CN219758022U - Hydrogen permeability testing device for solid detection material - Google Patents
Hydrogen permeability testing device for solid detection material Download PDFInfo
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- CN219758022U CN219758022U CN202321204123.8U CN202321204123U CN219758022U CN 219758022 U CN219758022 U CN 219758022U CN 202321204123 U CN202321204123 U CN 202321204123U CN 219758022 U CN219758022 U CN 219758022U
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000001257 hydrogen Substances 0.000 title claims abstract description 108
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 108
- 239000000463 material Substances 0.000 title claims abstract description 74
- 238000001514 detection method Methods 0.000 title claims abstract description 73
- 238000012360 testing method Methods 0.000 title claims abstract description 50
- 230000035699 permeability Effects 0.000 title claims abstract description 39
- 239000007787 solid Substances 0.000 title claims abstract description 24
- 239000012159 carrier gas Substances 0.000 claims abstract description 65
- 239000007789 gas Substances 0.000 claims abstract description 61
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims description 24
- 230000000087 stabilizing effect Effects 0.000 claims description 24
- 238000000034 method Methods 0.000 abstract description 36
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 13
- 239000000523 sample Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000007769 metal material Substances 0.000 description 7
- 238000011282 treatment Methods 0.000 description 7
- 238000003860 storage Methods 0.000 description 6
- 239000000306 component Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
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- 239000002985 plastic film Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000010325 electrochemical charging Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012533 medium component Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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Abstract
The utility model relates to the technical field of gas detection devices and discloses a hydrogen permeability testing device for a solid detection material, which comprises an incubator, a hydrogen conveying part for conveying hydrogen, a carrier gas conveying part for conveying carrier gas, a gas content measuring instrument for detecting the concentration of the hydrogen and a heat exchanger for adjusting the gas temperature, wherein a clamping tool for clamping a hollow cylinder of the detection material is arranged in the incubator, and the hydrogen conveying part, the carrier gas conveying part and the gas content measuring instrument are all arranged outside the incubator. The hydrogen permeability testing device of the solid detection material has the advantages of simple structure, simple and convenient operation method and higher testing precision.
Description
Technical Field
The utility model relates to the technical field of gas detection devices, in particular to a hydrogen permeability testing device and a hydrogen permeability testing method of a solid detection material.
Background
Hydrogen is widely used in petrochemical industry, electronics, metallurgy and other industries as an energy carrier and a chemical raw material, and clean hydrogen is prepared from new energy hydrogen production or fossil raw materials with carbon dioxide recovery, so that the hydrogen is an important way for realizing energy structure transformation and coping with climate change. The safe, reliable and economic storage and transportation of hydrogen in a hydrogen energy production chain is a main obstacle for large-scale application of hydrogen energy, and the main storage modes of the hydrogen energy which are realized in industrial popularization and application at present are high-pressure gas storage and liquefaction storage. Because the hydrogen molecule volume is very small, the diameter is only about 0.2nm, the hydrogen molecule has very strong penetrating power and diffusion power, and the difficulty and the potential safety hazard of hydrogen storage are increased, so that the hydrogen permeation characteristic of the material is one of the main limiting factors of hydrogen energy safe storage.
The existing devices and methods for detecting the permeability of hydrogen in a material to be detected are mainly based on electrochemical technology methods or pressure difference methods and mainly aim at metal materials.
The patent "device and method for measuring hydrogen permeability of metal" (CN 201010185642) proposes a method for measuring hydrogen permeability of metal sample by electrochemical technology, but it is necessary to perform surface polishing treatment, cathodic treatment, single-sided electroplating and other treatments on the metal sample, the procedure is complex, and the measurement result is greatly affected by the quality level of the sample surface treatment.
The patent 'a device for testing hydrogen permeability of metal materials and a using method thereof' (CN 201710061815) discloses a testing device, wherein a hydrogen receiving chamber and an electrochemical charging chamber are connected through a communicating body provided with a sample through a clamp, and the structure reduces the component bonding procedure and improves the tightness.
Patent "observation object gas permeation diffusion path observation device and observation object gas measurement method, point defect position detection device and point defect position detection method, and observation sample" (CN 202180017533.9) are configured to generate different gas pressure differences to be measured on both sides of a sample, to-be-detected gas diffuses and escapes from one side of the sample to the other side, ions are generated by exciting the escaping gas with electron beams, SEM images and ESD images are obtained by scanning electron microscopy to analyze permeation paths and behaviors of the gas in the sample, but quantification of permeation escaping gas cannot be realized to evaluate permeation characteristics of materials.
