CN110082201A - Material delayed fracture test method under high pressure hydrogen loading natural gas environment - Google Patents

Material delayed fracture test method under high pressure hydrogen loading natural gas environment Download PDF

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CN110082201A
CN110082201A CN201910302864.1A CN201910302864A CN110082201A CN 110082201 A CN110082201 A CN 110082201A CN 201910302864 A CN201910302864 A CN 201910302864A CN 110082201 A CN110082201 A CN 110082201A
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hydrogen
pressure
natural gas
test
environment cabinet
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CN110082201B (en
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郑津洋
尚娟
花争立
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
    • G01N3/02Details
    • 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
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • 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
    • G01N2203/023Pressure
    • G01N2203/0232High pressure
    • 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

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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 measuring technologies, it is desirable to provide the material delayed fracture test method under a kind of high pressure hydrogen loading natural gas environment.The present invention pushes steel ball by loading axis to apply load to disk sheet metal specimens, 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, carrying out delayed fracture test data acquired can be used to evaluate performance damage of the material under high pressure hydrogen loading natural gas environment.The invention avoids complicated servo test mechanisms to reduce cost with reducing equipment volume;The probability that hydrogen leaks is reduced, the reliability and safety of device are improved;Shorten test period, improves test efficiency;Meet test temperature requirement, carries out influence test of the temperature to hydrogen embrittlement;Realize the accurate proportion of hydrogen/natural oxygen mixture;Hydrogen gas leakage detection is carried out using density of hydrogen detection device, facilitates and judges whether disk sheet metal specimens rupture.

Description

Material delayed fracture test method under high pressure hydrogen loading natural gas environment
Technical field
Material the invention belongs to material mechanical performance measuring technology, in particular under a kind of high pressure hydrogen loading natural gas environment Delayed fracture test method.
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 loading axis frequency that exerts a force is lower, to cause test period at high cost, and test needs more people to operate equipment every time, experimental labor at This height.
Summary of the invention
The technical problem to be solved by the present invention is to overcome prior art Shortcomings, propose a kind of high pressure hydrogen loading natural gas Material delayed fracture test method under environment.
To solve critical issue, solution of the invention is:
A kind of material delayed fracture test method under high pressure hydrogen loading natural gas environment is provided, comprising the following steps:
(1) high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device is built
Natural gas bottle group, hydrogen cylinder group and argon bottle group are passed through into pipeline respectively and are connected to low pressure buffer tank and experimental enviroment Case, the outlet of low pressure buffer tank are 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-pressure buffering pot outlet are connected by pipeline with experimental enviroment case;High-pressure buffering pot, experimental enviroment case and chromatography The outlet of analyzer also passes through pipeline and is connected to vacuum pump and blowdown piping;
Experimental enviroment case and vertical loading axis are installed on the rack;Experimental enviroment case is by top environment cabinet and lower loop Cabinet composition in border is positioned by tongue and groove between the two and realizes connection by bolt;On top, the center of environment cabinet is equipped with perpendicular To cavity passage, the lower end of vertical loading axis is inserted, and the two is clearance fit;In lower part the center of environment cabinet with Cavity passage is correspondingly arranged counterbore similar in radial dimension, and the recessed portion for placing sheets shape sample is equipped at the upper limb of counterbore Position;Porting and stress section pin interfaces are equipped on the side wall of lower part environment cabinet, respectively by intake and exhaust channel and lead Channel is connected to counterbore base;One end of stress section lead connects two-way foil gauge, and the other end is by the lead in lead channels Sealing device is drawn;Experimental enviroment case is connect by its porting with air-channel system;
(2) top environment cabinet and lower part environment cabinet are separated, is installed at the lower surface center of disk flake sample After two-way foil gauge, sample is put into the depressed area at the environment cabinet counterbore upper limb of lower part, and arranges lead-in wire sealing dress It sets;It is aligned the tongue and groove of top environment cabinet and lower part environment cabinet, top environment cabinet and lower part environment cabinet are engaged, and It is attached with bolt;
(3) steel ball is placed at the upper surface center of sample, steel ball is located in the cavity passage of top environment cabinet;It will load Axis drops to the place of slightly above steel ball;
