Hydrogen isotope permeation amount measuring device and use method thereof

Abstract

The invention discloses a hydrogen isotope permeation amount measuring device and a use method thereof. The device comprises a mass spectrometer, a standard leak hole, a vacuum pump group, a first vacuum valve, a second vacuum valve, a plasma discharge chamber, a bias power supply, a thermocouple, a temperature recorder, a plasma source and a hydrogen cylinder, an isolator, a permeation pipeline, a heater and a sample table are arranged in the plasma discharge chamber, and the sample table is used for sealing and fixing the metal sample. By adopting the technical scheme provided by the invention, the permeation amount of the hydrogen isotope passing through the metal sample under the plasma irradiation condition can be simply and conveniently measured, so that the permeation amount is not limited by experimental conditions and operation time of large scientific devices such as Tokamak and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of fusion device measurement, and particularly relates to a measuring device for the permeation amount of hydrogen isotopes and a using method thereof. Background Art

[0002] The deuterium-tritium reaction is the most promising controllable nuclear fusion method. Therefore, fusion reactors usually use hydrogen isotopes deuterium and tritium as fuels. The magnetic confinement fusion reactor realizes the fusion reaction by confining high-temperature plasma of several keV with a strong magnetic field. The plasma reaching the boundary of the fusion reactor still has an energy of several eV to several hundred eV. The operating temperature range of the plasma-facing material in the reactor is several hundred degrees Celsius or even over a thousand degrees Celsius. Hydrogen isotopes are very easy to penetrate into the cooling circuit through materials at high temperatures. Especially expensive and radioactive tritium will irradiate the material in the form of plasma at the boundary of the fusion reactor and penetrate into the coolant, thus affecting the economy and safety of the fusion reactor. Therefore, the measurement of the permeation amount of hydrogen isotopes becomes very important.

[0003] Currently, due to the limitations of the experimental conditions and operating time of large scientific devices such as tokamaks, it is not convenient to experimentally evaluate the permeation amount of hydrogen isotopes during the steady-state operation of future fusion reactors. And the measurement of the permeation amount of hydrogen isotopes in the laboratory is usually carried out under the condition of hydrogen exposure. Under the condition of plasma irradiation, due to the existence of plasma current and the conductivity of the sample, it is difficult to measure the permeation of hydrogen isotopes. Summary of the Invention

[0004] The purpose of the embodiments of the present invention is to provide a measuring device for the permeation amount of hydrogen isotopes and a using method thereof, which can simply and conveniently measure the permeation amount of hydrogen isotopes passing through a metal sample under the condition of plasma irradiation, and is not restricted by the experimental conditions and operating time of large scientific devices such as tokamaks.

[0005] To achieve the above purpose, the embodiments of the present invention provide a measuring device for the permeation amount of hydrogen isotopes, which is used to measure the permeation amount of hydrogen isotopes passing through a metal sample under the condition of plasma irradiation, and includes: a mass spectrometer, a standard leak, a vacuum pump group, a first vacuum valve, a second vacuum valve, a plasma discharge chamber, a bias power supply, a thermocouple, a temperature recorder, a plasma source, and a hydrogen gas cylinder; the plasma discharge chamber includes an isolator, a permeation pipeline, a heater, and a sample stage, and the sample stage is used to seal and fix the metal sample; One end of the isolator is communicated with the sample stage through the permeation pipeline; the heater is arranged in the permeation pipeline and keeps a preset distance from the sample stage; the outlets of the plasma source and the hydrogen cylinder are both communicated with the plasma discharge chamber; the bias power supply is connected between the outer shell of the plasma discharge chamber and the sample stage; the thermocouple is connected between the sample stage and the temperature recorder; The other end of the isolator is communicated with the mass spectrometer through the first pipeline, communicated with the standard leak through the second pipeline, and communicated with the vacuum pump group through the third pipeline, and the ends of the first pipeline, the second pipeline, and the third pipeline close to the isolator converge into one path and then are docked to the other end of the isolator; the first vacuum valve is arranged at one end of the second pipeline close to the standard leak; the second vacuum valve is arranged at one end of the converged pipeline close to the isolator.

[0006] Further, the positive electrode of the bias power supply is connected to the outer shell of the plasma discharge chamber, the negative electrode of the bias power supply is connected to the sample stage, and the outer shell of the plasma discharge chamber is grounded.

[0007] Further, the sample stage includes a flange sealing structure, and the flange sealing structure includes a knife-edge flange, a gasket, a cover plate and fasteners.

