CN110118690A - A kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device - Google Patents

A kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device Download PDF

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CN110118690A
CN110118690A CN201910302862.2A CN201910302862A CN110118690A CN 110118690 A CN110118690 A CN 110118690A CN 201910302862 A CN201910302862 A CN 201910302862A CN 110118690 A CN110118690 A CN 110118690A
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hydrogen
environment cabinet
cabinet
natural gas
sample
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CN110118690B (en
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尚娟
花争立
郑津洋
顾超华
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/32Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0001Type of application of the stress
    • G01N2203/0003Steady
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0001Type of application of the stress
    • G01N2203/0005Repeated or cyclic
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014Type of force applied
    • G01N2203/0016Tensile or compressive
    • G01N2203/0019Compressive
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058Kind of property studied
    • G01N2203/006Crack, flaws, fracture or rupture
    • G01N2203/0067Fracture or rupture
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/022Environment of the test
    • G01N2203/0236Other environments
    • G01N2203/024Corrosive
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/026Specifications of the specimen
    • G01N2203/0262Shape of the specimen
    • G01N2203/0278Thin specimens
    • G01N2203/0282Two dimensional, e.g. tapes, webs, sheets, strips, disks or membranes

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)

Abstract

The present invention relates to material mechanical performance test equipments, it is desirable to provide a kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device.The device includes gas cylinders group, air-channel system and experimental enviroment case;The central upper portion of experimental enviroment case is equipped with vertical cavity passage and is inserted into loading axis, is correspondingly arranged counterbore in lower central, the edge of sample is clamped between upper and lower box;Steel ball is put at the upper surface center of sample, the two-way foil gauge of center arrangement in lower surface;Experimental enviroment case is connect by its porting with air-channel system.The present invention pushes steel ball using loading axis disk sheet metal specimens are applied with the method for load, avoids complicated servo test mechanism, reduces equipment volume, reduces cost;It avoids reducing the probability that hydrogen leaks using high pressure dynamic sealing element, improving the reliability and safety of device;Force frequency by increasing loading axis accelerates the fatigue failure of disk sheet metal specimens, shortens test period, improves test efficiency.

Description

A kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device
Technical field
The invention belongs to material mechanical performance test equipment, in particular to a kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device and.
Background technique
With continuing to optimize for China's energy resource structure, Renewable Energy Development is rapid.Although using wind energy and solar energy as generation The renewable energy of table rapidly develops, but wind/light power generation time intermittence and unpredictability limit it and be incorporated on a large scale The wind in mains network, especially China/light geographical resource is unevenly distributed weighing apparatus and results in power generation center to be separated with load centre, gives it Large-scale application causes serious " abandonment is rationed the power supply ".It is counted according to National Energy Board, only 2017, optical quantum is abandoned in China's abandonment Up to 41,900,000,000 kWh, abandonment rate are more than 12%.Day is mixed by extra wind-powered electricity generation or voltaic powered electrolysis hydrogen manufacturing, and by hydrogen obtained Right gas, form hydrogen loading natural gas (HCNG), then recycle existing gas distributing system to be conveyed, finally be used as traffic fuel, Fuel used to generate electricity and clean gas, it is considered to be solve the problems, such as extensive wind/photoelectricity consumption effective way, improving renewable energy Good environmental benefit can be also brought while source utilization rate, be with a wide range of applications.But the materialization with natural gas Matter is different, and high pressure hydrogen can deteriorate the mechanical property of metal material, cause the hydrogen damage of material.To ensure pipeline hydrogen loading day The safety of right gas, high pressure hydrogen loading natural gas environment material must carry out the experimental study of performance damage.
The research for carrying out the damage of high pressure hydrogen loading natural gas environmentally conscious materials performance, should be in true high pressure hydrogen loading natural gas Carry out the performance test of material under environment.This proposes higher requirement to corresponding experimental rig.Lack phase at present both at home and abroad The experimental rig answered.The device of only individual research institution's early developments for pure hydrogen environmentally conscious materials Mechanics Performance Testing, But above equipment all suffers from following critical issue:
(1) device structure is complicated, and there are security risks
Existing pure hydrogen environmentally conscious materials Mechanics Performance Testing device exists being transformed mostly by traditional material testing machine Installing is capable of providing the environmental cabinet of pure hydrogen environment needed for test on traditional material testing machine, to accommodate sample and its fixture, Volume inside environmental cabinet is commonly designed larger, and then causes environmental cabinet volume and wall thickness larger, and equipment overall structure is more multiple It is miscellaneous, it involves great expense.The inflammable and explosive medium of storage is more in environmental cabinet, and existing apparatus is added by piercing test machine environmental cabinet It carries axis to apply load to the sample of clamping, meter movable sealing structure is set up between loading axis and environmental cabinet contact surface to maintain to test Pressure inside case, still, movable sealing structure service life are limited, easily cause dielectric leakage, and there are larger security risks.