Enter heating agent in heat exchange jacket from heating agent feed line using refrigerating and heating machine, is then returned from heating agent return line It returns in refrigerating and heating machine and keeps circulating, it is constant with the temperature of experimental enviroment case during guarantee test and meet test Temperature requirement;
(4) voltage division formulas in Dalton's law (of partial pressures): PB=PAlwaysVB/VAlways, i.e., the partial pressure of component gas B be equal to gas it is total The product of pressure and the volume fraction of component gas B;Using Dalton law of partial pressure and hydrogen, total pressure is accounted in experimental condition Pressure size needed for calculating hydrogen than size, then takes out the residual air in experimental rig and subsidiary pipeline with vacuum pump, After vacuum degree reaches setting value in system, hydrogen is carried out to low pressure buffer tank and is filled, to Hydrogen Vapor Pressure in low pressure buffer tank After reaching setting value, then natural gas charging is carried out to low pressure buffer tank, until natural gas/hydrogen gas mixture in low pressure buffer tank After pressure reaches setting value, terminate gas filling;The pressure reducing valve for opening connection low pressure buffer tank, using chromatograph to low pressure Mixed gas in surge tank 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, it is adjusted correspondingly according to measurement result until what measurement obtained Hydrogen, natural Gas content meet experimental condition;
(5) it carries out high pressure hydrogen/natural gas gaseous mixture to high-pressure buffering pot using Pneumatic booster pump to fill, until high pressure is slow It rushes pressure inside the tank and reaches setting value;Enter the gaseous mixture in high-pressure buffering pot in experimental enviroment case by valve control, until The intracorporal air pressure of experimental enviroment case reaches setting value P1, loading axis is reduced, by forcing in steel ball to disk sheet metal specimens Apply load, until the reading of two-way foil gauge is the aerial yield strength Q of material for manufacturing disk sheet metal specimens;
(6) pressure maintaining 10h, and the reading of two-way foil gauge is recorded during the test;Using vacuum pump to experimental enviroment case And associated ping carries out being evacuated to setting vacuum degree, closes vacuum pump;If being carried out using argon gas to experimental enviroment case and pipeline After dry displacement, top environment cabinet and lower part environment cabinet are separated, sample is taken out;Whether cracked sample is observed, if going out Existing crackle then off-test, if without carrying out next step if cracked;
(7) step (2)-(6) are repeated, until sample is cracked;Wherein, change experimental enviroment when repeating step (5) Air pressure setting value in case is nP1And loading axis is Q+ (n-1) × 50 to the magnitude of load that disk sheet metal specimens apply;It is logical The mode that overweight retrial is tested, obtain final sample it is cracked when test number of repetition n.
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, 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, 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, valve is set on the pipeline between gas cylinders group exit and each equipment of air-channel system, it is slow in low pressure It rushes on the pipeline between tank and chromatograph and pressure reducing valve is set.
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, density of hydrogen detector is set in the cavity passage of top environment cabinet, and control system passes through signal Line 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.
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 device can carry out delay Destructive test keeps the hydrogen loading natural gas air pressure of its contact constant and pressure maintaining by applying certain load to disk sheet metal specimens For a period of time, if disk sheet metal specimens are not cracked, carry out the load for testing and increasing disk sheet metal specimens receiving again And the hydrogen loading natural gas air pressure of its contact, it so recycles, until disk sheet metal specimens are cracked.Data acquired can be used to comment Performance damage of the valence material 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, 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;
5, 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;
6, 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
Hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device used in the present embodiment is as depicted in figs. 1 and 2, including mentions Be for experiment natural gas natural gas bottle group 1, mention the hydrogen that is for experiment hydrogen cylinder group 2, for displaced argon bottle group 21, day The exhaust outlet of right gas cylinders 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: one Road is connected to Pneumatic booster pump 6, is then high-pressure buffering pot 7, and the exhaust outlet of high-pressure buffering pot 7 is connected to lower part environment cabinet 14 On lower part environment cabinet into (row) port 32;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 are connected into (row) port 32 dedicated for the replacement piping 20 of gas displacement, it can be with It directly carries out argon gas and purges lower part environment cabinet 14, to achieve the purpose that gas displacement;From lower part environment cabinet into (row) gas Mouth 32 is 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, starts vacuum pump 11, beats Low pressure buffer tank 3, high-pressure buffering pot 7 and lower part environment cabinet are opened into the valve on (row) port 32 and 11 connecting line of vacuum pump Door can be 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 by control system 19 controls.
