity (12) through the inlet pipe (7), it is connected to the permeation sub-cavity (13) through the intermediate pipe (9) and the outlet pipe (8). When the molecular pump group (42) is connected to the permeation sub-cavity (13) through the outlet pipe (8), it is connected to the inlet sub-cavity (12) through the intermediate pipe (9) and the inlet pipe (7).

2. The testing device for hydrogen isotope permeation parameters of fusion reactor application materials according to claim 1, characterized in that, The intake pipe (7) is connected to a first pressure detector (72), which is connected to the two first intake valves (71). A first detection control valve (73) is provided between the first pressure detector (72) and the intake pipe (7). And / or, the outlet pipe (8) is connected to a second pressure detector (82), the second pressure detector (82) is connected between the two first outlet valves (81), and a second detection control valve (83) is provided between the second pressure detector (82) and the outlet pipe (8).

3. The testing device for hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 1, characterized in that, The high-resolution mass spectrometer (6) is connected to the gas outlet pipeline (8) through a detection pipeline (61), and a detection control valve (62) is provided in the detection pipeline (61).

4. The testing device for hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 1, characterized in that, There are multiple air intake tanks (2), and each of the multiple air intake tanks (2) is configured to selectively communicate with the air intake sub-cavity (12), and at least two of the air intake tanks (2) have different gas compositions.

5. A method for testing hydrogen isotope permeation parameters of materials used in fusion reactors, characterized in that, The apparatus for testing hydrogen isotope permeation parameters of materials used in fusion reactors according to any one of claims 1-4, wherein the testing method comprises: The membrane sample (11) is installed in the membrane test chamber (1), and the inner cavity of the membrane test chamber (1) is divided into an air inlet sub-cavity (12) and a permeate sub-cavity (13). Vacuum the inlet sub-cavity (12) and the permeation sub-cavity (13); The air intake chamber (12) and the permeation chamber (13) are heated to the target temperature; Test gas is introduced into the air inlet sub-cavity (12), and the air pressure in the air inlet sub-cavity (12) is maintained at a set pressure value; The permeated gas in the permeation sub-cavity (13) is sampled and analyzed.

6. The method for testing hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 5, characterized in that, The process of evacuating the air inlet chamber (12) and the permeation chamber (13) includes: First, a vacuum is applied to the air inlet chamber (12) and the permeation chamber (13) using a mechanical pump (41); Then, a secondary vacuum is applied to the inlet sub-cavity (12) and the permeation sub-cavity (13) by a molecular pump assembly (42).

7. The method for testing hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 5, characterized in that, Also includes: After evacuating the air intake sub-cavity (12) and the permeation sub-cavity (13), the air intake sub-cavity (12) is purged of gas and leaks are detected.

8. The method for testing hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 7, characterized in that, The gas purging of the air intake sub-chamber (12) includes: High-purity inert gas is introduced into the air inlet sub-cavity (12) for flushing, and then vacuum is re-evacuated. This process is repeated several times to remove residual adsorbed gas from the pipeline and cavity.

9. The method for testing hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 7, characterized in that, The leakage detection of the air intake sub-cavity (12) includes: A high-purity inert gas at a certain pressure is introduced into the air inlet sub-cavity (12); Mass spectrometry was used to detect the gas in the permeation chamber (13); When no significant signal of the mass-to-charge ratio of the high-purity inert gas is detected in the gas from the permeation sub-cavity (13), it is determined that there is no leakage in the inlet sub-cavity (12); And, when a significant signal of the mass-to-charge ratio of the high-purity inert gas is detected from the gas in the permeation sub-cavity (13), it is determined that the inlet sub-cavity (12) is leaking.

10. The method for testing hydrogen isotope permeation parameters of materials used in fusion reactors according to claim 5, characterized in that, The step of installing the membrane sample (11) into the membrane test chamber (1) includes: The membrane sample (11) is fixed in the membrane test chamber (1) using a VCR connector or flange, and the air inlet chamber (12) and the permeate chamber (13) are sealed and isolated.

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