[0008] Further, the vacuum pump group is a molecular pump group, and the isolator is a ceramic isolator.

[0009] Further, the plasma source is a microwave plasma source, a radio frequency plasma source or a hot cathode plasma source.

[0010] To achieve the above object, an embodiment of the present invention further provides a usage method of a hydrogen isotope permeation amount measuring device, which is applied to the hydrogen isotope permeation amount measuring device described in any one of the above, including: Seal and fix the metal sample on the sample stage; Close the first vacuum valve, open the second vacuum valve, and use the vacuum pump group to evacuate the permeation pipeline; When the vacuum degree in the permeation pipeline reaches a preset vacuum degree threshold, open the mass spectrometer and start the hydrogen isotope permeation experiment; wherein, the permeation experiment includes: heating the metal sample by using the heater, applying a bias voltage to the metal sample by using the bias power supply, and opening the hydrogen cylinder and the plasma source, and bombarding the metal sample by using the generated plasma; After the permeation experiment is completed, open the first vacuum valve, close the second vacuum valve, open the standard leak, and record the steady-state current value of the mass spectrometer at the current sample temperature and the current ion incident energy. Based on the standard leakage rate of the standard leak hole, the steady-state calibration current value of the mass spectrometer, and the steady-state current value, obtain the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation conditions.

[0011] Further, the method further includes: Record in real time the permeation change state of hydrogen isotopes during the permeation experiment; Judge whether the steady permeation state is reached according to the permeation change state; When it is determined that the steady permeation state is reached, end the permeation experiment.

[0012] Further, the obtaining of the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation conditions according to the standard leakage rate of the standard leak hole, the steady-state calibration current value of the mass spectrometer, and the steady-state current value specifically includes: According to the formula Calculate to obtain the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation conditions; where, J ∞ is the steady-state permeation amount, S calib is the standard leakage rate of the standard leak hole, A is the effective permeation area of the metal sample, I ∞ is the steady-state current value, I calib is the steady-state calibration current value of the mass spectrometer.

[0013] Further, the method further includes: Use the heater to adjust the sample temperature of the metal sample to measure the steady-state permeation amount of hydrogen isotopes at different sample temperatures.

[0014] Further, the method further includes: Use the bias power supply to adjust the ion incident energy of the plasma to measure the steady-state permeation amount of hydrogen isotopes at different ion incident energies.

[0015] Compared with the prior art, the embodiment of the present invention provides a measuring device for the permeation amount of hydrogen isotopes and a using method thereof. The device includes a mass spectrometer, a standard leak, a vacuum pump group, a first vacuum valve, a second vacuum valve, a plasma discharge chamber, a bias power supply, a thermocouple, a temperature recorder, a plasma source, and a hydrogen gas cylinder. The plasma discharge chamber includes an isolator, a permeation pipeline, a heater, and a sample stage. The using method applied to the device includes: sealing and fixing a metal sample on the sample stage; closing the first vacuum valve and opening the second vacuum valve, and using the vacuum pump group to evacuate the permeation pipeline; when the vacuum degree in the permeation pipeline reaches a preset vacuum degree threshold, opening the mass spectrometer and starting the hydrogen isotope permeation experiment, that is, heating the metal sample by using the heater, applying a bias voltage to the metal sample by using the bias power supply, and opening the hydrogen gas cylinder and the plasma source, and bombarding the metal sample with the generated plasma; after the permeation experiment ends, opening the first vacuum valve, closing the second vacuum valve, opening the standard leak, and recording the steady-state current value of the mass spectrometer at the current sample temperature and the current ion incident energy; according to the standard leak rate of the standard leak, the steady-state calibration current value and the steady-state current value of the mass spectrometer, obtaining the steady-state permeation amount of the hydrogen isotope passing through the metal sample under the plasma irradiation condition. The embodiment of the present invention can simply and conveniently measure the permeation amount of the hydrogen isotope passing through the metal sample under the plasma irradiation condition, and make it not restricted by the experimental conditions and operation time of large scientific devices such as tokamaks. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 FIG. is a schematic structural diagram of a measuring device for the permeation amount of hydrogen isotopes provided by an embodiment of the present invention; Figure 2 FIG. is a schematic structural diagram of a flange sealing structure provided by an embodiment of the present invention; Figure 3 FIG. is a product example diagram of a ceramic isolator provided by an embodiment of the present invention; Figure 4 FIG. is a deuterium permeation amount curve diagram of a martensitic steel provided by an embodiment of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0017] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0018] The embodiment of the present invention provides a measuring device for the permeation amount of hydrogen isotopes. The device is used to measure the permeation amount of the hydrogen isotope passing through the metal sample under the plasma irradiation condition. Refer toFigure 1 As shown in the figure, it is a schematic structural diagram of a device for measuring the hydrogen isotope permeation amount provided by an embodiment of the present invention. The device includes: a mass spectrometer 1, a standard leak 2, a vacuum pump group 3, a first vacuum valve 4, a second vacuum valve 5, a plasma discharge chamber 6, a bias power supply 11, a thermocouple 12, a temperature recorder 13, a plasma source 14, and a hydrogen gas cylinder 15; inside the plasma discharge chamber 6, there are an isolator 7, a permeation pipeline 8, a heater 9, and a sample stage 10, and the sample stage 10 is used to seal and fix the metal sample; One end of the isolator 7 is communicated with the sample stage 10 through the permeation pipeline 8; the heater 9 is arranged inside the permeation pipeline 8 and keeps a preset distance from the sample stage 10; the outlet of the plasma source 14 and the outlet of the hydrogen gas cylinder 15 are both communicated with the plasma discharge chamber 6; the bias power supply 11 is connected between the outer shell of the plasma discharge chamber 6 and the sample stage 10; the thermocouple 12 is connected between the sample stage 10 and the temperature recorder 13; The other end of the isolator 7 is communicated with the mass spectrometer 1 through a first pipeline L1, communicated with the standard leak 2 through a second pipeline L2, and communicated with the vacuum pump group 3 through a third pipeline L3. And the ends of the first pipeline L1, the second pipeline L2, and the third pipeline L3 close to the isolator 7 converge into one path and then dock to the other end of the isolator 7; the first vacuum valve 4 is arranged at one end of the second pipeline L2 close to the standard leak 2; the second vacuum valve 5 is arranged at one end of the converged pipeline L4 close to the isolator 7.

