CN116222902A - Hydrogen permeation/leakage/fatigue integrated measurement device and process - Google Patents
Hydrogen permeation/leakage/fatigue integrated measurement device and process Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/202—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material using mass spectrometer detection systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/22—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators
- G01M3/223—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators for pipe joints or seals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
- G01M3/32—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
- G01M3/3236—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers
- G01M3/3263—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers using a differential pressure detector
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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
- G01N15/082—Investigating permeability by forcing a fluid through a sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/32—Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces
- G01N3/36—Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces generated by pneumatic or hydraulic means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0062—Crack or flaws
- G01N2203/0066—Propagation of crack
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0073—Fatigue
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/023—Pressure
- G01N2203/0234—Low pressure; Vacuum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0236—Other environments
- G01N2203/0242—With circulation of a fluid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Dispersion Chemistry (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Examining Or Testing Airtightness (AREA)
Abstract
The invention designs hydrogen permeation/leakage/fatigue integrated measurement equipment and a process, which comprise an air inlet pressurizing system, a temperature control system, a test die, a vacuumizing system, a hydrogen permeation/leakage amount detection system, a hydrogen circulation system and a safety system, and can be used for carrying out hydrogen permeation performance measurement, hydrogen circulation crack propagation performance measurement and bulge performance measurement in a rapid decompression process aiming at different hydrogen storage bottle liner materials, carbon fiber composite materials, sealing rings or other laboratory samples. Meanwhile, the invention designs various test die structures, and can provide various performance data of materials under hydrogen environment, different temperatures and pressures, such as permeability, leakage amount, cycle service life and the like. The invention is suitable for high-pressure hydrogen blocking detection and has the advantages of simple structure, easy replacement of the test die and easy adjustment of temperature and pressure. In addition, the invention can reduce the hydrogen loss of a single experiment by recycling hydrogen.
Description
Technical Field
The invention relates to the technical field of material hydrogen permeation, in particular to hydrogen permeation/leakage/fatigue integrated measurement equipment and a process.
Background
Along with the optimization and upgrading of hydrogen production front-end equipment and hydrogen terminal equipment for aerospace, fuel cell automobiles and the like, the development of safe and efficient hydrogen energy storage and transportation technology and equipment are important factors for promoting the upgrading of a hydrogen energy industry chain. The normal temperature and high pressure hydrogen storage is a main current technical route because of low energy consumption in hydrogen preparation and high filling speed. However, the high-pressure hydrogen storage bottle is provided with a short plate with low quality hydrogen storage density, and research and development of a plastic liner carbon fiber fully-wound composite material (IV type) gas bottle is one of important ways for improving the quality hydrogen storage density.
Under the severe conditions of high pressure, extreme use environment temperature and rapid hydrogen charging and discharging, hydrogen inevitably permeates/leaks from the high pressure side to the low pressure side, and certain damages to the material itself can be caused by high pressure, high and low pressure circulation, high and low temperature environment and the like, such as promotion of crack growth, generation of bulge defects, fatigue failure and the like. In addition, the hydrogen gas permeated/leaked to the outside may cause a failure of the high-pressure hydrogen storage container, an increase in the environmental hydrogen concentration, an explosion hazard, and the like. Therefore, in the front-end research process of hydrogen storage bottle manufacture, knowledge and strict control of the hydrogen permeation performance and fatigue performance of the high-pressure hydrogen storage bottle material and the sealing performance of the sealing piece and sealing structure of the hydrogen storage bottle are important means and requirements for improving the hydrogen storage safety, improving the hydrogen storage density and saving the cost.
The existing hydrogen permeability measuring device and method for the hydrogen storage bottle at present, such as CN202010253265.8, can judge whether the bottle reaches the standard or not after the whole bottle is formed, has high economic cost and a plurality of interference factors, and is difficult to judge the specific cause of the defect. Therefore, the detection method is not suitable for the performance research judgment of the front end of the material and the sealing structure.
Hydrogen aging/fatigue performance testing of materials are typically placed in autoclaves and the aging/fatigue performance is checked after subjecting all to high pressure cycles. The method has important significance for material research; but cannot acquire process data of the influence of the internal structure change of the sample on the permeability under the synergistic effect of pressure, temperature and time; in addition, the damage to the material caused by the single-side high pressure difference in the actual situation is not really realized, and the method has a gap from the accurate life prediction.
In terms of the permeability testing of materials, some patents propose a solution to the hydrogen permeation measurement system. The device can detect the hydrogen permeation quantity caused by the pressure difference in the direction vertical to the sheet sample, can create a temperature simulation environment for the sample by heating the die, and is relatively suitable for accurately detecting the detection medium quantity permeated into the sample container under the environmental conditions of different die temperatures. However, because the target detection sample aimed at is different from the sample detection requirement of the hydrogen storage bottle, the hydrogen storage bottle can only be used for the permeation quantity test of materials under the ultra-low vacuum condition, and the testing capability is single; the proposed die structure does not consider the influence of a sealing structure and the like on permeation data in the test process, and is not suitable for gas medium permeation test under high pressure and ultrahigh pressure conditions; in addition, the pressure, temperature, positive pressure control accuracy of the test medium is not considered; additionally, the related systems have no explicit recovery scheme for hydrogen and the like, which tends to result in excessive testing costs. In addition, some research institutions have also proposed a method of indirectly testing the hydrogen permeation performance of materials by testing the hydrogen content after swelling the materials in an autoclave, which has a certain test error from the actual hydrogen permeation.
