CN108204938B - Hydrogen diffusion permeability measuring device in tritium-resistant coating - Google Patents
Hydrogen diffusion permeability measuring device in tritium-resistant coating Download PDFInfo
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- CN108204938B CN108204938B CN201611186849.8A CN201611186849A CN108204938B CN 108204938 B CN108204938 B CN 108204938B CN 201611186849 A CN201611186849 A CN 201611186849A CN 108204938 B CN108204938 B CN 108204938B
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 34
- 239000001257 hydrogen Substances 0.000 title claims abstract description 34
- 238000009792 diffusion process Methods 0.000 title claims abstract description 22
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 20
- 238000000576 coating method Methods 0.000 title claims abstract description 20
- 150000002431 hydrogen Chemical class 0.000 title claims abstract description 20
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 20
- 239000011248 coating agent Substances 0.000 title claims abstract description 19
- 230000035699 permeability Effects 0.000 title claims abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 108010083687 Ion Pumps Proteins 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 9
- 230000006698 induction Effects 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000004888 barrier function Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 4
- 238000002848 electrochemical method Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000001171 gas-phase infiltration Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/0806—Details, e.g. sample holders, mounting samples for testing
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Measurement Of Radiation (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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Abstract
The invention belongs to a hydrogen measuring device, and particularly relates to an accurate measuring device for hydrogen diffusion permeability characteristics in a coating. A device for measuring the hydrogen diffusion permeability of a tritium-resistant coating comprises a sample chamber, wherein the sample chamber comprises an outer vacuum chamber and an inner vacuum chamber, the sample chamber is connected with a water cooling machine, the water cooling machine is used for cooling the sample chamber, the inner vacuum chamber of the sample chamber is respectively communicated with an inner vacuum chamber molecular pump and an inner vacuum chamber mechanical pump through valves, the inner vacuum chamber molecular pump and the inner vacuum chamber mechanical pump are used for vacuumizing the inner vacuum chamber, the outer vacuum chamber of the sample chamber is respectively communicated with the outer vacuum chamber molecular pump and the outer vacuum chamber mechanical pump through a quadrupole mass spectrometer, the outer vacuum chamber molecular pump and the outer vacuum chamber mechanical pump are used for vacuumizing the outer vacuum chamber, the quadrupole mass spectrometer is also respectively communicated with an industrial personal computer and an ion pump, and the sample chamber is. The invention has the following effects: and (4) accurately controlling the temperature of the test sample to finish tests at different temperatures.
Description
Technical Field
The invention belongs to a hydrogen measuring device, and particularly relates to an accurate measuring device for hydrogen diffusion permeability characteristics in a coating.
Background
Hydrogen and its isotopes, due to the small atomic radius, are rapidly permeable in many materials. There is a problem with preventing hydrogen permeation in either nuclear reactors, controlled thermal nuclear reactors, or thermal nuclear fuel storage and handling systems. In a fusion reactor, a large number of components and systems work in a tritium-containing environment, and permeation of hydrogen and isotopes thereof is a crucial problem and relates to influences in multiple aspects, such as effective utilization of tritium, reduction of mechanical properties of structural materials caused by hydrogen and tritium (hydrogen embrittlement problem), safety of system operation, environmental safety and the like. At present, the internationally accepted solution is to prepare a tritium-proof permeation layer on the surface of a structural material, so that the performance of the structural material is not damaged, and the purpose of reducing the permeation of hydrogen isotopes is achieved. Therefore, research on the diffusion and permeation performance of hydrogen and isotopes thereof in materials such as coatings and metals has certain importance and engineering value.