(2) testing efficiency is low, and time cost is high
Existing high pressure hydrogen loading natural gas environmentally conscious materials performance damaging device is slower to the sample application pressure loading of clamping, The single load experimental test to sample can not be fast implemented, loading axis force frequency is lower in constant pressure fatigue test, thus Cause test period at high cost, and test needs more people to operate equipment every time, experimental labor is at high cost.
Summary of the invention
The present invention is to solve critical issue existing for current test device and test method, proposes that a kind of high pressure hydrogen loading is natural Compression ring border material property Damage Evaluation device.
To solve critical issue, solution of the invention is:
A kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device is provided, including gas cylinders group, air-channel system and Experimental enviroment case;
The gas cylinders group includes being used to prepare the natural gas bottle group and hydrogen cylinder group of bulk testing gas, and for purging Argon bottle group;The air-channel system includes low pressure buffer tank, chromatograph, Pneumatic booster pump, high-pressure buffering pot and vacuum Pump;Natural gas bottle group, hydrogen cylinder group and argon bottle group pass through pipeline respectively and are connected to low pressure buffer tank and experimental enviroment case, and low pressure is slow It rushes tank outlet and chromatograph and Pneumatic booster pump is respectively connected to by pipeline, the outlet of Pneumatic booster pump is connected to high-pressure buffer Tank, high-pressure buffering pot outlet are connected by pipeline with experimental enviroment case;High-pressure buffering pot, experimental enviroment case and chromatograph Outlet is also connected to vacuum pump and blowdown piping by pipeline;
The experimental enviroment case and vertical loading axis are respectively mounted on the rack;Experimental enviroment case by top environment cabinet and Environment cabinet composition in lower part is positioned by tongue and groove between the two and realizes connection by bolt;At the center of top environment cabinet Equipped with vertical cavity passage, the lower end of vertical loading axis is inserted, and the two is clearance fit;The environment cabinet in lower part Center and cavity passage are correspondingly arranged counterbore similar in radial dimension, are equipped at the upper limb of counterbore for placing sheets shape sample Depressed area;After top environment cabinet is fixedly connected with lower part environment cabinet, the edge of sample is clamped between upper and lower box, Experimental enviroment case internal cavity is isolated into upper and lower two parts;Steel ball is put at the upper surface center of sample, in the following table of sample The two-way foil gauge of face center arrangement;Porting and stress section pin interfaces are set on the side wall of lower part environment cabinet, respectively Counterbore base is connected to by intake and exhaust channel and lead channels;One end of stress section lead connects two-way foil gauge, and the other end is by setting Lead sealing equipment in lead channels is drawn;Experimental enviroment case is connect by its porting with air-channel system.
In the present invention, on top, annular groove is arranged in the opposite junction of environment cabinet and lower part environment cabinet, built-in O-shaped Circle is used as sealing element.
In the present invention, the lower end of the loading axis is in inverted v-shaped.
In the present invention, the sample thin slice in the form of annular discs, the depressed area for placing sample has corresponding shape Shape.
In the present invention, between loading axis and the contact surface in top environment box cavity channel, sample and top environmental cabinet O-ring sealing element is set respectively between contact level, between sample and lower part environment cabinet contact surface.
In the present invention, valve is set on the pipeline between gas cylinders group exit and each equipment of air-channel system.
In the present invention, vertical passageway is set at counterbore base center, the intake and exhaust channel and lead channels are horizontally through Lower part environment cabinet, and it is connected to the bottom end of vertical passageway.
In the present invention, pressure reducing valve is set on the pipeline between low pressure buffer tank and chromatograph.
In the present invention, heat exchange jacket is respectively set on the outside of top environment cabinet and lower part environment cabinet, heat exchange jacket is logical Cross piping connection refrigerating and heating machine.
In the present invention, which further includes density of hydrogen detection device and control system;Density of hydrogen detector is set to upper In the cavity passage of portion's environment cabinet, control system is respectively connected to low pressure buffer tank, Pneumatic booster pump, high pressure by signal wire Surge tank, refrigerating and heating machine and density of hydrogen detection device.
In the present invention, top environment cabinet and lower part environment cabinet are by anti-hydrogen embrittlement PH stainless steel of good performance It is fabricated, steel ball is fabricated by high-strength steel.Load shaft diameter DJWith top environment box cavity channel diameter DkBe 50~ 80mm and be between the two clearance fit, loading axis end is in inverted v-shaped, and the angles of two bevel edges is 60~80 °, correspondingly, steel The diameter range of ball is 30~60mm.Disk sheet metal specimens with a thickness of 0.5~2mm, the diameter D of disk sheet metal specimensY=DK+ 30mm, the adjustable temperature range of heating agent is -80~150 DEG C in refrigerating and heating machine.The loading axis of testing machine has slow judgement of speed change Rate single load function, minimum strain loading rate are 10-7/ s, in addition, loading axis also has the function of reciprocating fatigue, maximum fatigue Frequency is 10Hz.The blowing pressure range of the blowing pressure range in 0~60MPa, high-pressure buffering pot in low pressure buffer tank exists 50~120MPa.