In summary, the active detection device has larger limitations (low test pressure, low temperature and pressure control precision, single test performance, difficult application to test specific sealing structures and high requirement on the structural size of samples) or can only be used for indirect measurement aiming at the permeability coefficient test of liner materials and carbon fiber composite materials for hydrogen storage bottles, the sealing performance test of sealing materials and sealing structures, and the performance test of various material samples under the conditions of high temperature and low hydrogen circulation and the like. There remains a need for an integrated testing apparatus and process that supports front-end development of materials for hydrogen storage bottles.
Disclosure of Invention
In order to avoid and overcome the technical problems in the prior art, the invention provides hydrogen permeation/leakage/fatigue integrated measurement equipment and a process. The method can be used for carrying out hydrogen permeability measurement, hydrogen circulation crack propagation performance measurement and bulge performance measurement in a rapid decompression process aiming at different hydrogen storage bottle liner materials, carbon fiber composite materials, sealing rings or other laboratory samples; in addition, the sealing performance of the nonmetallic material-metallic material sealing structure can be measured through the die structure adjustment. The invention can provide various performance data of materials under hydrogen environment and different temperature conditions, such as permeability, leakage amount, cycle service life and the like. Compared with the existing testing device, the hydrogen permeation/leakage/fatigue integrated testing device and the hydrogen permeation/leakage/fatigue integrated testing process are suitable for high-pressure hydrogen blocking detection, and have the advantages of being good in safety, simple in structure and easy to replace and adjust the die.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the invention relates to hydrogen permeation/leakage/fatigue integrated measurement equipment which comprises an air inlet pressurization system, a temperature control system, a test die, a vacuumizing system, a hydrogen permeation/leakage amount detection system, a hydrogen circulation system and a safety system. The air inlet pressurizing system comprises a hydrogen storage bottle group, a pressure regulating valve, a one-way valve, a compressor, a temperature and pressure sensor, a buffer pipeline, an overflow valve and a speed regulating pressure regulating valve. The temperature control system comprises buffer pipeline heating and cooling equipment, a temperature control system, a mold heating and cooling system and a temperature and pressure sensor. The basic structure of the test die comprises a high-pressure cavity die, a low-pressure cavity die, a sealing ring, a porous supporting plate and porous sintered ceramic. The vacuumizing system comprises a vacuum pump, a temperature and pressure sensor and a vacuum pressure gauge. The hydrogen permeation/leakage detection system comprises a hydrogen mass spectrometer, a purging system and an inert gas source. The hydrogen circulation system comprises a compressor, a speed regulating valve, a hydrogen recovery tank, a one-way valve and a pressure regulating valve. The safety system comprises an explosion-proof test box.
The invention relates to a specific connection mode of hydrogen permeation/leakage/fatigue integrated measurement equipment, which comprises the following steps: a plurality of pressure control channels with different levels are arranged between the hydrogen storage bottle group and the buffer pipeline, and the pressure of hydrogen entering the buffer pipeline is controlled through a pressure regulating valve and a one-way valve. For the low-pressure test requirement, the hydrogen storage bottle group is connected with the one-way valve through the pressure regulating valve and directly enters the buffer pipeline for heating and cooling; for the middle-high pressure test requirement, after the hydrogen of the hydrogen storage bottle group passes through the pressure regulating valve, the hydrogen enters the buffer pipeline from the outlets of the middle-pressure compressor and the high-pressure compressor through the one-way valve respectively by the multistage compressor according to different pressure requirements to be heated and cooled. The buffer pipeline outlet is connected with the overflow valve, so that the overpressure danger is prevented. Hydrogen enters the test die through the pressure and speed regulating valve after temperature treatment of the buffer pipeline. During the test, hydrogen leaking from the seal ring/seal structure will be purged into the hydrogen mass spectrometer from the side of the low pressure cavity die to verify mass; hydrogen gas permeated from the test sample will be purged into the hydrogen mass spectrometer assay mass from the tail of the low pressure cavity die. The high pressure hydrogen after the test is completed can be discharged through a needle valve or enter the next cycle. For hydrogen to be circulated, after the single test is finished, the hydrogen enters the hydrogen recovery tank from the check valve or the compressor after passing through the speed regulating valve by the high-pressure chamber of the test die. In addition, the hydrogen recovery tank is connected to the outlet position of the pressure regulating valve of the hydrogen storage bottle group through the pressure regulating valve. Aiming at the vacuumizing requirement before the test, each chamber, each pipeline and each environment box are respectively connected with a vacuum pump through needle valves to discharge the gas in the pipeline or the chamber. The temperature control system can directly heat and cool the buffer pipeline and the test mould through the environment box according to the heating and cooling requirements of the buffer pipeline and the test mould.
The test die consists of a high-pressure cavity die and a low-pressure cavity die, and is reliable in connection. The material is preferably 316L stainless steel with high fatigue strength. Alternatively, 6061 aluminum alloy with better heat conductivity is selected for the material.