The national standard GB/T30074 specifies a method for measuring the hydrogen permeability of a metal material by using an electrochemical technology, and hydrogen permeability data is obtained by using the electrochemical reaction principle of a sample in a solution and a method for measuring oxidation current. The method needs to carry out plating or chemical treatment on the metal surface, and has strict requirements on the preparation process and the external dimensions of the metal material sample to be detected, such as the ratio of radius to thickness, and the like.
The national standard GB/T1038 prescribes a device and a method for carrying out permeability test of plastic films and sheets by adopting a differential pressure method, a sample to be tested is arranged in a closed container, the sealing is carried out after high-pressure gas with the pressure of 105Pa is filled into one side of a sealing sheet, the sealing is carried out after the other vacuumizing pressure is less than 10Pa, and the gas permeability in the material to be tested is measured by measuring the change of the vacuum side pressure in unit time. The method needs to maintain a larger pressure difference at two sides of the test piece, and after the air sources at the two sides are sealed and isolated, the vacuum side pressure continuously rises in the penetration test process and cannot be maintained stable.
Therefore, in summary, it can be seen that the existing hydrogen permeability detection device for the material to be detected has complex process and is limited by the test piece structure, the detection temperature and other conditions.
Disclosure of Invention
The utility model aims to provide a hydrogen permeability testing device and a testing method for a solid detection material, which are used for solving the technical problems in the background technology.
In order to achieve the above purpose, the present utility model discloses the following technical solutions:
the utility model provides a hydrogen permeability testing arrangement of solid detection material, includes the incubator, is used for carrying hydrogen transport portion, is used for carrying the carrier gas transport portion of carrier gas, is used for carrying out the gas content measuring apparatu that detects the concentration of hydrogen and is used for adjusting the heat exchanger of gas temperature, be provided with the centre gripping frock that is used for centre gripping detection material hollow cylinder in the incubator, hydrogen transport portion, carrier gas transport portion, gas content measuring apparatu all set up in the outside of incubator;
the clamping tool comprises an upper cover, a lower cover, a shell, a sealing gasket and a fastening bolt, wherein the upper cover and the lower cover are respectively arranged at the top and the bottom of the shell, the upper cover and the lower cover are connected through the fastening bolt, and the sealing gasket is arranged at the bottom of the upper cover and the top of the lower cover; the top and the bottom of the detection material hollow cylinder are arranged in an opening way, the top and the bottom of the detection material hollow cylinder are respectively abutted against the sealing gasket, and the detection material hollow cylinder is clamped between the upper cover and the lower cover; the upper cover, the lower cover, the shell, the sealing gasket and the detection material hollow cylinder are concentrically arranged;
a high-pressure chamber is defined between the inner wall of the hollow cylinder of the detection material and the bottom of the upper cover and between the outer wall of the hollow cylinder of the detection material and the bottom of the upper cover, the top of the lower cover and the inner wall of the shell;
the upper cover is provided with a hydrogen inlet pipe and a first exhaust pipe, the hydrogen inlet pipe is communicated with the air outlet end of the hydrogen conveying part, and the bottom end of the hydrogen inlet pipe extends into the high-pressure chamber and is arranged close to the top of the lower cover; the bottom end of the exhaust pipe I extends into the high-pressure chamber and is arranged close to the bottom of the upper cover;
the housing is provided with a carrier gas inlet pipe and a second exhaust pipe, and the head end of the carrier gas inlet pipe is communicated with the air outlet end of the carrier gas conveying part; the tail end of the carrier gas inlet pipe and the head end of the exhaust pipe II extend into the low-pressure chamber, the carrier gas inlet pipe and the exhaust pipe II are respectively arranged on two sides of the shell, the tail end of the exhaust pipe II is communicated with the inlet end of the heat exchanger, and the outlet end of the heat exchanger is communicated with the gas content measuring instrument;
and pressure sensor interfaces for installing pressure gauges are arranged at the parts of the shell and the upper cover corresponding to the high-pressure chamber.
