CN108204938A - Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating - Google Patents
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating Download PDFInfo
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- CN108204938A CN108204938A CN201611186849.8A CN201611186849A CN108204938A CN 108204938 A CN108204938 A CN 108204938A CN 201611186849 A CN201611186849 A CN 201611186849A CN 108204938 A CN108204938 A CN 108204938A
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- vacuum chamber
- sample
- exterior
- sample room
- hydrogen
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 42
- 239000001257 hydrogen Substances 0.000 title claims abstract description 42
- 239000011248 coating agent Substances 0.000 title claims abstract description 26
- 238000000576 coating method Methods 0.000 title claims abstract description 26
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 26
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 25
- 238000005259 measurement Methods 0.000 title claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 10
- 230000005855 radiation Effects 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 5
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 239000000463 material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 238000011056 performance test Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000000155 isotopic effect Effects 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 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
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 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
- 239000010408 film Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000009738 saturating 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
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Measurement Of Radiation (AREA)
- Monitoring And Testing Of Nuclear Reactors (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to hydrogen measuring device, the device for accurately measuring of hydrogen scattering and permeating characteristic in more particularly to a kind of coating.Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating, including sample room, the sample room includes exterior vacuum chamber and inner vacuum chamber, sample room is connect with water cooling unit, water cooling unit is used to cool down for sample room, the inner vacuum chamber of sample room is connected by valve with inner vacuum chamber molecular pump and inner vacuum chamber mechanical pump respectively, the inner vacuum chamber molecular pump and inner vacuum chamber mechanical pump vacuumizing for inner vacuum chamber, the exterior vacuum chamber of sample room is connected by quadrupole mass spectrometer with exterior vacuum chamber's molecular pump and exterior vacuum chamber's mechanical pump respectively, exterior vacuum chamber's molecular pump and exterior vacuum chamber's mechanical pump vacuumizing for exterior vacuum chamber, quadrupole mass spectrometer is also connected with industrial personal computer and ionic pump respectively, sample room is connected by referance leak with inlet plenum.The present invention effect be：The temperature of accurate control test sample, completes the test under different temperatures.
Description
Technical field
The invention belongs to hydrogen measuring device, the device for accurately measuring of hydrogen scattering and permeating characteristic in more particularly to a kind of coating.
Background technology
Since atomic radius is smaller, hydrogen and its isotope can permeate rapidly in many materials.No matter atomic energy reacts
Heap, the storage of controllable thermonuclear reaction device or fusionable material and processing system all have that one prevents hydrogen from permeating.It is poly-
Become in heap, a large amount of components and system will all work in the environment containing tritium, and hydrogen and its isotopic osmosis are one crucial
Problem, it is related to the influence of many aspects, for example tritium efficiently uses, and the structural material mechanical performance that hydrogen, tritium are brought declines (hydrogen
Crisp problem), the safety of system operation and environmental safety etc..The solution generally acknowledged in the world at present is in structural material
Surface prepares anti-tritium diffusion layer, so not only will not structural damage material body performance, but also can reach and reduce hydrogen isotope and ooze
Saturating purpose.Therefore, the scattering and permeating performance of Study of Hydrogen and its isotope in the materials such as coating, metal has centainly important
Property and engineering value.
The method for measuring hydrogen and its isotopic osmosis common at present is mainly including electrochemical method and vapor infiltration method two
Class.The former test equipment is simple, at low cost, easy to operate, but the temperature tested by Influence of Electrolyte is relatively low, so electrochemistry side
Method is adapted to measure the material hydrogen penetrating quality in -100 DEG C of temperature ranges of room temperature.The development of gas-phase permeation method has benefited from very
The progress of empty technology, this method have become the common method for measuring hydrogen penetrating quality in material at present.Existing gas-phase permeation is surveyed
Trial assembly, which is put, is mostly integrally placed at sample room in heating unit, to achieve the purpose that heat sample, and then measures different
At a temperature of hydrogen infiltration coefficient in material.But the temperature that the heating temperature that above-mentioned heating unit thermocouple measures is stove uniform temperature zone,
And the actual temperature of sample room inner sample, there are certain deviation, system is poor to the control of temperature.Experiment shows heating up
In the case that rate is larger, thermocouple measured temperature and sample actual temperature differ dozens or even hundreds of degree Celsius.In addition, sample
Entirely in heating unit, hot environment when repeatedly long also accelerates the old of sample room and connecting pipe for room and connecting pipe
Change, shorten its service life.