The current common methods for measuring hydrogen and its isotope infiltration mainly include two types of electrochemical methods and gas phase infiltration methods. The former has simple test equipment, low cost and simple operation, but the test temperature influenced by the electrolyte is lower, so the electrochemical method is suitable for measuring the hydrogen permeability of the material within the temperature range of room temperature to 100 ℃. The development of the vapor phase permeation method, which has been the current common method for measuring hydrogen permeability in materials, has benefited from the advancement of vacuum technology. Most of the existing gas phase permeation testing devices are used for integrally placing a sample chamber in a heating device so as to achieve the purpose of heating the sample and further measure the hydrogen permeation coefficient of materials at different temperatures. However, the heating temperature measured by the thermocouple of the heating device is the temperature of the uniform temperature area of the furnace, and has a certain deviation with the actual temperature of the sample in the sample chamber, so that the system has poor temperature control. Experiments show that under the condition of large heating rate, the difference between the measured temperature of the thermocouple and the actual temperature of the sample is dozens of degrees centigrade or even hundreds of degrees centigrade. In addition, the sample chamber and the connecting pipeline are wholly arranged in the heating device, the aging of the sample chamber and the connecting pipeline is accelerated under the high-temperature environment for a plurality of times, and the service life of the sample chamber and the connecting pipeline is shortened.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device for measuring the hydrogen diffusion permeability in a tritium-resistant coating.
The invention is realized by the following steps: a device for measuring the hydrogen diffusion permeability of a tritium-resistant coating comprises a sample chamber, wherein the sample chamber comprises an outer vacuum chamber and an inner vacuum chamber, the sample chamber is connected with a water cooling machine, the water cooling machine is used for cooling the sample chamber, the inner vacuum chamber of the sample chamber is respectively communicated with an inner vacuum chamber molecular pump and an inner vacuum chamber mechanical pump through valves, the inner vacuum chamber molecular pump and the inner vacuum chamber mechanical pump are used for vacuumizing the inner vacuum chamber, the outer vacuum chamber of the sample chamber is respectively communicated with the outer vacuum chamber molecular pump and the outer vacuum chamber mechanical pump through a quadrupole mass spectrometer, the outer vacuum chamber molecular pump and the outer vacuum chamber mechanical pump are used for vacuumizing the outer vacuum chamber, the quadrupole mass spectrometer is also respectively communicated with an industrial personal computer and an ion pump, and the sample chamber is.
The device for measuring the hydrogen diffusion permeability of the tritium-resistant coating is characterized in that the inner vacuum chamber of the sample chamber is arranged inside the outer vacuum chamber, the inner vacuum chamber is communicated with the outside through the air outlet, the outer vacuum chamber is communicated with the outside through the air inlet, the top end of the inner vacuum chamber is provided with the sample base, the sample is arranged on the sample base, the periphery of the test sample is provided with the induction heating devices, and the induction heating devices are arranged in the outer vacuum chamber.
According to the device for measuring the hydrogen diffusion and permeability in the tritium-resistant coating, an online infrared thermometer is further arranged outside the sample chamber and used for detecting the temperature of the sample to be tested.
The device for measuring the hydrogen diffusion and permeation performance of the tritium-resistant coating is characterized in that the sample base is welded with the test sample.
The device for measuring the hydrogen diffusion and permeation performance in the tritium-resistant coating is characterized in that a water cooling device is arranged on the side wall of the outer vacuum chamber.
The device for measuring the hydrogen diffusion and permeation performance of the tritium-resistant coating is characterized in that a quartz observation window is arranged on the top wall of the outer vacuum chamber.
The device for measuring the hydrogen diffusion permeability of the tritium-resistant coating is characterized in that the gas inlet is connected with a hydrogen gas source, and the gas outlet is connected with a quadrupole mass spectrometer.
The invention has the following remarkable effects: the invention provides a device for accurately measuring hydrogen diffusion permeability in a tritium-resistant coating. The built-in heating system is adopted, so that the temperature of a test sample can be accurately controlled, and tests at different temperatures are completed; the induction heating device of the system has the advantages of simple structure, quick temperature rise and uniform heating of the sample. The built-in heating system is matched with a cooling device, so that the adverse effect of high heat on peripheral pipelines and parts is eliminated or reduced as much as possible, the stability of the system is improved, the pipelines and the parts are prevented from being oxidized at high temperature, and the service life of the system is prolonged. The base design adopted by the invention can test not only sheet samples, but also tubular samples. Through reasonable cutting, the base can be used repeatedly according to the situation, and the test cost is reduced on the basis of ensuring the test result.