Inventive principle description:
The present invention, as sample, is placed a steel ball in disk sheet metal specimens side, utilizes load using disc-like wafer Axis pushes steel ball that disk sheet metal specimens are applied with load, the hydrogen loading natural gas of another side contacts high pressure of disk sheet metal specimens, To realize effect of disk sheet metal specimens while contacting high pressure hydrogen loading natural gas by load.The deployable master of the device Testing type includes single load test, constant pressure hydrogen loading natural gas fatigue test and delayed fracture test.Single load test It is to continue to apply load to disk sheet metal specimens with constant strain rate by control loading axis, until disk sheet metal specimens are broken It splits, to realize the test of disk sheet metal specimens single load limiting pressure, and in an argon atmosphere with disk sheet metal specimens The comparison of single load limiting pressure size, obtains the single load damage index of disk sheet metal specimens.Constant pressure hydrogen loading natural gas is tired The hydrogen loading gas pressure for keeping disk sheet metal specimens to be born during labor test is constant, but its load born is followed Ring variation, thus the corresponding fatigue behaviour of test material, and respectively recording disc sheet metal specimens in hydrogen loading natural gas environment and The fatigue life cycle undergone before rupturing in ar gas environment, is calculated the fatigue damage index of disk sheet metal specimens.Delay is disconnected Splitting test is to keep the hydrogen loading natural gas air pressure of its contact constant and pressure maintaining one by applying certain load to disk sheet metal specimens Section the time, if disk sheet metal specimens are not cracked, again carry out test and increase disk sheet metal specimens receiving load with And its hydrogen loading natural gas air pressure of contact, it so recycles, until disk sheet metal specimens are cracked.Using proposed by the invention Experimental rig and method can obtain single load limiting pressure, the single load damage index, tired longevity of disk sheet metal specimens Life, fatigue damage index, delayed fracture ultimate load and hydrogen loading natural gas limit air pressure etc., above-mentioned data can be used to evaluate material Performance damage under high pressure hydrogen loading natural gas environment.
Compared with the existing technology, the beneficial effects of the present invention are:
1, steel ball is pushed disk sheet metal specimens are applied with the method for load using loading axis, avoid complicated servo examination Mechanism is tested, equipment volume greatly reduces, and equipment cost reduces;
2, it avoids having used high pressure dynamic sealing element in device, the probability that hydrogen leaks can be reduced, improve device Reliability and safety;
3, the mistake of disk sheet metal specimens can be accelerated by constant strain rate size when improving loading axis single load Effect rupture, the force frequency by increasing loading axis accelerates the fatigue failure of disk sheet metal specimens, when can shorten test in this way Between, greatly improve test efficiency;
4, these three materials are tested by single load test, constant pressure hydrogen loading natural gas fatigue test and delayed fracture Energy test method can study the damage of high pressure hydrogen loading natural gas environmentally conscious materials performance in many aspects;
5, heat medium temperature is controlled to which the temperature during guarantee test is kept constant and meets examination by refrigerating and heating machine Temperature requirement is tested, while influence test of the temperature to hydrogen embrittlement can be carried out;
6, it can analyze the measurement of each component content in hydrogen/natural oxygen mixture using chromatograph, and then adjust The content of each component is, it can be achieved that the accurate proportion of hydrogen/natural oxygen mixture in whole mixed gas;
7, top environment cabinet, disk sheet metal specimens can be constituted with loading axis using density of hydrogen detection device close It closes space and carries out hydrogen gas leakage detection, facilitate and judge whether disk sheet metal specimens rupture.
Detailed description of the invention
Fig. 1 is general arrangement schematic diagram of the invention;
Fig. 2 is experimental enviroment case and its internal structure chart of the invention.
In figure: natural gas bottle group 1, hydrogen cylinder group 2, low pressure buffer tank 3, pressure reducing valve 4, chromatograph 5, Pneumatic booster pump 6, high-pressure buffering pot 7, blow valve 8, blowdown piping 9, vavuum pump valve 10, vacuum pump 11, loading axis 12, top environment cabinet 13, lower part environment cabinet 14, refrigerating and heating machine 15, branch blow valve 16, flow control valve 17, high-pressure buffering pot outlet valve 18, control system 19, replacement piping 20, argon bottle group 21, heating agent feed line 22, heating agent 23, O-ring sealing element 24, on Portion's heat exchange jacket 25, lower part heat exchange jacket 26, heating agent return line 27, steel ball 28, two-way foil gauge 29, lead sealing equipment 30, bolt 31, porting 32, density of hydrogen detection device 33, disk sheet metal specimens 34.