In one embodiment, the hydrogen conveying part comprises a hydrogen cylinder, an outlet pipeline I, a stop valve I, a pressure reducing and stabilizing valve I and a pressure gauge I, wherein the stop valve I, the pressure reducing and stabilizing valve I and the pressure gauge I are arranged on the outlet pipeline I, the stop valve I is respectively arranged adjacent to the hydrogen cylinder and the pressure reducing and stabilizing valve I, the outlet pipeline I penetrates through the thermostat and is communicated with an inner cavity of the clamping tool, and a sealing ring is arranged at the joint of the outer wall of the outlet pipeline I and the thermostat.
In one embodiment, the carrier gas conveying part comprises a carrier gas cylinder, a second outlet pipeline, a second stop valve, a second pressure reducing and stabilizing valve, a second pressure meter and a flowmeter, wherein the second stop valve, the second pressure reducing and stabilizing valve, the pressure meter and the flowmeter are arranged on the second outlet pipeline, the second stop valve is respectively arranged adjacent to the carrier gas cylinder and the pressure reducing and stabilizing valve, the second outlet pipeline penetrates through the incubator and is communicated with the inner cavity of the clamping tool, and a sealing ring is arranged at the joint of the outer wall of the second outlet pipeline and the incubator.
In one embodiment, the gas content gauge comprises a hydrogen concentration analyzer and/or a chromatograph.
In one embodiment, the outlet end of the carrier gas inlet pipe is higher than the two inlet ends of the exhaust pipe.
In one embodiment, the heat exchanger comprises a first heat exchanger for adjusting the temperature of the hydrogen, a second heat exchanger for adjusting the temperature of the carrier gas, and a third heat exchanger for adjusting the temperature of the mixed gas, wherein the first heat exchanger is communicated between the hydrogen conveying part and the inlet end of the hydrogen inlet pipe, the second heat exchanger is communicated between the carrier gas conveying part and the inlet end of the carrier gas inlet pipe, the inlet end of the third heat exchanger is communicated with the tail end of the exhaust pipe, and the outlet end of the third heat exchanger is communicated with the gas content measuring instrument.
In one embodiment, the first heat exchanger and the second heat exchanger are disposed in the incubator, and the third heat exchanger is disposed outside the incubator.
The beneficial effects are that: according to the hydrogen permeability testing device and the hydrogen permeability testing method of the solid detection material, the gas permeability is tested based on the solid detection material, in the testing process, the carrier gas in the low-pressure chamber of the clamping tool is in a stable flowing state, so that constant pressure and constant gas medium components are kept in the low-pressure chamber, stable permeation environment conditions can be provided for permeation of hydrogen in the high-pressure chamber, and the problems that the side pressure of the carrier gas is increased, the partial pressure is reduced and the like due to permeation of the internal gas into the carrier gas side in a permeation side sealing mode in the conventional mode are avoided, so that the accuracy of the measuring process is improved. Meanwhile, the heat exchanger of the hydrogen and the carrier gas and the clamping tool are arranged in the incubator, different testing environment temperature conditions can be adjusted according to the material permeability testing requirement, the constant temperature of the testing process is maintained, the temperature difference between the gas and the testing tool is reduced, and the testing reliability is ensured.
Drawings
In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the utility model, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a hydrogen permeability test apparatus for a solid detection material according to an embodiment;
fig. 2 is a schematic perspective view of a clamping tool in an embodiment;
FIG. 3 is a schematic perspective view of a clamping tool according to an embodiment;
FIG. 4 is a schematic cross-sectional view of a clamping tool according to an embodiment;
FIG. 5 is a schematic diagram showing the operation of the hydrogen permeability test device for solid detection materials according to the embodiment of the present utility model.
Reference numerals: 1. a constant temperature box; 2. a gas content measuring instrument; 301. a first heat exchanger; 302. a second heat exchanger; 303. a third heat exchanger; 4. a hydrogen gas cylinder; 5. an outlet pipeline I; 6. a stop valve I; 7. a first pressure reducing and stabilizing valve; 8. a first pressure gauge; 9. a carrier gas cylinder; 10. an outlet pipeline II; 11. a second stop valve; 12. a pressure reducing and stabilizing valve II; 13. a second pressure gauge; 14. a flow meter; 15. an upper cover; 16. a lower cover; 17. a housing; 18. a sealing gasket; 19. a fastening bolt; 20. detecting a material hollow cylinder; 21. a high pressure chamber; 22. a low pressure chamber; 23. a hydrogen inlet pipe; 24. an exhaust pipe I; 25. a carrier gas inlet pipe; 26. and a second exhaust pipe.