The invention relates to a hydrogen permeation/leakage/fatigue integrated measurement device and a specific connection mode of a test die and a process, wherein the specific connection mode comprises the following steps: the high-pressure cavity die and the low-pressure cavity die are connected through axisymmetric fastening bolts, and the number of the fastening bolts is preferably 6 or 8. The high-pressure cavity die and the low-pressure cavity die are positioned through the positioning surface, are sealed in a circumferential direction through the sealing surface, and form a sealing ring testing channel. The sample is mounted in such a way that the axial direction from the low pressure chamber to the high pressure chamber is respectively a metal support plate, a porous sintered ceramic or a porous slide, a sealing ring, a sample, a sealing ring, a porous sintered ceramic or a porous slide (optional).
For some brittle materials, such as nylon 6, which have a specific structure after molding, such as a sample cut from a cylinder, it is difficult to forcibly flatten and seal in a test die, which is highly prone to inaccurate results during testing. Therefore, as an optimization, the high-pressure cavity die or the low-pressure cavity die of the test die can be composed of a replaceable die core and a die core pressing plate for fastening and bearing, the die core can be customized according to the appearance of a sample, and compared with the whole set of customized test die, the cost is lower. The core platen may limit axial movement of the high pressure cavity core. The combination mode of the mold core and the mold core pressing plate at one side is at least two, one is that the mold core is directly connected with an external pipeline, and the other is that the external pipeline is connected with the mold core pressing plate. The two connection modes can be adjusted according to specific requirements. When the test sample is a special-shaped surface and needs to be positioned, the mold core and the mold core pressing plate are suggested to be connected by adopting a rotation stopping structure, and the mold core pressing plate is fixedly connected with the mold at the other side or the mold core pressing plate by adopting bolts.
The mold core in the test mold scheme can be replaced according to the size of the sealing ring, the sealing structure form of nonmetal-metal connection, the curved surface shape of the detection sample and the like.
Alternatively, the mold core pressing plates on two sides or the mold core pressing plate on one side and the mold on the other side can be directly fastened through threaded connection. At this time, a connection mode capable of rotating is adopted between the mold core pressing plate and the mold core.
In the penetration test process of the invention, the sealing ring used for sealing the sample in the test die is preferably the diameter of the sealing ring of the high-pressure chamber is smaller than or equal to the diameter of the sealing ring of the low-pressure chamber.
The number of test dies in the device of the invention can be installed according to specific test requirements. The actual test area of the test die and the contact surface with the test sample can be tailored according to specific requirements, and are not particularly limited.
The pressurizing system of the invention preferably controls the pressure output through pressure regulating valves with different precision after pressurizing the multi-stage compressors according to different pressure demands and then obtains more accurate target pressure. Alternatively, the pressure is reduced by a pressure reducing valve and outputted after being increased by a single-stage booster compressor.
The pure hydrogen pressure of the hydrogen storage bottle group of the air inlet pressurizing system is preferably 5MPa to 20MPa.
The water volume of the hydrogen recovery tank of the hydrogen circulation system is preferably 10-20 times that of the high-pressure chamber of the test die and the sum of the volumes of the pipelines directly communicated with the high-pressure chamber.
The buffer pipeline has the main function of temporarily storing high-pressure hydrogen needed by the test, so that the pressure in the high-pressure test cavity can be built up quickly or according to a preset pressurizing rate; in addition, the buffer pipeline can preheat/precool high-pressure hydrogen for testing, so that the testing efficiency and the temperature uniformity of the hydrogen entering the testing cavity are improved. Preferably, the water volume of the buffer pipeline is 10-20 times of the sum of the volumes of the high-pressure chamber of the test die and the pipeline which is directly communicated with the high-pressure chamber. Alternatively, the buffer tube may be replaced with a buffer tank. The buffer pipeline is provided with an overpressure protection and automatic pressure relief device.
The buffer pipeline is preferably of a multi-layer structure, the inner high-pressure pipe is used for storing hydrogen, and the outer layer is used for introducing heating or cooling liquid to preheat/precool the hydrogen in the high-pressure pipe. As an improvement, the outer layer can also be coated with a heat insulation material, so that the heat exchange between heating or cooling liquid and the environment is reduced.
The buffer high-pressure pipeline heating and cooling device is preferably oil liquid heating and liquid nitrogen cooling. Alternatively, resistive wire heating or infrared heating may be used as the heating means.
The environment box is heated by infrared heating and cooled by liquid nitrogen cooling. Alternatively, the heating means may be heated by hot air.
The control valve of each position of the hydrogen permeation/leakage/fatigue integrated measuring equipment and the process is only used for clearly explaining the specific effect. It is within the scope of the present invention to use one valve body to combine two or more valve bodies or to split the function of one valve body into multiple valve bodies at a three-way position or other positions, as long as the primary function of the circuit is not changed. Part of the pipelines in the schematic diagram of the invention can also be replaced by valve plates.
The high-pressure valve of the hydrogen permeation/leakage/fatigue integrated measurement equipment and the process has a manual function.