As using example: top environment cabinet 13 and lower part environment cabinet 14 are by anti-hydrogen embrittlement precipitation-hardening of good performance Type stainless steel is fabricated, and steel ball 28 is fabricated by high-strength steel.Load shaft diameter DJWith 13 cavity passage of top environment cabinet Diameter DkIt is 50~80mm and between the two for clearance fit, loading axis end is in inverted v-shaped, and the angle of two bevel edges is 60~ 80 °, correspondingly, the diameter range of steel ball 28 is 30~60mm.Disk sheet metal specimens 34 with a thickness of 0.5~2mm, disk thin slice The diameter D of sample 34Y=DK+ 30mm, the adjustable temperature range of heating agent is -80~150 DEG C in refrigerating and heating machine 15.Testing machine Loading axis have the function of slow strain rate single load, minimum strain loading rate is 10-7/ s, in addition, loading axis also has Reciprocating fatigue function, maximum fatigue frequency is 10Hz.For the blowing pressure range in low pressure buffer tank 3 in 0~60MPa, high pressure is slow The blowing pressure range in tank 7 is rushed in 50~120MPa.
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 between the two for clearance fit, 12 end of loading axis is in inverted " v " shape, and two The angle of bevel edge is 60~80 °;Disk sheet metal specimens 34 with a thickness of 0.5~2mm, diameter DY=DK+30mm;On-test Two-way foil gauge 29 can be installed at 34 lower surface center of disk sheet metal specimens before, after arranging lead sealing equipment 30, will be justified Disk sheet metal specimens 34 are mounted in the groove of lower part environment cabinet 14, to measure the phase of disk sheet metal specimens 34 during the test Strain parameter is answered to change, 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 obtain;Steel ball 28, sky of the steel ball 28 in top environment cabinet 13 is arranged in 34 upper surface of disk sheet metal specimens In chamber channel, it is fabricated by high-strength steel, it in turn can to disk sheet metal specimens 34 to be able to bear the load of the application of loading axis 12 Apply enough pressure, the diameter range of steel ball 28 is 30~60mm, ensure that its replacement is convenient;Loading axis 12 and top environment Between cabinet 13, between disk sheet metal specimens 34 and top environment cabinet 13, between disk sheet metal specimens 34 and lower part environment cabinet 14 Setting O-ring sealing element 24 is sealed;Refrigerating and heating machine 15 connects heating agent feed line 22 and heating agent return line 27, leads to 23 temperature of control heating agent is crossed to test test gas control within the scope of required temperature;Thin by top environment cabinet 13, disk The confined space lining that piece sample 34 and loading axis 12 are constituted sets density of hydrogen detection device 33, for carrying out hydrogen gas leakage inspection It surveys, to judge whether disk sheet metal specimens 34 rupture.
Utilize the delayed fracture testing method of hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device:
Firstly, dropping to loading axis 12 higher than at top environment cabinet 13, top environment cabinet 13 and lower loop are separated Border cabinet 14 will be equipped with two-way foil gauge 29 after the two-way foil gauge 29 of arrangement at 34 lower surface center of disk sheet metal specimens Disk sheet metal specimens 34 are placed in the groove of lower part environment cabinet 14, after arranging lead sealing equipment 30, respectively in alignment The tongue and groove of portion's environment cabinet 13 and lower part environment cabinet 14 engages top environment cabinet 13 and lower part environment cabinet 14, and It is attached with bolt 31;Its place that loading axis 12 is dropped to slightly above steel ball 28 constructs a closed test cavity, The heating agent 23 of certain temperature is changed from the inflow top heat exchange jacket 25 of heating agent feed line 22 and lower part using refrigerating and heating machine 15 It in thermal jacket 26 and is full of, then returns in refrigerating and heating machine 15, loop back and forth like this from heating agent return line 27, until examination End is tested, kept constant with the temperature during guarantee test and meets test temperature requirement;Then, it is fixed to be divided using dalton Voltage division formulas in rule: PB=PAlwaysVB/VAlwaysAnd the accounting size of hydrogen total pressure in experimental condition calculates needed for hydrogen Pressure size takes out the residual air in experimental rig and subsidiary pipeline using vacuum pump 11, until vacuum degree reaches in system After setting value, hydrogen is carried out to low pressure buffer tank 3 and is filled, after Hydrogen Vapor Pressure reaches setting value in low pressure buffer tank 3, then to low Surge tank 3 is pressed to carry out natural gas charging, after natural gas/hydrogen gas mixture pressure reaches setting value in low pressure buffer tank 3, Terminate gas filling, open the pressure reducing valve 4 of connection low pressure buffer tank 3, using chromatograph 5 to mixed in