Detailed Description
The following description of the technical solutions in the embodiments of the present utility model will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
In this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other like elements in a process, method, article or apparatus that comprises the element.
The utility model discloses a hydrogen permeability testing device of a solid detection material shown in fig. 1, which comprises an incubator 1, a hydrogen conveying part for conveying hydrogen, a carrier gas conveying part for conveying carrier gas, a gas content measuring instrument 2 for detecting the concentration of the hydrogen and a heat exchanger for adjusting the gas temperature, wherein the incubator 1 can be any one of the prior art, and particularly, in the utility model, the incubator 1 is a box body with a temperature regulating function and is used for providing a temperature environment required by permeability testing.
The incubator 1 is internally provided with a clamping tool for clamping the hollow cylinder 20 of the detection material, and the hydrogen conveying part, the carrier gas conveying part and the gas content measuring instrument 2 are all arranged outside the incubator 1. It should be noted that, the hollow cylinder 20 of the detection material refers to a hollow cylindrical structure formed by preparing a solid detection material, and it is possible that the solid detection material may be prepared into a square or other structure with different properties under the condition that some test accuracy requirements are slightly low, which is simply thought by those skilled in the art, and may be obtained without any creative effort.
As a possible implementation manner of this embodiment, the hydrogen delivery portion includes a hydrogen gas cylinder 4, an outlet pipe 5, and a stop valve 6, a pressure reducing and stabilizing valve 7, and a pressure gauge 8 mounted on the outlet pipe 5, where the stop valve 6 is disposed adjacent to the hydrogen gas cylinder 4 and the pressure reducing and stabilizing valve 7, respectively, that is, the stop valve 6, the pressure reducing and stabilizing valve 7, and the pressure gauge 8 are disposed on the outlet pipe 5 in sequence. The first outlet pipeline 5 penetrates through the incubator 1 and is communicated with the inner cavity of the clamping tool, and a sealing ring is arranged at the joint of the outer wall of the first outlet pipeline 5 and the incubator 1.
As a possible implementation manner of this embodiment, the carrier gas conveying portion includes a carrier gas cylinder 9, an outlet pipe two 10, and a stop valve two 11, a pressure reducing and stabilizing valve two 12, a pressure gauge two 13, and a flow meter 14 mounted on the outlet pipe two 10, where the stop valve two 11 is disposed adjacent to the carrier gas cylinder 9 and the pressure reducing and stabilizing valve two 12, that is, on the outlet pipe two 10, the stop valve two 11, the pressure reducing and stabilizing valve two 12, the pressure gauge two 13, and the flow meter 14 are sequentially disposed. The second outlet pipeline 10 penetrates through the incubator 1 and is communicated with the inner cavity of the clamping tool, and a sealing ring is arranged at the joint of the outer wall of the second outlet pipeline 10 and the incubator 1.
As a possible implementation of the present example, the gas content measuring instrument 2 includes a hydrogen concentration analyzer and/or a chromatograph. The gas content measuring instrument 2 is applicable to a structure for detecting the components and amounts of the gas after the test, and any one of the prior art devices may be used, and is not limited to a hydrogen concentration analyzer and a chromatograph.
Referring to fig. 2-4, in this embodiment, the clamping fixture includes an upper cover 15, a lower cover 16, a housing 17, a gasket 18, and a fastening bolt 19. The upper cover 15 is typically made of a hard metal or organic material, and is provided with openings for mounting fastening bolts 19. The lower cover 16 is generally made of hard metal or organic material, and is provided with mounting holes for mounting the fastening bolts 19, which are equal in size to those of the upper cover 15. The upper cover 15 and the lower cover 16 are respectively arranged at the top and the bottom of the shell 17, and the upper cover 15 and the lower cover 16 are connected through the fastening bolts 19.
The gasket 18 is provided at the bottom of the upper cover 15 and the top of the lower cover 16; the top and the bottom of the hollow cylinder 20 of the detection material are arranged in an opening, the top and the bottom of the hollow cylinder 20 of the detection material respectively lean against the sealing gasket 18, and the hollow cylinder 20 of the detection material is clamped between the upper cover 15 and the lower cover 16. That is, one sealing pad 18 is located between the upper cover 15 and the top of the hollow cylinder 20 of detection material, and the other sealing pad 18 is located between the lower cover 16 and the bottom of the hollow cylinder 20 of detection material, and the sealing pad 18 can be made of soft silica gel pad or other materials, and has a ring-shaped or circular structure for forming a seal between the upper cover 15, the lower cover 16 and the hollow cylinder 20 of detection material.