Specific embodiment
High pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device in the present embodiment is as depicted in figs. 1 and 2, including Propose the natural gas bottle group 1 for the natural gas that is for experiment, the hydrogen cylinder group 2 for mentioning the hydrogen that is for experiment, for displaced argon bottle group 21, The exhaust outlet of natural gas bottle group 1 and hydrogen cylinder group 2 is connected to low pressure buffer tank 3, and the outlet of low pressure buffer tank 3 is divided into two-way: It is connected to Pneumatic booster pump 6 all the way, is then high-pressure buffering pot 7, the exhaust outlet of high-pressure buffering pot 7 is connected to lower part environment cabinet Lower part environment cabinet porting 32 on 14;It is connected to pressure reducing valve 4 all the way, is then chromatograph 5.Utilize chromatography Instrument 5 can measure each component content in hydrogen/natural oxygen mixture, and then adjust each component content ratio in mixed gas, Realize the accurate proportion of hydrogen/natural oxygen mixture.Be provided in above-mentioned pipeline flow control valve 17, replacement piping 20, Refrigerating and heating machine 15, vacuum pump 11 etc., wherein flow control valve 17 is used to control hydrogen/natural gas gaseous mixture charge and discharge speed Rate;Argon bottle group 21 and lower part environment cabinet porting 32, Ke Yizhi are connected dedicated for the replacement piping 20 of gas displacement Row argon gas purging lower part environment cabinet 14 is tapped into, to achieve the purpose that gas displacement;From lower part environment cabinet porting 32 Equipped with the blowdown piping 9 for being directly connected to low pressure buffer tank 3, high-pressure buffering pot 7 and vacuum pump 11, start vacuum pump 11, opens low The valve on surge tank 3, high-pressure buffering pot 7 and lower part environment cabinet porting 32 and 11 connecting line of vacuum pump is pressed, it can It is vented the gas of 14 the inside of low pressure buffer tank 3, high-pressure buffering pot 7 and lower part environment cabinet.Whole system is controlled by control system 19 System.
As shown in Fig. 2, the experimental enviroment case of testing machine is made of top environment cabinet 13 and lower part environment cabinet 14, Middle and upper part environment cabinet 13 and lower part environment cabinet 14 are fabricated by anti-hydrogen embrittlement PH stainless steel of good performance, with The life and reliability of guarantee test environmental cabinet;It is positioned between top environment cabinet 13 and lower part environment cabinet 14 by tongue and groove Blending bolt 31 is attached, and junction is sealed using O-ring sealing element 24;12 diameter D of loading axisJWith top environmental cabinet 13 cavity passage diameter D of bodykIt is 50~80mm and is between the two clearance fit, 12 end of loading axis is in inverted v-shaped, and two tiltedly The angle on side is 60~80 °;Disk sheet metal specimens 34 with a thickness of 0.5~2mm, diameter DY=DK+30mm;On-test it Before two-way foil gauge 29 can be installed at 34 lower surface center of disk sheet metal specimens, after arranging lead sealing equipment 30, by disk Sheet metal specimens 34 are mounted in the groove of lower part environment cabinet 14, to measure during the test corresponding of disk sheet metal specimens 34 Strain parameter variation, the corresponding displacement Parameters variation data of disk sheet metal specimens 34 during the test can pass through control system 19 Monitoring loading axis 12 obtains;Steel ball 28, cavity of the steel ball 28 in top environment cabinet 13 is arranged in 34 upper surface of disk sheet metal specimens It in channel, is fabricated by high-strength steel, to be able to bear the load of the application of loading axis 12 and then can be applied to disk sheet metal specimens 34 Add enough pressure, the diameter range of steel ball 28 is 30~60mm, ensure that its replacement is convenient;Loading axis 12 and top environmental cabinet It is all provided between body 13, between disk sheet metal specimens 34 and top environment cabinet 13, between disk sheet metal specimens 34 and lower part environment cabinet 14 O-ring sealing element 24 is set to be sealed;Refrigerating and heating machine 15 connects heating agent feed line 22 and heating agent return line 27, passes through 23 temperature of heating agent is controlled to control test gas within the scope of test required temperature;By top environment cabinet 13, disk thin slice The confined space lining that sample 34 and loading axis 12 are constituted sets density of hydrogen detection device 33, for carrying out hydrogen gas leakage detection, To judge whether disk sheet metal specimens 34 rupture.
The application method of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device of the present invention is introduced below.