Drawings
FIG. 1 is a schematic structural diagram of a device for testing hydrogen diffusion and permeation performance in a tritium-resistant coating.
FIG. 2 is a structural sectional view of a sample chamber of the device for testing the hydrogen diffusion permeability in the tritium-resistant coating.
In the figure, a sample chamber 1, a water cooling machine 2, a molecular pump of an outer vacuum chamber 3a, a molecular pump of an inner vacuum chamber 3b, a mechanical pump of an outer vacuum chamber 4a, a mechanical pump of an inner vacuum chamber 4b, an air inlet chamber 5, a standard leak hole 6, an industrial personal computer 7, a quadrupole mass spectrometer 8, a 9 ion pump, a film gauge of an air inlet chamber 10a, a film gauge of an air inlet chamber of an outer vacuum chamber 10b, a vacuum gauge of an outer vacuum chamber 11a, a mechanical pump vacuum gauge of an outer vacuum chamber 11b, an ion pump vacuum gauge of an inner vacuum chamber 11c, a mechanical pump vacuum gauge of an inner vacuum chamber 11d, an air inlet chamber connected with a gas cylinder 12a, an outer vacuum chamber connected with a hydrogen gas cylinder 12b, a quartz observation window 1-1, a test sample 1-2, an induction heating device 1-3, an air inlet 1-4, a sample base 1-5, a water cooling device 1-6.
Detailed Description
As shown in attached figures 1 and 2, the device for measuring the hydrogen diffusion permeability of the tritium-resistant coating comprises a sample chamber 1, the sample room 1 comprises an outer vacuum room and an inner vacuum room, the sample room 1 is connected with a water cooling machine 2, the water cooling machine 2 is used for cooling the sample room 1, the inner vacuum room of the sample room 1 is respectively communicated with a molecular pump 3b of the inner vacuum room and a mechanical pump 4b of the inner vacuum room through valves, the inner vacuum chamber molecular pump 3b and the inner vacuum chamber mechanical pump 4b are used for vacuumizing the inner vacuum chamber, the outer vacuum chamber of the sample chamber 1 is respectively communicated with the outer vacuum chamber molecular pump 3a and the outer vacuum chamber mechanical pump 4a through a quadrupole mass spectrometer 8, the outer vacuum chamber molecular pump 3a and the outer vacuum chamber mechanical pump 4a are used for vacuumizing the outer vacuum chamber, the quadrupole mass spectrometer 8 is also respectively communicated with an industrial personal computer 7 and an ion pump 9, and the sample chamber 1 is communicated with the air inlet chamber 5 through a standard leak hole 6.
The device comprises a sample chamber 1, an inner vacuum chamber 1-9, an outer vacuum chamber 1-7, a sample base 1-5, an induction heating device 1-3, an air inlet 1-4, a sample base 1-5, a test sample 1-2, an induction heating device 1-3, an air outlet 1-8, an air inlet 1-4, a sample base 1-9, an air inlet 1-7, an air outlet 1-7, an air inlet 1-4, an air outlet 1-7, a sample base 1-9, an air inlet 1-3, an air inlet 1-2, an air inlet 1-3, an air outlet.
An online infrared thermometer 1-10 is also arranged outside the sample chamber 1, and the online infrared thermometer 1-10 is used for detecting the temperature of the test sample.
The sample base 1-5 is welded to the test sample 1-2.
The side wall of the outer vacuum chamber 1-7 is provided with a water cooling device 1-6.
A quartz observation window 1-1 is arranged on the top wall of the outer vacuum chamber 1-7.
The gas inlet 1-4 is connected with a hydrogen gas source, and the gas outlet 1-8 is connected with a quadrupole mass spectrometer.
The device is mainly used for realizing the diffusion and permeation property test of hydrogen and isotopes thereof in solid materials at different temperatures. The testable samples included mainly coated test specimens (sheet and tube), stainless steel (sheet and tube) and ceramic sheets. The hydrogen diffusion permeability testing device comprises a sample chamber with an inner vacuum chamber and an outer vacuum chamber, a built-in heating system with a cooling device, a quadrupole mass spectrometer, a standard leak hole, a gas supply system, a vacuum maintaining system, a vacuum measuring system, a pressure testing system and a pipeline.