[0019] Specifically, the device is mainly composed of a mass spectrometer 1, a standard leak 2, a vacuum pump group 3, a first vacuum valve 4, a second vacuum valve 5, a plasma discharge chamber 6, an isolator 7, a permeation pipeline 8, a heater 9, a sample stage 10, a bias power supply 11, a thermocouple 12, a temperature recorder 13, a plasma source 14, and a hydrogen gas cylinder 15. And the isolator 7, the permeation pipeline 8, the heater 9, and the sample stage 10 are arranged inside the plasma discharge chamber 6.

[0020] Further, one end of the isolator 7 (i.e., Figure 1 the right end of the isolator 7 shown in the figure) is communicated with the sample stage 10 through the permeation pipeline 8. The heater 9 is arranged at one end of the inside of the permeation pipeline 8 close to the sample stage 10, and a preset distance is kept between the heater 9 and the sample stage 10. The outlet of the plasma source 14 is communicated with the plasma discharge chamber 6, the outlet of the hydrogen gas cylinder 15 is communicated with the plasma discharge chamber 6, one end of the bias power supply 11 is connected to the outer shell of the plasma discharge chamber 6, the other end of the bias power supply 11 is connected to the sample stage 10, one end of the thermocouple 12 is connected to the sample stage 10, and the other end of the thermocouple 12 is connected to the temperature recorder 13.

[0021] Further, the other end of the isolator 7 (i.e., Figure 1 the left end of the isolator 7 shown) is connected to the mass spectrometer 1 through the first pipeline L1. The other end of the isolator 7 is also connected to the standard leak 2 through the second pipeline L2. The other end of the isolator 7 is also connected to the vacuum pump group 3 through the third pipeline L3. And one end of the first pipeline L1 close to the isolator 7, one end of the second pipeline L2 close to the isolator 7, and one end of the third pipeline L3 close to the isolator 7 converge into one path, that is, Figure 1 the converged pipeline L4 shown. It is connected to the other end of the isolator 7 through the converged pipeline L4. Equivalently, the first pipeline L1, the second pipeline L2, and the third pipeline L3 share the converged pipeline L4 to be connected to the isolator 7. The first vacuum valve 4 is arranged on the second pipeline L2, and the first vacuum valve 4 is arranged at one end of the second pipeline L2 close to the standard leak 2. The second vacuum valve 5 is arranged on the converged pipeline L4, and the second vacuum valve 5 is arranged at one end of the converged pipeline L4 close to the isolator 7.