Invention content
The present invention provides hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating for prior art defect.
The invention is realized in this way：Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating, should including sample room
Sample room includes exterior vacuum chamber and inner vacuum chamber, and sample room is connect with water cooling unit, and water cooling unit is used to cool down for sample room, sample room
Inner vacuum chamber connected respectively with inner vacuum chamber molecular pump and inner vacuum chamber mechanical pump by valve, the inner vacuum chamber molecular pump and
Inner vacuum chamber mechanical pump vacuumizes for inner vacuum chamber, the exterior vacuum chamber of sample room by quadrupole mass spectrometer respectively with outer vacuum
Room molecular pump is connected with exterior vacuum chamber mechanical pump, and exterior vacuum chamber's molecular pump and exterior vacuum chamber's mechanical pump are used for the pumping of exterior vacuum chamber
Vacuum, quadrupole mass spectrometer are also connected with industrial personal computer and ionic pump respectively, and sample room is connected by referance leak with inlet plenum.
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described above, wherein, the sample room it is interior
Vacuum chamber is arranged on inside exterior vacuum chamber, and inner vacuum chamber is connected by gas outlet with outside, and exterior vacuum chamber is by air inlet and outside
Portion connects, and sets sample base on inner vacuum chamber top, test sample is set on sample base, set in test sample surrounding
Induction heating apparatus, induction heating apparatus are arranged in exterior vacuum chamber.
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described above, wherein, it is also set up outside sample room
Online infrared radiation thermometer, the online infrared radiation thermometer are used to detect test sample temperature.
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described above, wherein, the sample base with
Test sample is welded.
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described above, wherein, in the side wall of exterior vacuum chamber
Upper setting water cooling plant.
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described above, wherein, in the roof of exterior vacuum chamber
Upper setting quartz observing window.
Hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described above, wherein, air inlet with hydrogen gas
Source is connected, and gas outlet is connected with quadrupole mass spectrometer.
The present invention remarkable result be：The present invention provides a kind of accurate measure to hinder hydrogen scattering and permeating performance in tritium coating
Device.Using built-in heating system, the temperature of test sample can be accurately controlled, completes the test under different temperatures；The sense of system
Heating unit is answered, is not only simple in structure, quick heating also has the advantage for making sample thermally equivalent.Built-in heating system mating one
Cooling device eliminate or reduces harmful effect of the high fever to periphery pipeline and parts, increases the steady of system as far as possible
It is qualitative, the oxidation of pipeline and parts at high temperature is prevented, extends its service life.The pedestal design that the present invention uses, both may be used
Sheet sample is tested, can also test tubulose sample.By rationally cutting, pedestal can optionally be repeated as many times and use, and ensure to survey
Testing cost is reduced on the basis of test result.
Description of the drawings
Fig. 1 is hydrogen scattering and permeating performance test device structure diagram in resistance tritium coating of the invention.
Fig. 2 is the structure sectional view for hindering hydrogen scattering and permeating performance test device sample room in tritium coating of the present invention.