Claims (2)
1. The utility model provides a hinder hydrogen diffusion permeability survey device in tritium coating which characterized in that: comprises a sample chamber (1), the sample chamber (1) comprises an outer vacuum chamber and an inner vacuum chamber, the sample chamber (1) is connected with a water cooling machine (2), the water cooling machine (2) is used for cooling the sample chamber (1), the inner vacuum chamber of the sample chamber (1) is respectively communicated with an inner vacuum chamber molecular pump (3b) and an inner vacuum chamber mechanical pump (4b) through valves, the inner vacuum chamber molecular pump (3b) and the inner vacuum chamber mechanical pump (4b) are used for vacuumizing the inner vacuum chamber, the outer vacuum chamber of the sample chamber (1) is respectively communicated with the outer vacuum chamber molecular pump (3a) and the outer vacuum chamber mechanical pump (4a) through a quadrupole mass spectrometer (8), the outer vacuum chamber molecular pump (3a) and the outer vacuum chamber mechanical pump (4a) are used for vacuumizing the outer vacuum chamber, the quadrupole mass spectrometer (8) is also respectively communicated with an industrial personal computer (7) and an ion pump (9), and the sample chamber (1) is communicated with the air inlet chamber (5) through a standard leak hole (6);
an inner vacuum chamber (1-9) of the sample chamber (1) is arranged inside an outer vacuum chamber (1-7), the inner vacuum chamber (1-9) is communicated with the outside through an air outlet (1-8), the outer vacuum chamber (1-7) is communicated with the outside through an air inlet (1-4), a sample base (1-5) is arranged at the top end of the inner vacuum chamber (1-9), a test sample (1-2) is arranged on the sample base (1-5), induction heating devices (1-3) are arranged around the test sample (1-2), and the induction heating devices (1-3) are arranged in the outer vacuum chamber (1-7);
an online infrared thermometer (1-10) is arranged outside the sample chamber (1), and the online infrared thermometer (1-10) is used for detecting the temperature of the test sample;
the sample base (1-5) is welded with the test sample (1-2);
a water cooling device (1-6) is arranged on the side wall of the outer vacuum chamber (1-7);
a quartz observation window (1-1) is arranged on the top wall of the outer vacuum chamber (1-7).
2. A device for measuring hydrogen diffusion permeability in a tritium barrier coating as claimed in claim 1, wherein: the gas inlet (1-4) is connected with a hydrogen gas source, and the gas outlet (1-8) is connected with a quadrupole mass spectrometer.
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| CN201611186849.8A CN108204938B (en) | 2016-12-20 | 2016-12-20 | Hydrogen diffusion permeability measuring device in tritium-resistant coating |
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| CN201611186849.8A CN108204938B (en) | 2016-12-20 | 2016-12-20 | Hydrogen diffusion permeability measuring device in tritium-resistant coating |
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| CN108204938B true CN108204938B (en) | 2020-08-21 |
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| CN109612881B (en) * | 2018-11-15 | 2022-03-25 | 中国科学院合肥物质科学研究院 | Method for measuring hydrogen isotope permeation of first wall of fusion device |
| CN110208311B (en) * | 2019-05-21 | 2021-06-08 | 四川大学 | Tritium-resistant coating multi-field coupling performance test method and test device based on accelerator ion irradiation |
| CN112485285B (en) * | 2020-11-16 | 2023-09-19 | 中国工程物理研究院核物理与化学研究所 | Thermal analysis device for existence state of helium in tritium storage material |
| CN113252529B (en) * | 2021-04-30 | 2022-12-20 | 核工业西南物理研究院 | High-temperature gas-driven penetration testing system and method for metal pipe fitting |
| CN115343391A (en) * | 2022-08-23 | 2022-11-15 | 中国原子能科学研究院 | System and method for chromatographic analysis of isotopic gas components |
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