The upper cover 15, the lower cover 16, the outer shell 17, the sealing gasket 18 and the hollow cylinder 20 of the detection material are concentrically arranged, so that the advantage of the arrangement is that the flow of hydrogen in the clamping tool is facilitated, and the stability of the air pressure in the testing tool is facilitated.
A high-pressure chamber 21 is defined between the inner wall of the detection material hollow cylinder 20 and the bottom of the upper cover 15 and the top of the lower cover 16, a hydrogen inlet pipe 23 and an exhaust pipe 24 are arranged on the upper cover 15, the hydrogen inlet pipe 23 is communicated with the air outlet end of the hydrogen conveying part, and the bottom end of the hydrogen inlet pipe 23 extends into the high-pressure chamber 21 and is arranged close to the top of the lower cover 16; the bottom end of the first exhaust pipe 24 extends into the high-pressure chamber 21 and is disposed near the bottom of the upper cover 15.
The outer wall of the hollow cylinder 20 of detection material and the bottom of the upper cover 15, the top of the lower cover 16 and the inner wall of the housing define a low pressure chamber 22 therebetween. A carrier gas inlet pipe 25 and a second exhaust pipe 26 are arranged on the shell 17, and the head end of the carrier gas inlet pipe 25 is communicated with the air outlet end of the carrier gas conveying part; the tail end of the carrier gas inlet pipe 25 and the head end of the exhaust pipe II 26 extend into the low-pressure chamber 22, the carrier gas inlet pipe 25 and the exhaust pipe II 26 are respectively arranged on two sides of the shell 17, the tail end of the exhaust pipe II 26 is communicated with the inlet end of the heat exchanger, and the outlet end of the heat exchanger is communicated with the gas content measuring instrument 2. The outer shell 17 is a tubular structure of thin-wall metal or organic material, has the same height as the hollow cylinder 20 of the detection material, and has a diameter larger than the outer diameter of the hollow cylinder 20 of the detection material.
Preferably, the outlet end of the carrier gas inlet pipe 25 is arranged at a higher level than the inlet end of the exhaust pipe two 26, which has the advantage of reducing the dead angle of the air flow.
The parts of the casing 17 and the upper cover 15 corresponding to the high pressure chamber 21 are respectively provided with a pressure sensor interface 27 for installing a pressure gauge, the pressure sensor interface 27 can be connected with the pressure gauge in a threaded connection manner, and the pressure sensor interface 27 is communicated with the high pressure chamber 21 and the low pressure chamber 11 through a small hole. In particular, the side wall of the housing 17 may optionally be provided with an aperture for a cable through the thermometer, but this is not necessary, and whether or not to set is selected according to the temperature measurement requirements. Wherein the pressure gauge mounted through the pressure sensor port 27 on the upper cover 15 is used for measuring the pressure of the medium in the high pressure chamber 21, and the pressure gauge mounted through the pressure sensor port 27 on the housing 17 is used for measuring the pressure of the medium in the low pressure chamber 22. The thermometer probe selected can be adhered to the inner surface of the hollow cylinder 20 of the detection material, the outer surface of the hollow cylinder 20 of the detection material, the high-pressure chamber 21, the low-pressure chamber 22 and the like for measuring the temperature of the corresponding area or component, and the data wire of the thermometer is connected out through the small hole on the side wall of the shell 17, meanwhile, if the temperature inside the workpiece is not required to be measured in the test process, the related equipment of the thermometer can be omitted, and the small hole is not required to be formed on the side wall of the shell 17.