[0022] It should be noted that the device can measure the permeation amount of hydrogen isotopes passing through the metal sample in real time under plasma irradiation conditions. And during the actual measurement of the permeation amount of hydrogen isotopes, the sample stage 10 (equipped with a cooling function) is used to seal and fix the metal sample through which hydrogen isotopes will permeate. The sealed metal sample can separate the plasma discharge chamber 6 from the permeation pipeline 8; the isolator 7 is used to cut off the electrical connection between the metal sample on the sample stage 10 and the device; the heater 9 is used to heat the metal sample on the sample stage 10 to change the sample temperature of the metal sample; the thermocouple 12 is used to measure the sample temperature of the metal sample on the sample stage 10 in real time; the temperature recorder 13 is used to record the sample temperature value measured by the thermocouple 12; the bias power supply 11 is used to apply a bias voltage to the metal sample on the sample stage 10, and different magnitudes of bias voltages can be applied to change the ion incident energy of the plasma 16 (generated by the plasma source 14); the plasma source 14 (which can work stably for a long time) is used to generate plasma 16 in the plasma discharge chamber 6 under certain conditions. Preferably, the outlet of the plasma source 14 is arranged opposite to the sample stage 10, so that the plasma 16 generated by the plasma source 14 bombards the surface of the metal sample on the sample stage 10 head-on; the hydrogen cylinder 15 is used to generate hydrogen in the plasma discharge chamber 6 to provide a source of hydrogen isotopes; the vacuum pump group 3 is used to evacuate the inside of the permeation pipeline 8 to provide a vacuum environment; the standard leak 2 (containing calibration gas) is used to calibrate the mass spectrometer 1; the mass spectrometer 1 is used to measure the permeation amount of hydrogen isotopes passing through the metal sample on the sample stage 10.

[0023] It should be noted that the first vacuum valve 4 is used to control the on-off of the passage between the second pipeline L2 and all other pipelines (the first pipeline L1, the third pipeline L3, and the merged pipeline L4), that is, to control the on-off of the passage between the standard leak 2 and the mass spectrometer 1, the vacuum pump group 3, and the permeation pipeline 8; the second vacuum valve 5 is used to control the on-off of the merged pipeline L4, that is, to control the on-off of the passage between the permeation pipeline 8 and the mass spectrometer 1, the standard leak 2, and the vacuum pump group 3.

[0024] Exemplarily, the metal sample can be a sample made of metal materials such as tungsten, copper, steel, etc., and the embodiments of the present invention do not make specific limitations.

[0025] Combined with Figure 1 As shown, in one optional embodiment, the positive electrode of the bias power supply 11 is connected to the outer shell of the plasma discharge chamber 6, the negative electrode of the bias power supply 11 is connected to the sample stage 10, and the outer shell of the plasma discharge chamber 6 is grounded.

[0026] Specifically, combined with the above embodiments, in this embodiment, the outer shell of the plasma discharge chamber 6 can be grounded, the positive electrode of the bias power supply 11 can be connected to the outer shell of the plasma discharge chamber 6, and the negative electrode of the bias power supply 11 can be connected to the sample stage 10, so as to apply different negative biases to the metal sample on the sample stage 10 by using the bias power supply 11 during the actual measurement of the hydrogen isotope permeation amount, thereby changing the ion incident energy.

[0027] Referring to Figure 2 As shown, it is a schematic structural diagram of a flange sealing structure provided by an embodiment of the present invention. In one optional embodiment, the sample stage 10 includes a flange sealing structure, and the flange sealing structure includes a knife-edge flange 17, a gasket 18, a cover plate 19, and a fastener 20.

[0028] It should be noted that the fastener 20 includes Figure 2 the bolt 20a and nut 20b shown, and there is a pair of bolt 20a and nut 20b on each side of the flange sealing structure.

[0029] Specifically, combined with the above embodiments, in this embodiment, the sample stage 10 can use the flange sealing principle to seal the metal sample. In this embodiment, the sample stage 10 includes a flange sealing structure, and when actually sealing the metal sample, the gasket 18 and the metal sample 21 can be sequentially placed on the knife-edge flange 17 first, then the cover plate 19 is covered, and then the bolts 20a and nuts 20b on both sides are tightened. By pressing with the bolts 20a, the knife edge of the knife-edge flange 17 is embedded into the sealing gasket 18, thereby forming a tight sealing structure.

[0030] Combined with Figure 1As shown, in one of the alternative embodiments, the vacuum pump set 3 is a molecular pump set, and the isolator 7 is a ceramic isolator.