One, the single load testing method of hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device is utilized:
As depicted in figs. 1 and 2, firstly, dropping to loading axis 12 higher than at top environment cabinet 13, top environment is separated Cabinet 13 and lower part environment cabinet 14 will be equipped with after the two-way foil gauge 29 of arrangement at 34 lower surface center of disk sheet metal specimens The disk sheet metal specimens 34 of two-way foil gauge 29 are placed in the groove of lower part environment cabinet 14, arrange lead sealing equipment 30 Afterwards, it is aligned the tongue and groove of top environment cabinet 13 and lower part environment cabinet 14 respectively, by top environment cabinet 13 and lower part environment Cabinet 14 engages, and blending bolt 31 is attached;Secondly, in the cavity passage inner disk sheet metal specimens 34 of top environment cabinet 13 Upper surface place steel ball 28, loading axis 12 is dropped to the place of slightly above steel ball 28, is made centainly using refrigerating and heating machine 15 The heating agent 23 of temperature is flowed into top heat exchange jacket 25 and lower part heat exchange jacket 26 and is full of from heating agent feed line 22, then from Heating agent return line 27 returns in refrigerating and heating machine 15, loops back and forth like this, until off-test, during guarantee test Temperature keep constant and meet test temperature requirement;Then, the voltage division formulas in Dalton's law (of partial pressures): P is utilizedB=PAlwaysVB/ VAlwaysAnd pressure size needed for the accounting size calculating hydrogen of hydrogen total pressure in experimental condition, it is taken out using vacuum pump 11 Residual air in experimental rig and subsidiary pipeline carries out low pressure buffer tank 3 after vacuum degree reaches setting value in system Hydrogen fills, and carries out natural gas charging after Hydrogen Vapor Pressure reaches setting value in low pressure buffer tank 3, then to low pressure buffer tank 3, directly After natural gas/hydrogen gas mixture pressure reaches setting value in low pressure buffer tank 3, terminate gas filling, opens connection low pressure The pressure reducing valve 4 of surge tank 3 carries out the survey of each component content using chromatograph 5 to the mixed gas in low pressure buffer tank 3 Amount carries out next step if hydrogen, natural Gas content that measurement obtains meet experimental condition, if being unsatisfactory for experimental condition, It is adjusted correspondingly according to measurement result until measuring obtained hydrogen, natural Gas content meets experimental condition;Using pneumatic Booster pump 6 carries out high pressure hydrogen/natural oxygen mixture to high-pressure buffering pot 7 and fills, until hydrogen/day in high-pressure buffering pot 7 After right gas mixture pressure reaches setting value, loading axis 12 is reduced, until two-way 29 registration of foil gauge is close to zero and will be big Width increases, and stops decline;Flow control valve 17 and high-pressure buffering pot outlet valve 18 are opened, and guarantees that branch blow valve 16 closes It closes, enters the hydrogen in high-pressure buffering pot 3/natural gas gaseous mixture in lower part environment cabinet 14 with specific rate, until examination It tests the intracorporal air pressure of environmental cabinet and reaches test requirements document;Record the load cell readings S of loading axis 12 at this time1, pass through loading axis 12 with 10-5/ s~10-7The constant strain rate of/s forces in steel ball 28 to apply load to disk sheet metal specimens 34, until Disk sheet metal specimens 34 rupture, and the strain and displacement at 34 center of recording disc sheet metal specimens during the test, record circle The load cell readings S of loading axis 12 after disk sheet metal specimens 34 rupture2, the difference (S of load cell readings twice2-S1) i.e. For the stress size of disk sheet metal specimens 34;Blow valve 8 is closed, vavuum pump valve 10, branch blow valve 16 and flow control are opened Valve 17 processed carries out lower part environment cabinet 14 and its attached pipeline using vacuum pump 11 to be evacuated to setting vacuum degree, and Vacuum pump 11 is closed afterwards;It is several to the hydrogen in respective line/natural gas gaseous mixture progress using argon gas by replacement piping 20 After secondary displacement, top environment cabinet 13 and lower part environment cabinet 14 are separated, takes out disk sheet metal specimens 34.So far, hydrogen loading is natural The single load off-test of compression ring border lower disc sheet metal specimens 34.Carry out disk sheet metal specimens 34 in an argon atmosphere below Performance test.Therewith preamble it is rapid unlike: argon gas directly is carried out to low pressure buffer tank 3 and is filled, until low pressure buffer tank 3 Pressure settings in hydrogen loading natural gas environmental testing before interior argon pressure reaches, hydrogen loading natural gas later also all become For argon gas;The difference for being recorded twice load cell readings is S4-S3, then disk sheet metal specimens 34 are in hydrogen environment and argon gas Stress ratio (S in environment2-S1)/(S4-S3) be disk sheet metal specimens 34 single load damage index.