In this embodiment, the heat exchangers include a first heat exchanger 301 for adjusting the temperature of the hydrogen, a second heat exchanger 302 for adjusting the temperature of the carrier gas, and a third heat exchanger 303 for adjusting the temperature of the mixed gas, where the first heat exchanger 301 is communicated between the hydrogen delivery portion and the inlet end of the hydrogen inlet pipe 23, the second heat exchanger 302 is communicated between the carrier gas delivery portion and the inlet end of the carrier gas inlet pipe 25, the inlet end of the third heat exchanger 303 is communicated with the tail end of the second exhaust pipe 26, and the outlet end of the third heat exchanger 303 is communicated with the gas content measuring instrument 2. The first heat exchanger 301 and the second heat exchanger 302 are arranged in the incubator 1, and the third heat exchanger 303 is arranged outside the incubator 1. The first heat exchanger 301 and the second heat exchanger 302 are used for adjusting the temperature of the gas to a required test temperature before the gas enters the clamping tool, so that the temperature disturbance of the gas in the hollow cylinder 20 of the detection material is reduced, the first heat exchanger 301 and the second heat exchanger 302 are usually in coil pipe form, and a fan can be optionally arranged to perform forced flow of the gas flow according to the temperature regulation requirement. The third heat exchanger 303 is used for adjusting the temperature of the air flow excluding the test tool, so that the air flow meets the measurement requirement of the air content measuring instrument 2. Heat exchanger three 303 is typically in the form of a coil and the outlet may be provided with a thermometer to indicate the temperature of the air stream. And the exhaust gas of the gas content measuring instrument 2 is led to the safety area for treatment together with the rest of the discharged carrier gas through a pipeline.
Working principle: the solid detection material is manufactured into a hollow cylindrical tubular structure (namely, a detection material hollow cylinder body 20) which is equal to the height of the shell 17 and has an outer diameter smaller than the inner diameter of the shell 17, the detection material hollow cylinder body 20 is installed through a clamping tool to form an inner-outer isolated closed space (namely, a high-pressure chamber 21 corresponding to an inner cavity isolated by the clamping tool and a low-pressure chamber 22 corresponding to an isolated outer cavity), hydrogen is introduced into the high-pressure chamber 21, and the pressure stability in the high-pressure chamber 22 is maintained by controlling a stop valve I6 and a decompression pressure stabilizing valve I7 and closing an exhaust pipe I24 after the high-pressure chamber 22 is completely filled with hydrogen; the low pressure chamber 22 is internally matched with the second stop valve 11, the second pressure reducing and stabilizing valve 12 and the adjustment of the flowmeter 14 to continuously introduce a carrier gas with stable flow rate (usually, inert gas such as high-purity nitrogen is used as carrier gas). The hydrogen permeates through the hollow cylinder 20 of the detection material and then is mixed with carrier gas to be discharged out of the clamping tool. The clamping fixture provides a required test temperature environment through the incubator 1, in the test process, mixed gas in the low-pressure chamber 22 is led out of the incubator 1 through the exhaust pipe II 26 and rewarmed to a temperature range required by the gas content measuring instrument 2 through the heat exchanger III 303, then one part of the mixed gas is measured through the gas content measuring instrument 2, and the other part of the mixed gas is discharged to a safety area for treatment. In the measuring process, the permeability characterization measurement can be carried out by adopting a concentration method of hydrogen in the mixed gas discharged by the clamping tool. The device has simple structure and operation method, and has higher precision (generally reaching 0.1ppm level and below).
As shown in fig. 5, the method for operating the gas permeability test apparatus for a solid detection material in this embodiment includes the following steps:
s101, arranging a hydrogen permeability testing device of the solid detection material;
s102, hydrogen is conveyed into a high-pressure chamber 21 of a clamping tool after pressure regulation through a pressure reducing and stabilizing valve I7 and temperature regulation through a heat exchanger I301, a stop valve I6 is closed to stop the exhaust of a hydrogen cylinder 4, and the pressure of the high-pressure chamber 21 is maintained stable in the test process;
s103, regulating the pressure of the carrier gas through a pressure reducing and stabilizing valve II 12 and regulating the temperature through a heat exchanger II 302, regulating the pressure and flow rate of the carrier gas by combining the pressure reducing and stabilizing valve II 12 and a flow meter 14, continuously conveying the carrier gas into a low pressure chamber 22 of a clamping tool, and enabling the pressure of the low pressure chamber 22 to be smaller than that of a high pressure chamber 21 in the test process;
and S104, after the test is started, the gas in the low-pressure chamber 21 is discharged to the gas content measuring instrument 2 through the second exhaust pipe 26 to detect the concentration of the hydrogen, and the permeation index of the hydrogen based on the detection material hollow cylinder 20 installed in the clamping tool is obtained according to the detection result of the concentration of the hydrogen.