[0031] Specifically, in combination with the above embodiments, in this embodiment, the vacuum pump set 3 can be a molecular pump set, that is, the interior of the permeation pipeline 8 is evacuated by the molecular pump set, and the isolator 7 can be a ceramic isolator (as Figure 3 shown), that is, the electrical connection between the metal sample on the sample stage 10 and the device is interrupted by the ceramic isolator.

[0032] It can be understood that in addition to the molecular pump set and the ceramic isolator, the vacuum pump set 3 can also use other pump sets with a vacuum pumping function, and the isolator 7 can also use other isolation devices with an isolation function. The embodiments of the present invention do not make specific limitations.

[0033] Combined with Figure 1 As shown, in one of the alternative embodiments, the plasma source 14 is a microwave plasma source, a radio frequency plasma source, or a hot cathode plasma source.

[0034] Specifically, in combination with the above embodiments, in this embodiment, the plasma source 14 can be a microwave plasma source, a radio frequency plasma source, or a hot cathode plasma source, corresponding to generating microwave plasma, radio frequency plasma, or hot cathode plasma.

[0035] It can be understood that in addition to the microwave plasma source, the radio frequency plasma source, and the hot cathode plasma source, other types of plasma sources can also be used. The embodiments of the present invention do not make specific limitations.

[0036] The embodiments of the present invention also provide a usage method of a hydrogen isotope permeation amount measuring device, which is applied to the hydrogen isotope permeation amount measuring device described in any of the above embodiments, including: Seal and fix the metal sample on the sample stage; Close the first vacuum valve, open the second vacuum valve, and evacuate the permeation pipeline using the vacuum pump set; When the vacuum degree in the permeation pipeline reaches a preset vacuum degree threshold, turn on the mass spectrometer and start the hydrogen isotope permeation experiment; wherein, the permeation experiment includes: heating the metal sample using a heater, applying a bias voltage to the metal sample using a bias power supply, and opening the hydrogen gas cylinder and the plasma source, and bombarding the metal sample with the generated plasma; After the permeation experiment ends, open the first vacuum valve, close the second vacuum valve, open the standard leak hole, and record the steady-state current value of the mass spectrometer at the current sample temperature and the current ion incident energy; Obtain the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation conditions based on the standard leak rate of the standard leak hole, the steady-state calibration current value of the mass spectrometer, and the steady-state current value.

[0037] Specifically, in combination with Figure 1 and the above embodiments, in this embodiment, the metal sample can be first sealed and fixed on the sample stage 10 of the device. Then, close the first vacuum valve 4 to block the channels between the standard leak hole 2 and the mass spectrometer 1, the vacuum pump group 3, and the permeation pipeline 8. Open the second vacuum valve 5 to connect the channels between the permeation pipeline 8 and the mass spectrometer 1 and the vacuum pump group 3, and use the vacuum pump group 3 to evacuate the permeation pipeline 8 until the vacuum degree in the permeation pipeline 8 reaches a preset vacuum degree threshold. For example, when the vacuum degree reaches 10 -5 Pa, turn on the mass spectrometer 1 and start the hydrogen isotope permeation experiment, that is: use the heater 9 to heat the metal sample on the sample stage 10, use the thermocouple 12 to measure the sample temperature of the metal sample on the sample stage 10, and use the temperature recorder 13 to record the measured temperature value in real time. Also, use the bias power supply 11 to apply a bias voltage to the metal sample on the sample stage 10, open the hydrogen gas cylinder 15 to introduce hydrogen gas into the plasma discharge chamber 6, turn on the plasma source 14 to generate plasma 16, and use the generated plasma 16 to bombard the metal sample on the sample stage 10 until the permeation amount of hydrogen isotopes reaches a steady state, then end the hydrogen isotope permeation experiment, that is: close the second vacuum valve 5 to block the channels between the permeation pipeline 8 and the mass spectrometer 1 and the vacuum pump group 3, open the first vacuum valve 4 to connect the channels between the standard leak hole 2 and the mass spectrometer 1 and the vacuum pump group 3, and open the standard leak hole 2, and record the steady-state current value of the mass spectrometer 1 at the current sample temperature and the current ion incident energy; finally, based on the standard leak rate of the standard leak hole 2, the steady-state calibration current value and the steady-state current value of the mass spectrometer 1, obtain the steady-state permeation amount of hydrogen isotopes passing through the metal sample on the sample stage 10 under plasma irradiation conditions.