Two, it is tested using the constant pressure hydrogen loading natural gas fatigue test of hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device Method:
As depicted in figs. 1 and 2, firstly, measuring and recording the thickness of disk sheet metal specimens 34, loading axis 12 is declined supreme At top environment cabinet 13, top environment cabinet 13 and lower part environment cabinet 14 are separated, in 34 lower surface of disk sheet metal specimens After arranging two-way foil gauge 29 at center, the disk sheet metal specimens 34 equipped with two-way foil gauge 29 are placed on lower part environment cabinet In 14 groove, after arranging lead sealing equipment 30, it is aligned the recessed of top environment cabinet 13 and lower part environment cabinet 14 respectively Tongue engages top environment cabinet 13 and lower part environment cabinet 14, and blending bolt 31 is attached;Secondly, in top environment Steel ball 28 is placed in the upper surface of the cavity passage inner disk sheet metal specimens 34 of cabinet 13, and loading axis 12 is dropped to slightly above steel ball 28 place makes the heating agent 23 of certain temperature flow into top heat exchange jacket 25 from heating agent feed line 22 using refrigerating and heating machine 15 With in lower part heat exchange jacket 26 and be full of, then from heating agent return line 27 back to refrigerating and heating machine 15 in, so recycle past It is multiple, until off-test, is kept constant with the temperature during guarantee test and meets test temperature requirement;Then, road is utilized Voltage division formulas in your law of partial pressure: PB=PAlwaysVB/VAlwaysAnd the accounting size of hydrogen total pressure in experimental condition calculates Pressure size needed for hydrogen takes out the residual air in experimental rig and subsidiary pipeline using vacuum pump 11, until in system After vacuum degree reaches setting value, hydrogen is carried out to low pressure buffer tank 3 and is filled, reaches setting to Hydrogen Vapor Pressure in low pressure buffer tank 3 After value, then natural gas charging is carried out to low pressure buffer tank 3, until natural gas/hydrogen gas mixture pressure reaches in low pressure buffer tank 3 To after setting value, terminate gas filling, opens the pressure reducing valve 4 of connection low pressure buffer tank 3, it is slow to low pressure using chromatograph 5 The mixed gas rushed in tank 3 carries out the measurement of each component content, if hydrogen, natural Gas content that measurement obtains meet test bar Part then carries out next step, if being unsatisfactory for experimental condition, is adjusted correspondingly according to measurement result until what measurement obtained Hydrogen, natural Gas content meet experimental condition;It is mixed that high pressure hydrogen/natural gas is carried out to high-pressure buffering pot 7 using Pneumatic booster pump 6 Gas filling is closed, after hydrogen/natural gas mixture pressure reaches setting value in high-pressure buffering pot 7, opens flow control valve Door 17 and high-pressure buffering pot outlet valve 18, and guarantee that branch blow valve 16 is closed, make hydrogen/natural gas in high-pressure buffering pot 3 Gaseous mixture is entered in lower part environment cabinet 14 with specific rate, until the intracorporal air pressure of experimental enviroment case reaches test requirements document, T at the time of record gas filling terminates1;Pressure maintaining for a period of time, observes the reading of density of hydrogen detection device 33, until its reading It is not zero, records this moment T2, 34 thickness of disk sheet metal specimens, concentration and the time (T that are obtained according to measurement2-T1), utilize phenanthrene Gram diffusion second law calculate hydrogen diffusion coefficient;Record the reading Y of two-way foil gauge 29 at this time1, loading axis 12 is reduced, until The two-way reading of foil gauge 29 is-Y1, to test the reciprocal loading axis 12 of frequency cycle of setting, make the two-way reading of foil gauge 29 in Y1 ~-Y1Between change, and then cyclic loading is applied to disk sheet metal specimens 34, until density of hydrogen detection device 33 reads quickly Increase, and the strain and displacement at 34 center of recording disc sheet metal specimens during the test;Recording disc sheet metal specimens 34 are broken The fatigue life cycle F undergone before splitting1, lower part environment cabinet 14 and its attached pipeline are vacuumized using vacuum pump 11 To setting vacuum degree, vacuum pump 11 is then closed;Using argon gas by replacement piping 20 to the hydrogen in experimental enviroment case and pipeline Gas/natural gas gaseous mixture carries out after replacing several times, separates top environment cabinet 13 and lower part environment cabinet 14, and it is thin to take out disk Piece sample 34.So far, the constant pressure hydrogen loading natural gas fatigue test of hydrogen loading natural gas environment lower disc sheet metal specimens 34 terminates.Below Carry out the fatigue property test of disk sheet metal specimens 34 in an argon atmosphere.Therewith preamble it is rapid unlike: directly to low Pressure surge tank 3 carries out argon gas and fills, until before argon pressure reaches in low pressure buffer tank 3 in hydrogen loading natural gas environmental testing Pressure settings, hydrogen loading natural gas later also all becomes argon gas;Recording disc sheet metal specimens 34 are broken in an argon atmosphere The fatigue life cycle F undergone before splitting2, the ratio (F of fatigue life cycle twice1/F2) be disk sheet metal specimens 34 fatigue Damage index.