In this embodiment, the permeation index of the hydrogen gas based on the detection material hollow cylinder 20 installed in the clamping fixture includes the permeation Q of the hydrogen gas in the detection material g And the permeability coefficient p of hydrogen in the detection material g 。
Permeation quantity Q of hydrogen in detection material g Calculated by the following formula:
wherein q c To convert to the permeability of hydrogen under standard conditions, the unit is m 3 /(m 2 ·h·Pa)；q 2 The unit is m for the flow rate of the carrier gas 3 A/min; c is the concentration of hydrogen in the carrier gas in mg/L; a is the contact area between the hydrogen and the inner wall of the hollow cylinder 20 of the detection material, and the unit is m 2 The method comprises the steps of carrying out a first treatment on the surface of the ΔP is the pressure difference between the inner and outer chambers of the sample, and the unit is Pa; m is M 1 The molecular weight of hydrogen is 2g/mol; v (V) m Is an ideal gas constant under standard conditions, and is 22.4L/mol.
Permeability coefficient p of hydrogen in the detection material g Calculated by the following formula:
wherein L is the thickness of the hollow cylinder (20) of the detection material, and the unit is m; q (Q) g Is m 3 ·m/(m 2 ·h·Pa)。
In the embodiment, high-purity hydrogen (the purity is more than or equal to 99.999%) is used as hydrogen and high-purity nitrogen (the purity is more than or equal to 99.999%) is used as carrier gas. The hydrogen gas cylinder 4 and the carrier gas cylinder 9 are respectively used for storing hydrogen and nitrogen, after the outlet of the hydrogen gas cylinder is stabilized by corresponding stop valves and pressure reducing and stabilizing valves to the pressure and flow requirements required by the test, the hydrogen gas cylinder is connected into the corresponding heat exchanger component and the incubator 1, and the pressure of the hydrogen gas cylinder is generally required to be higher than the pressure of the nitrogen gas after pressure regulation so as to form an osmotic pressure difference. And after the high-pressure chamber 21 is completely filled with hydrogen, the exhaust pipe I24 is closed, and the pressure of the inner cavity of the clamping tool is kept stable. The nitrogen pressure and flow are maintained stable in the test. The gas source of the gas content measuring instrument 2 is connected with the exhaust pipe II 26 of the self-clamping tool, recording is started after the data is stable, and the permeability coefficient are calculated according to the methods of the formula I and the formula II.
In the description of the present disclosure, it should be noted that the positional or positional relationship indicated by terms such as "top", "bottom", "leading", "trailing" and the like are based on the positional or positional relationship shown in the drawings, and are merely for convenience of describing the present disclosure and simplifying the description, and are not indicative or implying that the apparatus or element in question must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present disclosure.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present utility model, and although the present utility model has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present utility model.
Claims (7)
1. The utility model provides a hydrogen permeability testing arrangement of solid detection material, includes thermostated container (1), is used for carrying hydrogen transport portion, is used for carrying the carrier gas transport portion of carrier gas, is used for carrying out the gas content measuring apparatu (2) that detects to the concentration of hydrogen and is used for adjusting the heat exchanger of gas temperature, its characterized in that, be provided with the centre gripping frock that is used for centre gripping detection material hollow cylinder (20) in thermostated container (1), hydrogen transport portion, carrier gas transport portion, gas content measuring apparatu (2) all set up in the outside of thermostated container (1);
the clamping tool comprises an upper cover (15), a lower cover (16), a shell (17), a sealing gasket (18) and a fastening bolt (19), wherein the upper cover (15) and the lower cover (16) are respectively arranged at the top and the bottom of the shell (17), the upper cover (15) and the lower cover (16) are connected through the fastening bolt (19), and the sealing gasket (18) is arranged at the bottom of the upper cover (15) and the top of the lower cover (16); the top and the bottom of the detection material hollow cylinder (20) are arranged in an opening way, the top and the bottom of the detection material hollow cylinder (20) are respectively propped against the sealing gasket (18), and the detection material hollow cylinder (20) is clamped between the upper cover (15) and the lower cover (16); the upper cover (15), the lower cover (16), the shell (17), the sealing gasket (18) and the detection material hollow cylinder (20) are concentrically arranged;
a high-pressure chamber (21) is formed by enclosing between the inner wall of the detection material hollow cylinder (20) and the bottom of the upper cover (15) and the top of the lower cover (16), and a low-pressure chamber (22) is formed by enclosing between the outer wall of the detection material hollow cylinder (20) and the bottom of the upper cover (15), the top of the lower cover (16) and the inner wall of the shell;
the upper cover (15) is provided with a hydrogen inlet pipe (23) and an exhaust pipe I (24), the hydrogen inlet pipe (23) is communicated with the air outlet end of the hydrogen conveying part, and the bottom end of the hydrogen inlet pipe (23) extends into the high-pressure chamber (21) and is arranged close to the top of the lower cover (16); the bottom end of the exhaust pipe I (24) extends into the high-pressure chamber (21) and is arranged close to the bottom of the upper cover (15);
a carrier gas inlet pipe (25) and a second exhaust pipe (26) are arranged on the shell (17), and the head end of the carrier gas inlet pipe (25) is communicated with the air outlet end of the carrier gas conveying part; the tail end of the carrier gas inlet pipe (25) and the head end of the exhaust pipe II (26) extend into the low-pressure chamber (22), the carrier gas inlet pipe (25) and the exhaust pipe II (26) are respectively arranged on two sides of the shell (17), the tail end of the exhaust pipe II (26) is communicated with the inlet end of the heat exchanger, and the outlet end of the heat exchanger is communicated with the gas content measuring instrument (2);
a pressure sensor interface (27) for mounting a pressure gauge is arranged on the housing (17) and the upper cover (15) at the part corresponding to the high-pressure chamber (21).