[0038] It should be noted that the signal current value of the mass spectrometer 1 is proportional to the permeation amount of hydrogen isotopes. By using the proportional relationship between the steady-state current value of the mass spectrometer 1 under plasma irradiation conditions and the steady-state calibration current value of the mass spectrometer 1, combined with the standard leak rate of the standard leak hole 2, the steady-state permeation amount of hydrogen isotopes passing through the metal sample on the sample stage 10 under plasma irradiation conditions can be calculated.

[0039] In one alternative embodiment, the method further includes: Record in real time the permeation change state of hydrogen isotopes during the permeation experiment; Judge whether the stable permeation state is reached according to the permeation change state; When it is determined that the stable penetration state is reached, the penetration experiment is terminated.

[0040] Specifically, in combination with the above embodiments, during the hydrogen isotope penetration experiment of this embodiment, a mass spectrometer 1 can also be used to record in real time the penetration change state of the hydrogen isotope passing through the metal sample during the entire hydrogen isotope penetration experiment, so as to judge whether the penetration amount of the hydrogen isotope reaches a steady state according to the penetration change state of the hydrogen isotope. If it is determined according to the penetration change state of the hydrogen isotope that the penetration amount of the hydrogen isotope does not reach a steady state, the hydrogen isotope penetration experiment continues; if it is determined according to the penetration change state of the hydrogen isotope that the penetration amount of the hydrogen isotope reaches a steady state, the hydrogen isotope penetration experiment is terminated.

[0041] Exemplarily, referring to Figure 4 As shown, it is a deuterium penetration amount curve graph of a martensitic steel provided by an embodiment of the present invention. Among them, the metal sample is martensitic steel, and the thickness of the metal sample is 0.75 mm. A heater 9 is used to heat the martensitic steel on the sample stage 10 so that the sample temperature of the martensitic steel reaches 256 °C. A bias voltage is applied to the martensitic steel on the sample stage 10 by a bias voltage power supply 11 so that the ion incident energy is 15 eV, and a mass spectrometer 1 is used to record in real time the penetration change state of deuterium passing through the martensitic steel from the start of the hydrogen isotope penetration experiment. The corresponding change curve graph of the deuterium penetration amount passing through the martensitic steel with a thickness of 0.75 mm at a sample temperature of 256 °C and an ion incident energy of 15 eV is as Figure 4 shown, and Figure 4 the abscissa of which is time (unit: s), and the ordinate is the deuterium penetration flux (i.e., the deuterium penetration amount, unit: atoms / (m 2 ·s)); According to Figure 4 it can be seen that with the change of the experimental time, the deuterium penetration amount passing through the martensitic steel will increase rapidly at first, but finally reach a stable state and basically no longer change. At this time, the hydrogen isotope penetration experiment can be terminated, and the steady-state penetration amount of deuterium passing through the martensitic steel under plasma irradiation conditions can be measured.

[0042] In one optional embodiment, the obtaining of the steady-state penetration amount of the hydrogen isotope passing through the metal sample under plasma irradiation conditions according to the standard leak rate of the standard leak hole, the steady-state calibration current value of the mass spectrometer, and the steady-state current value specifically includes: According to the formula calculate to obtain the steady-state penetration amount of the hydrogen isotope passing through the metal sample under plasma irradiation conditions; where J ∞ is the steady-state penetration amount, S calib is the standard leak rate of the standard leak hole, A is the effective penetration area of the metal sample, I ∞is the steady-state current value, I calib is the steady-state calibration current value of the mass spectrometer.

[0043] Specifically, in combination with the above embodiments, in this embodiment, when obtaining the steady-state permeation amount of hydrogen isotopes through the metal sample on the sample stage 10 under plasma irradiation conditions according to the standard leak rate of the standard leak orifice 2, the steady-state calibration current value and the steady-state current value of the mass spectrometer 1, the steady-state permeation amount J of hydrogen isotopes through the metal sample on the sample stage 10 under plasma irradiation conditions can be directly calculated according to the following formula ∞ (in units of atoms per square meter per second, i.e., atoms / (m 2 ·s)): ; where S calib represents the standard leak rate of the standard leak orifice 2 (in units of molecules per second, i.e., molecules / s), A represents the effective permeation area of the metal sample (in units of square meters, i.e., m 2 ), I ∞ represents the steady-state current value (in units of amperes, i.e., A) recorded by the mass spectrometer 1 after the hydrogen isotope permeation experiment is completed at the current sample temperature and the current ion incident energy, and I calib represents the steady-state calibration current value of the mass spectrometer 1 (in units of amperes, i.e., A).

[0044] In one alternative embodiment, the method further includes: Adjusting the sample temperature of the metal sample using the heater to measure the steady-state permeation amount of hydrogen isotopes at different sample temperatures.