Preferably, the hydrogen entering the high-pressure chamber and the hydrogen leaving the high-pressure chamber are controlled by a computer servo, so that higher experimental precision is provided.
As a safety concern, all components in contact with hydrogen or other flammable media should be subjected to an explosion-proof treatment.
The invention relates to a hydrogen permeation/leakage/fatigue integrated measuring device and a process, which designs various test die structures, can measure the hydrogen permeation rate of a planar sample or a sample with a certain curved surface under different temperature conditions by a differential pressure method, is also suitable for testing the sealing performance of an annular sealing material and a sealing structure, and is used for guiding the modification and structural design of a hydrogen storage bottle material. In addition, the hydrogen permeation/leakage/fatigue integrated measurement equipment and process can also regulate the speed, the temperature and the pressure of compressed hydrogen or other test media entering and exiting the high-pressure chamber, so that the bulge, the crack expansion and the hydrogen permeation of a test target sample in the processes of rapid hydrogen filling and discharging, cyclic hydrogen filling and discharging fatigue or accelerated hydrogen aging and the like are closer to the instruction sample materials and structural design of actual use working conditions, and the test cost of the whole bottle is reduced. The invention provides more efficient and more accurate test conditions by buffering the pipeline to heat or cool the hydrogen. In addition, the hydrogen consumption of a single experiment can be reduced and the experiment cost can be reduced by recycling the hydrogen.
Drawings
FIG. 1 is a schematic diagram of the system connection of a hydrogen permeation/leakage/fatigue integrated measurement device and process.
Fig. 2 is a schematic diagram of the basic structure of a test die of a hydrogen permeation/leakage/fatigue integrated measurement device and process.
FIG. 3 is a schematic diagram of a first construction of a test mold with replaceable mold cores for a hydrogen permeation/leakage/fatigue integrated test apparatus and process.
FIG. 4 is a schematic diagram of a second construction of a test mold with replaceable mold cores for a hydrogen permeation/leakage/fatigue integrated test apparatus and process.
FIG. 5 is a schematic diagram of a third construction of a test mold with replaceable mold cores for a hydrogen permeation/leakage/fatigue integrated test apparatus and process.
FIG. 6 is a schematic diagram showing the connection of a seal structure test die of a hydrogen permeation/leakage/fatigue integrated test apparatus and process.
FIG. 7 is a schematic diagram of the connection of a seal ring test die of a hydrogen permeation/leakage/fatigue integrated test apparatus and process.
FIG. 8 is a schematic diagram of a buffer pipeline structure of a hydrogen permeation/leakage/fatigue integrated measurement device and process.
1-a hydrogen cylinder group; 2-a pressure regulating valve; 3-a one-way valve; 4-1-compressor; 4-2-compressor; 5-a one-way valve; 6-a one-way valve; 7-buffer piping; 7-1-buffer inner layer of pipeline; 7-2-an outer layer of the buffer pipeline; 8-a pressure and speed regulating valve; 9-overflow valve; 10-an environmental box; 11-testing the mould; 12-a speed regulating valve; 13-a pressure regulating valve; 14-a hydrogen recovery tank; 15-needle valve; 16-a one-way valve; 17-needle valve; 18-a vacuum pump; 19-needle valve; 20-a compressor; 21-needle valve; 22-needle valve; a 23-hydrogen mass spectrometer; 24-a temperature control system; 25-low pressure cavity mold; 25-2-low pressure cavity mold; 26-a porous support plate; 27-porous sintered ceramic; 28-sealing rings; 29-sample; 30-sealing rings; 31-a sealing ring; 32-positioning surface; 33-high pressure cavity mold; 34-porous sintered ceramic; 35-1 of a high-pressure cavity mold core pressing plate; 36-1 of a high-pressure cavity mold core; 37-1-a low-pressure cavity mold core; 38-1-a low pressure cavity mold core pressing plate; 35-2-a high-pressure cavity mold core pressing plate; 36-2-high pressure cavity mold core; 37-2-low pressure cavity mold cores; 38-2-a low pressure cavity mold core pressing plate; 35-4-high pressure cavity mold core pressing plate; 36-4 of a high-pressure cavity mold core; 36-5-high pressure cavity mold cores; 36-6-high pressure cavity mold core; 37-5-low pressure cavity mold cores; 37-6-low pressure cavity mold core.
Detailed Description
As shown in FIG. 1, the hydrogen permeation/leakage/fatigue integrated measurement device and process of the invention comprise an air inlet pressurization system, a temperature control system, a test mold, a vacuumizing system, a hydrogen permeation/leakage amount detection system, a hydrogen circulation system and a safety system. The air inlet pressurizing system comprises a hydrogen storage bottle group 1, a pressure regulating valve 2, a one-way valve, a compressor, a temperature and pressure sensor, a buffer pipeline 7, an overflow valve 9 and a speed regulating pressure regulating valve 8. The temperature control system comprises buffer pipeline heating and cooling equipment, a temperature control system, a mold heating and cooling system and a temperature and pressure sensor. The test die comprises a high-pressure cavity die 33, a low-pressure cavity die 25, a sealing ring, a porous supporting plate and porous sintered ceramics. The vacuum pumping system comprises a vacuum pump 18, a temperature and pressure sensor and a vacuum pressure gauge. The hydrogen permeation/leakage detection system comprises a hydrogen mass spectrometer, a purging system and an inert gas source. The hydrogen circulation system comprises a compressor 20, a speed regulating valve 12, a hydrogen recovery tank 14, a one-way valve 16 and a pressure regulating valve 13. The safety system comprises an explosion-proof test box.