2. The hydrogen permeability test device of a solid detection material according to claim 1, wherein the hydrogen conveying part comprises a hydrogen gas cylinder (4), an outlet pipeline I (5), a stop valve I (6), a pressure reducing and stabilizing valve I (7) and a pressure gauge I (8) which are arranged on the outlet pipeline I (5), the stop valve I (6) is respectively arranged adjacent to the hydrogen gas cylinder (4) and the pressure reducing and stabilizing valve I (7), the outlet pipeline I (5) penetrates through the constant temperature box (1) and is communicated with an inner cavity of the clamping tool, and a sealing ring is arranged at a joint of the outer wall of the outlet pipeline I (5) and the constant temperature box (1).
3. The hydrogen permeability test device for a solid detection material according to claim 1, wherein the carrier gas conveying part comprises a carrier gas cylinder (9), an outlet pipeline II (10), a stop valve II (11), a pressure reducing and stabilizing valve II (12), a pressure gauge II (13) and a flow meter (14) which are arranged on the outlet pipeline II (10), the stop valve II (11) is respectively arranged adjacent to the carrier gas cylinder (9) and the pressure reducing and stabilizing valve II (12), the outlet pipeline II (10) penetrates through the constant temperature box (1) and is communicated with an inner cavity of the clamping tool, and a sealing ring is arranged at the joint of the outer wall of the outlet pipeline II (10) and the constant temperature box (1).
4. The hydrogen permeability test device of a solid detection material according to claim 1, characterized in that the gas content meter (2) comprises a hydrogen concentration analyzer and/or a chromatograph.
5. The hydrogen permeability test device for a solid detection material according to claim 1, wherein the outlet end of the carrier gas inlet pipe (25) is disposed at a higher level than the inlet end of the exhaust pipe two (26).
6. The hydrogen permeability test device for a solid detection material according to claim 1, wherein the heat exchanger includes a first heat exchanger (301) for performing temperature adjustment on hydrogen, a second heat exchanger (302) for performing temperature adjustment on carrier gas, and a third heat exchanger (303) for performing temperature adjustment on mixed gas, the first heat exchanger (301) is communicated between the hydrogen conveying portion and an inlet end of the hydrogen intake pipe (23), the second heat exchanger (302) is communicated between the carrier gas conveying portion and an inlet end of the carrier gas intake pipe (25), an inlet end of the third heat exchanger (303) is communicated with a tail end of the second exhaust pipe (26), and an outlet end of the third heat exchanger (303) is communicated with the gas content measuring instrument (2).
7. The hydrogen permeability test apparatus for a solid detection material according to claim 6, wherein the first heat exchanger (301) and the second heat exchanger (302) are disposed inside the incubator (1), and the third heat exchanger (303) is disposed outside the incubator (1).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117169088A (en) * | 2023-11-03 | 2023-12-05 | 大连理工大学 | High-pressure hydrogen permeation continuous monitoring device and testing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117169088A (en) * | 2023-11-03 | 2023-12-05 | 大连理工大学 | High-pressure hydrogen permeation continuous monitoring device and testing method thereof |
| CN117169088B (en) * | 2023-11-03 | 2024-01-09 | 大连理工大学 | High-pressure hydrogen permeation continuous monitoring device and testing method thereof |
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