[0045] Specifically, in combination with the above embodiments, in this embodiment, the heater 9 can be used to heat the metal sample to change the sample temperature of the metal sample, so as to measure the steady-state permeation amount of hydrogen isotopes through the metal sample at different sample temperatures.

[0046] It should be noted that the steady-state permeation amount of hydrogen isotopes at a certain determined sample temperature and a determined ion incident energy can be measured in each hydrogen isotope permeation experiment. Then, the hydrogen isotope permeation experiment can be repeated multiple times, and in each hydrogen isotope permeation experiment, the heater 9 is used to change the metal sample to different sample temperatures. At this time, the ion incident energy remains unchanged, and the steady-state permeation amounts of hydrogen isotopes at different sample temperatures under the same ion incident energy can be correspondingly obtained, so as to obtain the dependence relationship between the permeation amount of hydrogen isotopes and the sample temperature.

[0047] In one alternative embodiment, the method further includes: Adjust the ion incident energy of the plasma by using the bias power supply to measure the steady-state permeation amount of hydrogen isotopes at different ion incident energies.

[0048] Specifically, in combination with the above embodiments, in this embodiment, the bias power supply 11 can be used to change the magnitude of the bias voltage applied to the metal sample, so as to change the ion incident energy of the plasma 16, thereby measuring the steady-state permeation amount of hydrogen isotopes passing through the metal sample at different ion incident energies.

[0049] It should be noted that in each hydrogen isotope permeation experiment, the steady-state permeation amount of hydrogen isotopes at a certain determined sample temperature and determined ion incident energy can be measured. Then, the hydrogen isotope permeation experiment can be repeated multiple times. And in each hydrogen isotope permeation experiment, the ion incident energy is changed by using the bias power supply 11. At this time, the sample temperature remains unchanged, and the steady-state permeation amounts of hydrogen isotopes at the same sample temperature and different ion incident energies are correspondingly obtained, so that the dependence relationship between the permeation amount of hydrogen isotopes and the ion incident energy can be obtained.

[0050] It can be understood that for the sample temperature and the ion incident energy, in each hydrogen isotope permeation experiment, only the sample temperature or only the ion incident energy can be changed, or both the sample temperature and the ion incident energy can be changed simultaneously. The embodiments of the present invention do not make specific limitations.

[0051] In summary, a measurement device for hydrogen isotope permeation amount and its usage method provided by the embodiments of the present invention. The device includes a mass spectrometer, a standard leak, a vacuum pump group, a first vacuum valve, a second vacuum valve, a plasma discharge chamber, a bias power supply, a thermocouple, a temperature recorder, a plasma source, and a hydrogen gas cylinder. The plasma discharge chamber includes an isolator, a permeation pipeline, a heater, and a sample stage. The usage method applied to the device includes: sealing and fixing a metal sample on the sample stage; closing the first vacuum valve and opening the second vacuum valve, and using the vacuum pump group to evacuate the permeation pipeline; when the vacuum degree in the permeation pipeline reaches a preset vacuum degree threshold, opening the mass spectrometer and starting the hydrogen isotope permeation experiment, that is, heating the metal sample using the heater, applying a bias voltage to the metal sample using the bias power supply, and opening the hydrogen gas cylinder and the plasma source, and bombarding the metal sample with the generated plasma; after the permeation experiment is completed, opening the first vacuum valve, closing the second vacuum valve, opening the standard leak, and recording the steady-state current value of the mass spectrometer at the current sample temperature and the current ion incident energy; according to the standard leak rate of the standard leak, the steady-state calibration current value and the steady-state current value of the mass spectrometer, obtaining the steady-state permeation amount of hydrogen isotope passing through the metal sample under plasma irradiation conditions. The embodiments of the present invention can simply and conveniently realize the real-time measurement of the permeation amount of hydrogen isotope passing through the metal sample under plasma irradiation conditions, can conveniently change the sample temperature and the ion incident energy, and can also work stably for a long time, making it not restricted by the experimental conditions and operation time of large scientific devices such as tokamaks.

[0052] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the technical principle of the present invention, several improvements and deformations can be made, and these improvements and deformations should also be regarded as the protection scope of the present invention.