In figure, 1 sample room, 2 water cooling units, 3a exterior vacuum chamber molecular pump, 3b inner vacuum chamber molecular pumps, 4a exterior vacuum chamber machinery
Pump, 4b inner vacuum chamber mechanical pumps, 5 inlet plenums, 6 referance leaks, 7 industrial personal computers, 8 quadrupole mass spectrometer, 9 ionic pumps, 10a inlet plenums are thin
Film is advised, 10b exterior vacuum chamber air inlet film rule, 11a exterior vacuum chamber vacuum gauge, 11b exterior vacuum chamber mechanical pump vacuum gauge, in 11c
Vacuum chamber ionic pump vacuum gauge, 11d inner vacuum chamber mechanical pump vacuum gauges, 12a inlet plenums connection gas cylinder, the connection of 12b exterior vacuum chamber
Hydrogen cylinder, 1-1 quartz observing windows, 1-2 test samples, 1-3 induction heating apparatuses, 1-4 air inlets, 1-5 sample bases, 1-6
Water cooling plant, 1-7 exterior vacuum chamber, 1-8 gas outlets, 1-9 inner vacuum chambers, the online infrared radiation thermometers of 1-10.
Specific embodiment
As shown in Figures 1 and 2, hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating, including sample room 1,
The sample room 1 includes exterior vacuum chamber and inner vacuum chamber, and sample room 1 is connect with water cooling unit 2, and water cooling unit 2 is used to drop for sample room 1
Temperature, the inner vacuum chamber of sample room 1 are connected by valve with inner vacuum chamber molecular pump 3b and inner vacuum chamber mechanical pump 4b respectively, this is interior
Vacuum chamber molecular pump 3b and inner vacuum chamber mechanical pump 4b vacuumizes for inner vacuum chamber, and the exterior vacuum chamber of sample room 1 passes through four
Pole mass spectrograph 8 connects respectively with exterior vacuum chamber molecular pump 3a and exterior vacuum chamber mechanical pump 4a, exterior vacuum chamber molecular pump 3a and outer
Vacuum chamber mechanical pump 4a vacuumizes for exterior vacuum chamber, and quadrupole mass spectrometer 8 is also connected with industrial personal computer 7 and ionic pump 9 respectively, sample
Product room 1 is connected by referance leak 6 with inlet plenum 5.
The inner vacuum chamber 1-9 of the sample room 1 is arranged on inside exterior vacuum chamber 1-7, and inner vacuum chamber 1-9 passes through gas outlet
1-8 is connected with outside, and exterior vacuum chamber 1-7 is connected by air inlet 1-4 with outside, and sample base is set on inner vacuum chamber 1-9 tops
Seat 1-5, sets test sample 1-2 on sample base 1-5, and induction heating apparatus 1-3, sense are set in test sample 1-2 surroundings
Heating unit 1-3 is answered to be arranged in exterior vacuum chamber 1-7.
Wire type infrared radiation thermometer 1-10 is additionally arranged at outside sample room 1, which is used to detect
Test sample temperature.
Sample base 1-5 and test sample 1-2 is welded.
Water cooling plant 1-6 is set on the side wall of exterior vacuum chamber 1-7.
Quartz observing window 1-1 is set on the roof of exterior vacuum chamber 1-7.
Air inlet 1-4 is connected with hydrogen source gas, and gas outlet 1-8 is connected with quadrupole mass spectrometer.
Apparatus of the present invention are mainly used under realization different temperatures, the diffusion permeability of hydrogen and its isotope in solid material
Matter is tested.Can test sample mainly include coating sample (sheet and tubulose), stainless steel (sheet and tubulose) and potsherd.It is described
Hydrogen scattering and permeating performance test device include one have the sample room of inside and outside vacuum chamber, the built-in heating system with cooling device,
Quadrupole mass spectrometer, referance leak, air supply system, vacuum maintain system, vacuum measurement system, pressure testing system and pipeline.