low pressure buffer tank 3 The measurement that gas carries out each component content is closed to carry out next if hydrogen, natural Gas content that measurement obtains meet experimental condition Step is adjusted correspondingly until measuring obtained hydrogen, natural gas according to measurement result and contains if being unsatisfactory for experimental condition Amount meets experimental condition;It carries out high pressure hydrogen/natural oxygen mixture to high-pressure buffering pot 7 using Pneumatic booster pump 6 to fill, directly After hydrogen/natural gas mixture pressure reaches setting value in high-pressure buffering pot 7, flow control valve 17 and high-pressure buffer are opened Tank outlet valve 18, and guarantee that branch blow valve 16 is closed, make hydrogen/natural gas gaseous mixture in high-pressure buffering pot 3 with specific Rate enters in lower part environment cabinet 14, until the intracorporal air pressure of experimental enviroment case reaches test setting value P1, reduce loading axis 12, by forcing in steel ball 28 to apply load to disk sheet metal specimens 34, until the reading of two-way foil gauge 29 is manufacture The aerial yield strength Q of the material of disk sheet metal specimens 34;Pressure maintaining 10h, and two-way foil gauge is recorded during the test 29 reading 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;Using argon gas by replacement piping 20 to the hydrogen in experimental enviroment case and pipeline/natural gas gaseous mixture It carries out after replacing several times, separates top environment cabinet 13 and lower part environment cabinet 14, take out disk sheet metal specimens 34, observation circle Whether disk sheet metal specimens 34 are cracked, if cracked, off-test, if without cracked, by experimental enviroment case Interior pressure settings are adjusted to nP1, loading axis 12 is Q+ (n-1) × 50 to the magnitude of load that disk sheet metal specimens 34 apply, Wherein n value is to test duplicate number, for example, if desired carry out testing for second, then pressure settings in experimental enviroment case For 2P1, loading axis 12 is Q+50 to the magnitude of load that disk sheet metal specimens 34 apply;It repeats to test, until disk sheet metal specimens 34 is cracked.Repeat test by way of, obtain final sample it is cracked when test number of repetition n.
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 a 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, however, it is not intended to limit the invention, any skill for being familiar with this profession Art personnel, without departing from the scope of the present invention, when the structure and technology contents using the disclosure above make it is certain Change 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 this The technical spirit of invention still falls within the present invention to any simple modification, equivalent change and modification made by the above case study on implementation In technical proposal scope.

Claims (8)

1. the material delayed fracture test method under a kind of high pressure hydrogen loading natural gas environment, which comprises the following steps:
(1) high pressure hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device is built
Natural gas bottle group, hydrogen cylinder group and argon bottle group are passed through into pipeline respectively and are connected to low pressure buffer tank and experimental enviroment case, it is low The outlet of pressure surge tank is respectively connected to chromatograph and Pneumatic booster pump by pipeline, and it is slow that the outlet of Pneumatic booster pump is connected to high pressure Tank is rushed, high-pressure buffering pot outlet is connected by pipeline with experimental enviroment case;High-pressure buffering pot, experimental enviroment case and chromatograph Outlet also pass through pipeline and be connected to vacuum pump and blowdown piping;
Experimental enviroment case and vertical loading axis are installed on the rack;Experimental enviroment case is by top environment cabinet and lower part environmental cabinet Body 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 vertically The lower end of cavity passage, vertical loading axis is inserted, and the two is clearance fit;The center of environment cabinet and cavity in lower part Channel is correspondingly arranged counterbore similar in radial dimension, and the depressed area for placing sheets shape sample is equipped at the upper limb of counterbore; Porting and stress section pin interfaces are equipped on the side wall of lower part environment cabinet, respectively by intake and exhaust channel and lead channels It is connected to counterbore base;One end of stress section lead connects two-way foil gauge, and the other end is by the lead-in wire sealing in lead channels Device is drawn;Experimental enviroment case is connect by its porting with air-channel system;