As shown in fig. 1, the specific connection mode of the hydrogen permeation/leakage/fatigue integrated measurement device and the technology of the invention is as follows: a plurality of pressure control channels with different levels are arranged between the hydrogen storage bottle group 1 and the buffer pipeline 7, and the pressure of hydrogen entering the buffer pipeline 7 is controlled through the pressure regulating valve 2 and the one-way valve. For the low-pressure test requirement, the hydrogen storage bottle group 1 is connected with the one-way valve 3 through the pressure regulating valve 2 and directly enters the buffer pipeline 7 for heating and cooling; for the middle-high pressure test requirement, after the hydrogen of the hydrogen storage bottle group 1 passes through the pressure regulating valve 2, the hydrogen enters the buffer pipeline 7 from the outlets of the middle-pressure compressor 4-1 and the high-pressure compressor 4-2 through the one-way valve respectively by the multistage compressor according to different pressure requirements for heating and cooling. The outlet of the buffer pipeline 7 is connected with an overflow valve 9, so that the risk of overpressure is prevented. After the hydrogen is subjected to temperature treatment through the buffer pipeline 7, the hydrogen enters the test die 11 through the pressure and speed regulating valve 8. During testing, hydrogen gas leaking from the seal ring 30/seal structure will be purged into the hydrogen mass spectrometer 24 from the side of the low pressure cavity die 25 to verify mass; hydrogen gas permeated from the test sample 29 will be purged into the hydrogen mass spectrometer 24 from the tail of the low pressure cavity die 25 to verify mass. The high pressure hydrogen after the test is completed may be discharged through the needle valve 15 or may be passed to the next cycle. For hydrogen to be circulated, after the single test is finished, the high-pressure chamber of the test die 11 passes through the speed regulating valve 12 and then enters the hydrogen recovery tank 14 from the one-way valve 16 or the compressor 20. The hydrogen recovery tank 14 is connected to the outlet position of the hydrogen storage bottle group pressure regulating valve 2 through a pressure regulating valve. The chambers, lines and environmental chambers are connected to a vacuum pump 18 via needle valves to vent the gases from the lines or chambers, respectively, for the vacuum requirements prior to testing. For the heating and cooling requirements of the buffer pipe 7 and the test mold 11, the temperature control system 24 can directly perform the heating and cooling treatment on the buffer pipe 7 and the test mold 11 through the environmental box 10.
As shown in fig. 2, the test die 11 of the hydrogen permeation/leakage/fatigue integrated measurement device and process of the present invention is composed of a high-pressure cavity die 33 and a low-pressure cavity die 25. The invention relates to a hydrogen permeation/leakage/fatigue integrated measurement device and a specific connection mode of a test die 11 according to the process, wherein the specific connection mode comprises the following steps: the high-pressure chamber die 33 and the low-pressure chamber die 25 are connected by axisymmetric fastening bolts, the number of which is preferably 6 or 8. The high-pressure cavity die 33 and the low-pressure cavity die 25 are positioned through the positioning surface 32 and are sealed in a circumferential direction through the sealing ring 31; in addition, a hydrogen gas test passage leaking from the position of the seal ring 30 is formed between the high-pressure chamber die 33 and the low-pressure chamber die 25. The sample 29 for the permeation test is mounted in such a manner that the metal support plate 26, the porous sintered ceramic 27 or the porous slide, the seal ring 28, the sample 29, the seal ring 30, the porous sintered ceramic 34 or the porous slide (optional), respectively, are installed from the low pressure chamber toward the axial direction of the high pressure chamber.
As shown in fig. 4, for some brittle materials such as nylon 6 or carbon fiber composite, which may be non-planar samples 29 after being formed into a liner, carbon fiber composite layer, or other alternative samples 29 using newly developed processes, it is difficult to forcibly flatten and seal in the test mold 11, which can easily lead to inaccurate results during testing. Thus, the high-pressure cavity mold 33 or the low-pressure cavity mold 25 of the test mold 11 according to the present invention may be composed of a replaceable mold core and a mold core pressing plate for fastening and pressing, and the mold core may be customized according to the shape of the sample, and the cost is lower than the cost of customizing the entire test mold 11. The core platen may limit axial movement of the high pressure cavity core. The combination mode of the mold core and the mold core pressing plate at one side comprises at least two modes: first, as shown in fig. 3, the high-pressure cavity mold core 36-1 or the low-pressure cavity mold core 37-1 is directly connected with an external pipeline, and the high-pressure cavity mold core pressing plate 35-1 or the low-pressure cavity mold core pressing plate 38-1 is mainly used for fastening the mold core and bearing high pressure. Second, as shown in FIG. 4, the high-pressure cavity mold core 36-2 or the low-pressure cavity mold core 37-2 is only used to adapt to the shape of the sample to form a test cavity; the external pipeline is directly connected with the high-pressure cavity mold core pressing plate 35-2 or the low-pressure cavity mold core pressing plate 38-2; compared with the first connecting mode, the connecting mode can avoid repeated disassembly and assembly to abrade the connecting surface between the external pipeline and the die, but the sealing surface is increased. The two connection modes can be adjusted according to specific requirements. When the test sample is a special-shaped surface and needs to be positioned, the mold core and the mold core pressing plate are suggested to be connected by adopting a rotation stopping structure, and the mold core pressing plate is fixedly connected with the mold or the mold core pressing plate on the other side by adopting bolts, as shown in fig. 3. The number of test dies 11 according to the present invention may be installed according to specific test requirements.