Three, the delayed fracture testing method of hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device is utilized:
As depicted in figs. 1 and 2, firstly, dropping to loading axis 12 higher than at top environment cabinet 13, top environment is separated Cabinet 13 and lower part environment cabinet 14 will be equipped with after the two-way foil gauge 29 of arrangement at 34 lower surface center of disk sheet metal specimens The disk sheet metal specimens 34 of two-way foil gauge 29 are placed in the groove of lower part environment cabinet 14, arrange lead sealing equipment 30 Afterwards, it is aligned the tongue and groove of top environment cabinet 13 and lower part environment cabinet 14 respectively, by top environment cabinet 13 and lower part environment Cabinet 14 engages, and blending bolt 31 is attached;Its place that loading axis 12 is dropped to slightly above steel ball 28, building one are close The test cavity closed makes the heating agent 23 of certain temperature flow into top heat exchange folder from heating agent feed line 22 using refrigerating and heating machine 15 It in set 25 and lower part heat exchange jacket 26 and is full of, then returns in refrigerating and heating machine 15 from heating agent return line 27, so follow Ring is reciprocal, until off-test, is kept constant with the temperature during guarantee test and meet test temperature requirement;Then, sharp With the voltage division formulas in Dalton's law (of partial pressures): PB=PAlwaysVB/VAlwaysAnd hydrogen big subtotal of the accounting of total pressure in experimental condition Pressure size needed for calculating hydrogen, takes out the residual air in experimental rig and subsidiary pipeline using vacuum pump 11, until system After interior vacuum degree reaches setting value, hydrogen is carried out to low pressure buffer tank 3 and is filled, reaches to Hydrogen Vapor Pressure in low pressure buffer tank 3 and sets After definite value, then natural gas charging is carried out to low pressure buffer tank 3, until natural gas/hydrogen gas mixture pressure in low pressure buffer tank 3 After reaching setting value, terminate gas filling, the pressure reducing valve 4 of connection low pressure buffer tank 3 is opened, using chromatograph 5 to low pressure Mixed gas in surge tank 3 carries out the measurement of each component content, if hydrogen, natural Gas content that measurement obtains meet test bar Part then carries out next step, if being unsatisfactory for experimental condition, is adjusted correspondingly according to measurement result until what measurement obtained Hydrogen, natural Gas content meet experimental condition;It is mixed that high pressure hydrogen/natural gas is carried out to high-pressure buffering pot 7 using Pneumatic booster pump 6 Gas filling is closed, after hydrogen/natural gas mixture pressure reaches setting value in high-pressure buffering pot 7, opens flow control valve Door 17 and high-pressure buffering pot outlet valve 18, and guarantee that branch blow valve 16 is closed, make hydrogen/natural gas in high-pressure buffering pot 3 Gaseous mixture is entered in lower part environment cabinet 14 with specific rate, until the intracorporal air pressure of experimental enviroment case reaches test setting value P1, loading axis 12 is reduced, by forcing in steel ball 28 to apply load to disk sheet metal specimens 34, until two-way foil gauge 29 Reading be manufacture disk sheet metal specimens 34 the aerial yield strength Q of material;Pressure maintaining 10h, and remember during the test The reading for recording two-way foil gauge 29 be evacuated to setting using vacuum pump 11 to lower part environment cabinet 14 and its attached pipeline Determine vacuum degree, then closes vacuum pump 11;Using argon gas by replacement piping 20 to hydrogen/day in experimental enviroment case and pipeline Right gas gaseous mixture carries out after replacing several times, separates top environment cabinet 13 and lower part environment cabinet 14, takes out the examination of disk thin slice Sample 34, whether observation disk sheet metal specimens 34 are cracked, if cracked, off-test, if without cracked, it will Pressure settings in experimental enviroment case are adjusted to nP1, loading axis 12 is Q+ to the magnitude of load that disk sheet metal specimens 34 apply (n-1) × 50, wherein n value is to test duplicate number, for example, if desired carrying out testing for second, then in experimental enviroment case Pressure settings are 2P1, loading axis 12 is Q+50 to the magnitude of load that disk sheet metal specimens 34 apply;It repeats to test, until circle Disk sheet metal specimens 34 are cracked.
As described above, forcing in steel ball 28 using loading axis 12 with the frequency of setting and then applying to disk sheet metal specimens 34 The load of certain frequency avoids complicated servo test mechanism, and weight of equipment, volume greatly reduce, and cost reduces, test Efficiency improves, and hydrogen/gas consumption is few in test;All sealing elements in device are all static seal O-ring sealing element 24, it avoids using high pressure dynamic sealing element, the probability that hydrogen leaks can be reduced, improve the reliability and safety of device Property;Density of hydrogen detection device 33, strain detection testing device 29, displacement monitor, that is, control system 19 in device be not by high pressure Hydrogen/natural gas influences, signal stabilization;23 temperature of heating agent is controlled using refrigerating and heating machine 15, thus during guarantee test Temperature keeps constant and meets test temperature requirement, while can carry out influence test of the temperature to hydrogen embrittlement;Utilize chromatograph 5 It can analyze the measurement of each component content in hydrogen/natural oxygen mixture, and then adjust the content of each component in mixed gas, The accurate proportion of hydrogen/natural oxygen mixture can be achieved;It can be to top environment cabinet using density of hydrogen detection device 33 13, the confined space that disk sheet metal specimens 34 and loading axis 12 are constituted carries out hydrogen gas leakage detection, facilitates and judges that disk thin slice tries Whether sample 34 ruptures.