(2) top environment cabinet and lower part environment cabinet are separated, is installed at the lower surface center of disk flake sample two-way After foil gauge, sample is put into the depressed area at the environment cabinet counterbore upper limb of lower part, and arrange lead sealing equipment;It is right The tongue and groove of neat top environment cabinet and lower part environment cabinet, top environment cabinet and lower part environment cabinet is engaged, and use spiral shell Bolt is attached;
(3) steel ball is placed at the upper surface center of sample, steel ball is located in the cavity passage of top environment cabinet;It will be under loading axis It is down to the place of slightly above steel ball;
Enter heating agent in heat exchange jacket from heating agent feed line using refrigerating and heating machine, is then returned to from heating agent return line In refrigerating and heating machine and keep circulating, it is constant with the temperature of experimental enviroment case during guarantee test and meet test temperature It is required that;
(4) voltage division formulas in Dalton's law (of partial pressures): PB=PAlwaysVB/VAlways, i.e., the partial pressure of component gas B be equal to gas stagnation pressure with The product of the volume fraction of component gas B;Using Dalton law of partial pressure and hydrogen, the accounting of total pressure is big in experimental condition Then pressure size needed for small calculating hydrogen takes out the residual air in experimental rig and subsidiary pipeline with vacuum pump, until After vacuum degree reaches setting value in system, hydrogen is carried out to low pressure buffer tank and is filled, is reached to Hydrogen Vapor Pressure in low pressure buffer tank After setting value, then natural gas charging is carried out to low pressure buffer tank, until natural gas/hydrogen gas mixture pressure in low pressure buffer tank After reaching setting value, terminate gas filling;The pressure reducing valve for opening connection low pressure buffer tank, using chromatograph to low pressure buffer Mixed gas in tank carries out the measurement of each component content, if hydrogen, natural Gas content that measurement obtains meet experimental condition, Carry out next step;If being unsatisfactory for experimental condition, according to measurement result be adjusted correspondingly until measure obtain hydrogen, Natural Gas content meets experimental condition;
(5) it carries out high pressure hydrogen/natural gas gaseous mixture to high-pressure buffering pot using Pneumatic booster pump to fill, until high-pressure buffering pot Interior pressure reaches setting value;Enter the gaseous mixture in high-pressure buffering pot in experimental enviroment case by valve control, until test The intracorporal air pressure of environmental cabinet reaches setting value P1, loading axis is reduced, disk sheet metal specimens are applied by forcing in steel ball Load, until the reading of two-way foil gauge is the aerial yield strength Q of material for manufacturing disk sheet metal specimens;
(6) pressure maintaining 10h, and the reading of two-way foil gauge is recorded during the test;Using vacuum pump to experimental enviroment case and attached Belong to pipeline to carry out being evacuated to setting vacuum degree, closes vacuum pump;Experimental enviroment case and pipeline are carried out several times using argon gas After displacement, top environment cabinet and lower part environment cabinet are separated, takes out sample;Whether cracked sample is observed, if splitting Line then off-test, if without carrying out next step if cracked;
(7) step (2)-(6) are repeated, until sample is cracked;Wherein, change in experimental enviroment case when repeating step (5) Air pressure setting value be nP1And loading axis is Q+ (n-1) × 50 to the magnitude of load that disk sheet metal specimens apply;Pass through weight The mode that retrial is tested, obtain final sample it is cracked when test number of repetition n.
2. the method according to claim 1, wherein connecting in top environment cabinet and the opposite of lower part environment cabinet Place's setting annular groove is connect, built-in O-ring is as sealing element.
3. the method according to claim 1, wherein 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.
4. the method according to claim 1, wherein the lower end of the loading axis is in inverted v-shaped.
5. the method according to claim 1, wherein sample thin slice in the form of annular discs, for placing sample Depressed area has corresponding shape.
6. the method according to claim 1, wherein between gas cylinders group exit and each equipment of air-channel system Valve is set on pipeline, pressure reducing valve is set on the pipeline between low pressure buffer tank and chromatograph.
7. the method according to claim 1, wherein counterbore base center be arranged vertical passageway, 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 method according to claim 1, wherein density of hydrogen detector is set to the cavity of top environment cabinet In channel, control system is respectively connected to low pressure buffer tank, Pneumatic booster pump, high-pressure buffering pot, cooling and warming by signal wire Machine and density of hydrogen detection device.
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