As an alternative to the screw fastening connection, the mold core press plates on both sides as shown in fig. 4 or the mold core press plate on one side and the mold on the other side as shown in fig. 5 can be directly fastened by screw threads. At this time, a connection mode capable of rotating is adopted between the mold core pressing plate and the mold core.
As shown in fig. 2, in the test die 11 according to the present invention, the sealing ring for sealing the sample 29 is preferably a sealing ring 28 of the low-pressure chamber with a diameter equal to or smaller than that of the sealing ring 30 of the high-pressure chamber.
The main function of the buffer pipeline 7 is to temporarily store high-pressure hydrogen needed by the test, so that the pressure in the high-pressure test cavity can be built up quickly or according to a preset pressurizing rate; in addition, the buffer pipe 7 can preheat/precool the high-pressure hydrogen for testing. As shown in FIG. 8, the buffer pipeline of the present invention is preferably a multi-layered structure, the inner layer 7-1 high pressure pipe of the buffer pipeline is used for storing hydrogen, and the outer layer 7-2 of the buffer pipeline is used for introducing heating or cooling liquid to preheat/precool the hydrogen in the inner layer 7-1 high pressure pipe. As a modification, the outer part of the buffer pipeline outer layer 7-2 can be coated with heat insulation materials.
The control valve of each position of the hydrogen permeation/leakage/fatigue integrated measuring equipment and the process is only used for clearly explaining the specific effect. It is within the scope of the present invention to use one valve body to combine two or more valve bodies or to split the function of one valve body into multiple valve bodies at a three-way position or other positions, as long as the primary function of the circuit is not changed. Part of the pipelines in the schematic diagram of the invention can also be replaced by valve plates.
Preferably, the hydrogen entering the high pressure chamber and the hydrogen leaving the high pressure chamber are controlled by computer servo.
As shown in fig. 1, a sample preparation process of the hydrogen permeation/leakage/fatigue integrated measurement device and process of the present invention comprises: the connection seal is reliable at all connection positions of the checking equipment. Test sample 29 is installed. Relief valve 9 sets a safety pressure, closes needle valve 15, opens all other valves to allow passage of the tubing and test chamber, and opens vacuum pump 18 to empty the system of air. If necessary, nitrogen or inert gas can be introduced into the pipelines in the system one by one to promote the oxygen in the pipelines to be emptied. When the low-pressure vacuum gauge stably reaches the set vacuum pressure, the needle valve 17, the needle valve 19, the needle valve 21 and the needle valve 22 are closed, then the vacuum pump 18 is closed, and all valves are closed.
The following examples are provided to aid in the testing of an integrated hydrogen permeation/leakage/fatigue testing apparatus of the present invention.
Example 1: the hydrogen permeation performance in the direction perpendicular to the sample was measured.
As shown in fig. 1, after the system is evacuated, hydrogen is supplied to the high pressure chamber at the pressure and temperature required for the sample testing. The temperature of the hydrogen in the buffer conduit 7 and the environmental chamber 10 and the temperature of the test mould 11 are controlled by a temperature control system 24. When the test pressure difference is low pressure, hydrogen can be directly supplied by the hydrogen storage bottle group 1, and the pressure regulating valve 2 and the one-way valve 3 are opened, so that the hydrogen with higher test pressure enters the buffer pipeline 7 for preheating/precooling. The pressure and speed regulating valve 8 is opened to enable the hydrogen with the regulated temperature, pressure and speed to enter the high-pressure chamber. When a medium pressure difference is needed, the pressure regulating valve 2, the compressor 4-1 and the one-way valve 5 can be opened to enable medium pressure hydrogen to enter the buffer pipeline 7. When a high-pressure differential pressure is needed, the pressure regulating valve 2, the compressor 4-1, the compressor 4-2 and the one-way valve 6 can be opened to enable high-pressure hydrogen to enter the buffer pipeline 7. The high-pressure hydrogen can be discharged a certain amount of hydrogen through the overflow valve 9 when the temperature and the pressure are exceeded, so that the safety of equipment is ensured. As shown in fig. 2, in the testing process, the compression condition of the sample 29 and the sealing ring can be controlled by adjusting the screw pretightening force between the high-pressure cavity mold and the low-pressure cavity mold, and the hydrogen permeation amount of the sample 29 and the hydrogen leakage amount of the sealing ring 30 of the high-pressure cavity are respectively connected into the hydrogen mass spectrometer 23 for verification through the lower side channel and the right side channel of the low-pressure cavity mold 25. After the test is finished, all valves are closed to form open circuit. The high-pressure hydrogen in the high-pressure chamber of the test die 11 and the buffer pipe 7 can enter the hydrogen recovery tank 14 through the speed regulating valve 12 and the check valve 16 or be directly emptied through the needle valve 15. After the hydrogen gas in the high pressure chamber cannot enter the hydrogen recovery tank 14 by the pressure difference driving, the hydrogen gas can be driven into the hydrogen recovery tank 14 by the compressor 20. After the test is finished, if the gas in the test cavity of the sealing ring is to be exhausted, the needle valve 21 and the vacuum pump 18 can be opened, and after the test is finished, the needle valve 21 is closed and then the vacuum pump 18 is closed. To evacuate the sample permeation testing chamber, needle valve 22 and vacuum pump 18 may be opened to evacuate, and after completion, needle valve 22 and vacuum pump 18 may be closed.