The above is only case study on implementation of the invention, not does limitation in any form to the present invention, although The present invention is disclosed as above with preferable case study on implementation, and however, it is not intended to limit the invention, any technology people for being familiar with this profession Member, without departing from the scope of the present invention, when making certain changes using the structure and technology contents of the disclosure above Or modify and become the equivalence enforcement case of equivalent variations.
Anything that does not depart from the technical scheme of the invention according to the technical essence of the invention make the above case study on implementation Any simple modification, equivalent change and modification, still fall within the scope of technical solution of the present invention.

Claims (10)

1. a kind of high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device, including gas cylinders group, air-channel system and proving ring Border case;It is characterized in that,
The gas cylinders group includes being used to prepare the natural gas bottle group and hydrogen cylinder group of bulk testing gas, and the argon for purging Gas cylinders group;The air-channel system includes low pressure buffer tank, chromatograph, Pneumatic booster pump, high-pressure buffering pot and vacuum pump;It Right gas cylinders group, hydrogen cylinder group and argon bottle group pass through pipeline respectively and are connected to low pressure buffer tank and experimental enviroment case, low pressure buffer tank Outlet is respectively connected to chromatograph and Pneumatic booster pump by pipeline, and the outlet of Pneumatic booster pump is connected to high-pressure buffering pot, high The outlet of pressure surge tank is connected by pipeline with experimental enviroment case;The outlet of high-pressure buffering pot, experimental enviroment case and chromatograph Vacuum pump and blowdown piping are also connected to by pipeline;
The experimental enviroment case and vertical loading axis are respectively mounted on the rack;Experimental enviroment case is by top environment cabinet and lower part Environment cabinet composition is positioned by tongue and groove between the two and realizes connection by bolt;On top, the center of environment cabinet is equipped with The lower end of vertical cavity passage, vertical loading axis is inserted, and the two is clearance fit;At the center of lower part environment cabinet It is correspondingly arranged counterbore similar in radial dimension with cavity passage, the recess for placing sheets shape sample is equipped at the upper limb of counterbore Position;After top environment cabinet is fixedly connected with lower part environment cabinet, the edge of sample is clamped between upper and lower box, test Environmental cabinet internal cavity is isolated into upper and lower two parts;Steel ball is put at the upper surface center of sample, in the lower surface of sample The heart arranges two-way foil gauge;Porting and stress section pin interfaces are set on the side wall of lower part environment cabinet, respectively by into Exhaust passage and lead channels are connected to counterbore base;One end of stress section lead connects two-way foil gauge, and the other end is drawn by being set to Lead sealing equipment in line passage is drawn;Experimental enviroment case is connect by its porting with air-channel system.
2. the apparatus according to claim 1, which is characterized in that on top, environment cabinet and the opposite of lower part environment cabinet connect Place's setting annular groove is connect, built-in O-ring is as sealing element.
3. the apparatus according to claim 1, which is characterized in that the lower end of the loading axis is in inverted v-shaped.
4. the apparatus according to claim 1, which is characterized in that the sample thin slice in the form of annular discs, for placing sample Depressed area has corresponding shape.
5. the apparatus according to claim 1, which is characterized in that in the contact of loading axis and top environment box cavity channel It is close that O-ring is set respectively between face, between sample and top environment cabinet contact surface, between sample and lower part environment cabinet contact surface Seal element.
6. the apparatus according to claim 1, which is characterized in that between gas cylinders group exit and each equipment of air-channel system Valve is set on pipeline.
7. the apparatus according to claim 1, which is characterized in that at counterbore base center, vertical passageway is set, it is described into row Gas channel and lead channels are horizontally through lower part environment cabinet, and are connected to the bottom end of vertical passageway.
8. the apparatus according to claim 1, which is characterized in that on the pipeline between low pressure buffer tank and chromatograph Pressure reducing valve is set.
9. the apparatus according to claim 1, which is characterized in that on the outside of top environment cabinet and lower part environment cabinet respectively Heat exchange jacket is set, and heat exchange jacket passes through piping connection refrigerating and heating machine.
10. according to claim 1 to device described in 9 any one, which is characterized in that the device further includes density of hydrogen detection Device and control system;Density of hydrogen detector is set in the cavity passage of top environment cabinet, and control system passes through signal wire It is respectively connected to low pressure buffer tank, Pneumatic booster pump, high-pressure buffering pot, refrigerating and heating machine and density of hydrogen detection device.
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