Claims (7)
1. a kind of hydrogen scattering and permeating performance measurement device in resistance tritium coating, it is characterised in that：Including sample room (1), the sample room
(1) including exterior vacuum chamber and inner vacuum chamber, sample room (1) is connect with water cooling unit (2), water cooling unit (2) for for sample room (1) drop
Temperature, the inner vacuum chamber of sample room (1) are connected by valve with inner vacuum chamber molecular pump (3b) and inner vacuum chamber mechanical pump (4b) respectively
It is logical, the inner vacuum chamber molecular pump (3b) and inner vacuum chamber mechanical pump (4b) vacuumizing for inner vacuum chamber, outside sample room (1)
Vacuum chamber is connected by quadrupole mass spectrometer (8) with exterior vacuum chamber's molecular pump (3a) and exterior vacuum chamber's mechanical pump (4a) respectively, this is outer
Vacuum chamber molecular pump (3a) and exterior vacuum chamber's mechanical pump (4a) vacuumizing for exterior vacuum chamber, quadrupole mass spectrometer (8) are also distinguished
It is connected with industrial personal computer (7) and ionic pump (9), sample room (1) is connected by referance leak (6) with inlet plenum (5).
2. hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as described in claim 1, it is characterised in that：Described
The inner vacuum chamber (1-9) of sample room (1) is arranged on exterior vacuum chamber (1-7) inside, and inner vacuum chamber (1-9) passes through gas outlet (1-8)
It is connected with outside, exterior vacuum chamber (1-7) is connected by air inlet (1-4) with outside, and sample is set on inner vacuum chamber (1-9) top
Pedestal (1-5) sets test sample (1-2) on sample base (1-5), and sensing heating is set in test sample (1-2) surrounding
Device (1-3), induction heating apparatus (1-3) are arranged in exterior vacuum chamber (1-7).
3. hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as claimed in claim 2, it is characterised in that：In sample
Wire type infrared radiation thermometer (1-10) is additionally arranged at outside room (1), the online infrared radiation thermometer (1-10) is for detecting test sample
Temperature.
4. hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as claimed in claim 3, it is characterised in that：Described
Sample base (1-5) is welded with test sample (1-2).
5. hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as claimed in claim 4, it is characterised in that：It is true outside
Water cooling plant (1-6) is set on the side wall of empty room (1-7).
6. hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as claimed in claim 5, it is characterised in that：It is true outside
Quartz observing window (1-1) is set on the roof of empty room (1-7).
7. hydrogen scattering and permeating performance measurement device in a kind of resistance tritium coating as claimed in claim 6, it is characterised in that：Air inlet
(1-4) is connected with hydrogen source gas, and gas outlet (1-8) is connected with quadrupole mass spectrometer..
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611186849.8A CN108204938B (en) | 2016-12-20 | 2016-12-20 | Hydrogen diffusion permeability measuring device in tritium-resistant coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611186849.8A CN108204938B (en) | 2016-12-20 | 2016-12-20 | Hydrogen diffusion permeability measuring device in tritium-resistant coating |
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| Publication Number | Publication Date |
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| CN108204938A true CN108204938A (en) | 2018-06-26 |
| CN108204938B CN108204938B (en) | 2020-08-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109612881A (en) * | 2018-11-15 | 2019-04-12 | 中国科学院合肥物质科学研究院 | A method of measurement fusion facility the first wall hydrogen isotope infiltration |
| CN110208311A (en) * | 2019-05-21 | 2019-09-06 | 四川大学 | Resistance tritium coating multi- scenarios method performance test methods and its test device based on accelerator ion irradiation |
| CN112485285A (en) * | 2020-11-16 | 2021-03-12 | 中国工程物理研究院核物理与化学研究所 | Thermal analysis device for helium existing state in tritium storage material |
| CN113252529A (en) * | 2021-04-30 | 2021-08-13 | 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109612881A (en) * | 2018-11-15 | 2019-04-12 | 中国科学院合肥物质科学研究院 | A method of measurement fusion facility the first wall hydrogen isotope infiltration |
| CN110208311A (en) * | 2019-05-21 | 2019-09-06 | 四川大学 | Resistance tritium coating multi- scenarios method performance test methods and its test device based on accelerator ion irradiation |
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| CN112485285A (en) * | 2020-11-16 | 2021-03-12 | 中国工程物理研究院核物理与化学研究所 | Thermal analysis device for helium existing state in tritium storage material |
| 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 |
| CN113252529A (en) * | 2021-04-30 | 2021-08-13 | 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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| CN108204938B (en) | 2020-08-21 |
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