Example 2: and measuring the sealing performance of a circumferential sealing material such as a sealing ring or a metal-plastic connecting interface structure.
In the test, the treatment methods of hydrogen pressure build-up in the high-pressure chamber, and bleeding after the test is completed are the same as those of example 1.
When it is desired to measure the hydrogen diffusion properties of the non-metallic material interface or to subject the interface to high-pressure hydrogen treatment, as shown in fig. 6, a sample 29 of the metal-non-metallic connection can be produced by injection, molding, casting solidification, transfer molding, or the like. As necessary, the high pressure cavity mold core 36-4 is sealed with the high pressure cavity mold core platen 35-4 by a threaded connection and a sealing ring, preventing the high pressure cavity mold core 36-4 from moving axially to form a stable high pressure cavity. When high pressure hydrogen is applied to the outside of the connection structure, as shown in the left test structure in fig. 6. The amount of hydrogen leakage from the connection structure is equal to the amount of hydrogen entering the hydrogen mass spectrometer 23 from the lower side passage of the test die 11 minus the hydrogen permeation amount of the sample. When high pressure hydrogen is applied to the inside of the connection structure, as shown in the right test structure in fig. 6. The amount of hydrogen leakage from the connection structure is equal to the amount of hydrogen entering the hydrogen mass spectrometer 23 from the right-hand path of the test die 11
As shown in the left-hand structure of FIG. 7, when only the hydrogen sealing performance of the axial seal ring or other annular sealing material needs to be tested, the high-pressure cavity mold core 36-5 and the low-pressure cavity mold core 37-5 can be remanufactured for fixing the seal sample 29, and the compression condition of the seal ring can be controlled by adjusting the pretightening force of the bolt. Hydrogen gas leaking from the sealed sample 29 under test will enter the hydrogen mass spectrometer 23 through the channel on the right side of the test die 11 for verification.
As shown in the right-hand structure of FIG. 7, high pressure cavity mold core 36-6 and low pressure cavity mold core 37-6 may be remanufactured for holding seal sample 29 when only the hydrogen sealing performance of the annular seal ring or other annular sealing material is to be tested. The contact surface of the high-pressure cavity mold core 36-6 and the sealed sample 29 is a conical surface, and the surface of the low-pressure cavity mold core 37-6 for limiting the sealed sample 29 is a cylindrical surface. Therefore, the compression condition of the sealing ring can be controlled by the pretightening force of the adjusting bolt. Hydrogen gas leaking from the sealed sample 29 under test will enter the hydrogen mass spectrometer 23 through the channel on the right side of the test die 11 for verification.
Example 3: and (3) measuring crack growth and hydrogen permeability of the sample under the conditions of rapid decompression, hydrogen circulation and accelerated aging.
As shown in fig. 1, the hydrogen cycle and aging test process of sample 29 according to the present invention comprises: on the basis of a single hydrogen permeation/leakage test, the porous sintered ceramic 34 is removed, and the hydrogen rate entering the high-pressure chamber is controlled by controlling the pressure and speed regulating valve 8; the rate of hydrogen gas exiting the high pressure chamber is controlled by a speed valve 12, high pressure hydrogen gas is cycled on and off the high pressure chamber according to a set program, and the amount of hydrogen gas that permeates or leaks from the sample during the cycle is verified by a hydrogen mass spectrometer 23. The hydrogen gas in the hydrogen recovery tank 14 can be reused in the circulation system by the pressure regulating valve 13, and the inside and outside of the pipe are in a positive pressure difference state, so that other impurities are not mixed in the recovered hydrogen gas.
The foregoing examples are illustrative only and not intended to be limiting, and equivalent modifications and variations are possible within the scope of the invention as defined in the appended claims.