Claims

1. A measuring device for the permeation amount of hydrogen isotopes, characterized in that, Used to measure the permeation amount of hydrogen isotopes through a metal sample under plasma irradiation conditions, including: a mass spectrometer, a standard leak hole, a vacuum pump set, a first vacuum valve, a second vacuum valve, a plasma discharge chamber, a bias power supply, a thermocouple, a temperature recorder, a plasma source, and a hydrogen gas cylinder; inside the plasma discharge chamber, there are an isolator, a permeation pipeline, a heater, and a sample stage, and the sample stage is used to seal and fix the metal sample; One end of the isolator is communicated with the sample stage through the permeation pipeline; the heater is arranged inside the permeation pipeline and keeps a preset distance from the sample stage; the outlet of the plasma source and the outlet of the hydrogen gas cylinder are both communicated with the plasma discharge chamber; the bias power supply is connected between the outer shell of the plasma discharge chamber and the sample stage; the thermocouple is connected between the sample stage and the temperature recorder; The other end of the isolator is communicated with the mass spectrometer through a first pipeline, communicated with the standard leak hole through a second pipeline, and communicated with the vacuum pump set through a third pipeline, and the ends of the first pipeline, the second pipeline, and the third pipeline close to the isolator converge into one path and then dock to the other end of the isolator; the first vacuum valve is arranged at one end of the second pipeline close to the standard leak hole; the second vacuum valve is arranged at one end of the converged pipeline close to the isolator.

2. The measuring device for the hydrogen isotope permeation amount according to claim 1, wherein The positive pole of the bias power supply is connected to the outer shell of the plasma discharge chamber, the negative pole of the bias power supply is connected to the sample stage, and the outer shell of the plasma discharge chamber is grounded.

3. The measuring device for the permeation amount of hydrogen isotopes according to claim 1, characterized in that, The sample stage includes a flange sealing structure, and the flange sealing structure includes a knife-edge flange, a gasket, a cover plate, and a fastener.

4. The measuring device for the hydrogen isotope permeation amount according to claim 1, wherein The vacuum pump set is a molecular pump set, and the isolator is a ceramic isolator.

5. The measuring device for the permeation amount of hydrogen isotopes according to claim 1, characterized in that, The plasma source is a microwave plasma source, a radio frequency plasma source, or a hot cathode plasma source.

6. A method for using a measuring device for the permeation amount of hydrogen isotopes, characterized in that, Applied to the measuring device for the permeation amount of hydrogen isotopes as described in any one of claims 1 to 5, including: Seal and fix the metal sample on the sample stage; Close the first vacuum valve, open the second vacuum valve, and use the vacuum pump set to evacuate the permeation pipeline; When the vacuum degree inside the permeation pipeline reaches a preset vacuum degree threshold, turn on the mass spectrometer and start the hydrogen isotope permeation experiment; wherein, the permeation experiment includes: heating the metal sample with the heater, applying a bias voltage to the metal sample with the bias power supply, opening the hydrogen gas cylinder and the plasma source, and bombarding the metal sample with the generated plasma; After the permeation experiment ends, open the first vacuum valve, close the second vacuum valve, open the standard leak hole, and record the steady-state current value of the mass spectrometer at the current sample temperature and the current ion incident energy; According to the standard leak rate of the standard leak hole, the steady-state calibration current value of the mass spectrometer, and the steady-state current value, obtain the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation conditions.

7. The method for using the measuring device for hydrogen isotope permeation amount according to claim 6, characterized in that, The method further includes: Real-time record the permeation change state of hydrogen isotopes during the permeation experiment; Judge whether the stable permeation state is reached according to the permeation change state; When it is determined that the stable permeation state is reached, end the permeation experiment.

8. The method for using the measuring device for hydrogen isotope permeation amount according to claim 6, characterized in that, The method for obtaining the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation according to the standard leakage rate of the standard leak hole, the steady-state calibration current value of the mass spectrometer, and the steady-state current value specifically includes: According to the formula calculate the steady-state permeation amount of hydrogen isotopes passing through the metal sample under plasma irradiation conditions; wherein, J ∞ is the steady-state permeation amount, S calib is the standard leak rate of the standard leak hole, A is the effective permeation area of the metal sample, I ∞ is the steady-state current value, I calib is the steady-state calibration current value of the mass spectrometer.

9. The method for using the measuring device for hydrogen isotope permeation amount according to claim 6, characterized in that The method further includes: Adjust the sample temperature of the metal sample by using the heater to measure the steady-state permeation amount of hydrogen isotopes at different sample temperatures.

10. The method for using the measuring device for hydrogen isotope permeation amount according to claim 6, characterized in that The method further includes: Adjust the ion incident energy of the plasma by using the bias power supply to measure the steady-state permeation amount of hydrogen isotopes at different ion incident energies.

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