Claims (9)
1. A hydrogen permeation/leakage/fatigue integrated measurement device and process are characterized in that: the device comprises an air inlet pressurizing system, a temperature control system, a test die, a vacuumizing system, a hydrogen permeation/leakage amount detection system, a hydrogen circulation system and a safety system; the air inlet pressurizing system comprises a hydrogen storage bottle group, a pressure regulating valve, a one-way valve, a compressor, a temperature and pressure sensor, a buffer pipeline, an overflow valve and a speed regulating pressure regulating valve; the temperature control system comprises buffer pipeline heating and cooling equipment, a temperature control system, a mould heating and cooling system and a temperature and pressure sensor; the test die comprises a high-pressure cavity die, a low-pressure cavity die, a sealing ring, a porous supporting plate and porous sintered ceramic; the vacuumizing system comprises a vacuum pump, a temperature and pressure sensor and a vacuum pressure gauge; the hydrogen permeation/leakage detection system comprises a hydrogen mass spectrometer, a purging system and an inert gas source; the hydrogen circulation system comprises a compressor, a speed regulating valve, a hydrogen recovery tank, a one-way valve and a pressure regulating valve; the safety system comprises an explosion-proof test box.
2. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 1, wherein: the test die consists of a high-pressure cavity die and a low-pressure cavity die; the high-pressure cavity die and the low-pressure cavity die are positioned through the positioning surface, are sealed in a circumferential direction through the sealing surface, and form a sealing ring testing channel; the sample is installed in the axial direction from the low pressure chamber to the high pressure chamber by a metal support plate, porous sintered ceramic or porous slide, a sealing ring, a sample, a sealing ring, porous sintered ceramic or porous slide.
3. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 1, wherein: the high-pressure cavity die or the low-pressure cavity die of the test die can consist of a replaceable die core and a die core pressing plate for fastening and bearing, and the die core can be customized according to the appearance of a sample; the mold core pressing plate can limit the axial movement of the high-pressure cavity mold core; the combination modes of the mold core and the mold core pressing plate at one side are at least two, wherein one mold core is directly connected with an external pipeline, and the other mold core is connected with the mold core pressing plate; the two connection modes can be adjusted according to specific requirements; when the test sample is a special-shaped surface and needs to be positioned, the mold core and the mold core pressing plate are connected by adopting a rotation stopping structure, and the mold core pressing plate is preferably fastened and connected with the mold at the other side or the mold core pressing plate by adopting bolts; the mold core of the test mold can be replaced according to the size of the sealing ring, the sealing structure form of nonmetal-metal connection, the curved surface shape of the test sample and the like.
4. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 3, wherein: when it is desired to determine the sealing properties of the non-metallic material interface or to subject the interface to high pressure hydrogen treatment, the mold core should be fabricated as a sample of the metal-non-metallic connection with the non-metallic material by injection, molding, casting curing, transfer molding, etc.
5. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 2, wherein: the sealing ring for sealing the sample in the test die is preferably a sealing ring of which the diameter of the sealing ring of the high-pressure chamber is smaller than or equal to that of the sealing ring of the low-pressure chamber.
6. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 1, wherein: the buffer pipeline has the main function of temporarily storing high-pressure hydrogen required by the test and is used for preheating/precooling the high-pressure hydrogen for the test; the buffer pipeline is preferably of a multi-layer structure, the inner high-pressure pipe is used for storing hydrogen, and the outer layer is used for introducing heating or cooling liquid to preheat/precool the hydrogen in the high-pressure pipe; as a modification, the outer layer may be coated with a thermal insulation material.
7. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 1, wherein: the pressurizing system preferably controls pressure output through pressure regulating valves with different precision after pressurizing by the multi-stage compressors according to different pressure demands; namely, for the low-pressure test requirement, the hydrogen storage bottle group is connected with the one-way valve through the pressure regulating valve and directly enters the buffer pipeline for heating and cooling; for the middle-high pressure test requirement, after the hydrogen of the hydrogen storage bottle group passes through the pressure regulating valve, the multi-stage compressor can respectively enter the buffer pipeline through the one-way valve from the outlets of the middle-pressure compressor and the high-pressure compressor according to different pressure requirements for heating and cooling.
8. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 1, wherein: the buffer high-pressure pipeline heating and cooling equipment is preferably oil liquid heating and liquid nitrogen cooling; alternatively, the heating mode may be a resistance wire heating mode or an infrared heater heating mode; the environment box is heated by an infrared heating mode preferably and cooled by a liquid nitrogen cooling mode; alternatively, the heating means may be heated by hot air.
9. The hydrogen permeation/leakage/fatigue integrated measurement device and process according to claim 1, wherein: according to the hydrogen circulation and aging test process, on the basis of single hydrogen permeation/leakage test, the hydrogen rate entering the high-pressure chamber is controlled by controlling the pressure regulating and speed regulating valve, the hydrogen rate discharged from the high-pressure chamber is controlled by controlling the speed regulating valve, high-pressure hydrogen is loaded and discharged in the high-pressure chamber according to a set program circulation, and the amount of hydrogen permeated or leaked from a sample in the circulation process is verified by the hydrogen mass spectrometer.
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| CN116642776A (en) * | 2023-07-27 | 2023-08-25 | 浙江大学 | Material hydrogen induced cracking testing device and method for high-pressure hydrogen environment |
| CN116642776B (en) * | 2023-07-27 | 2024-01-02 | 浙江大学 | Material hydrogen induced cracking testing device and method for high-pressure hydrogen environment |
| CN117092010A (en) * | 2023-09-13 | 2023-11-21 | 中国特种设备检测研究院 | High-pressure hydrogen permeation test device and pressure difference test method for IV type gas cylinder liner material |
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