CN110095359A - Material fatigue damage test method under high pressure hydrogen loading natural gas environment - Google Patents

Material fatigue damage test method under high pressure hydrogen loading natural gas environment Download PDF

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CN110095359A
CN110095359A CN201910302833.6A CN201910302833A CN110095359A CN 110095359 A CN110095359 A CN 110095359A CN 201910302833 A CN201910302833 A CN 201910302833A CN 110095359 A CN110095359 A CN 110095359A
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hydrogen
pressure
natural gas
gas
environment cabinet
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CN110095359B (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
    • G01N3/02Details
    • 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
    • G01N3/32Investigating 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
    • 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
    • G01N2203/0001Type 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
    • G01N2203/0069Fatigue, creep, strain-stress relations or elastic constants
    • G01N2203/0073Fatigue
    • 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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  • 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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  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)

Abstract

The present invention relates to material mechanical performance measuring technologies, it is desirable to provide the material fatigue damage 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, 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 to disk sheet metal specimens.The fatigue life cycle undergone before rupture in hydrogen loading natural gas environment and in ar gas environment by recording disc sheet metal specimens, the fatigue damage index of disk sheet metal specimens is calculated, 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, reduce equipment volume, and equipment cost reduces;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.

Description

Material fatigue damage 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 Fatigue and damage experiment 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, is given Its large-scale application causes serious " abandonment is rationed the power supply ".By extra wind-powered electricity generation or voltaic powered electrolysis hydrogen manufacturing, and by hydrogen obtained Natural gas is mixed, forms hydrogen loading natural gas (HCNG), existing gas distributing system is then recycled to be conveyed, it is final to be used as friendship Logical 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 Good environmental benefit can be also brought while renewable energy utilization rate, be with a wide range of applications.But with it is natural The physico-chemical property of gas is different, and high pressure hydrogen can deteriorate the mechanical property of metal material, cause the hydrogen damage of material.To ensure pipe Road conveys the safety of hydrogen loading natural gas, and 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 all by piercing test machine environmental cabinet Loading axis to apply load to the sample of clamping, and meter movable sealing structure is set up between loading axis and environmental cabinet contact surface to maintain Pressure inside chamber, still, movable sealing structure service life are limited, easily cause dielectric leakage, and there are larger safety is hidden Suffer from.
(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, Loading axis force frequency is lower in constant pressure fatigue test, to cause test period at high cost, and test needs more people behaviour every time Make equipment, experimental labor is at high cost.
Summary of the invention
The technical problem to be solved by the present invention is to overcome prior art Shortcomings, provide a kind of high pressure hydrogen loading natural gas Material fatigue damage test method under environment.
To solve critical issue, solution of the invention is:
A kind of material fatigue damage 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 color The outlet of spectrum analysis instrument 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;At the center of lower part environment cabinet It is correspondingly arranged counterbore similar in radial dimension with cavity passage, is equipped at the upper limb of counterbore for the recessed of placing sheets shape sample Concave portion 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 channels are connected to counterbore base;One end of stress section lead connects two-way foil gauge, and the other end is by being set in lead channels Lead sealing equipment 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, Blending 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 add Carry the place that axis drops to 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 examination 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 mixed gas in low pressure buffer tank After body pressure reaches setting value, terminate gas filling;The pressure reducing valve for opening connection low pressure buffer tank, utilizes chromatograph pair Mixed gas in low pressure buffer tank carries out the measurement of each component content, if hydrogen, natural Gas content that measurement obtains meet examination Condition is tested, then carries out next step;If being unsatisfactory for experimental condition, it is adjusted correspondingly according to measurement result until measuring Obtained hydrogen, natural Gas content meets experimental condition;
(5) it carries out 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;Then gaseous mixture is made to set rate and enter in the environment cabinet of lower part by valve control, proving ring Border case is intracorporal until air pressure reaches test requirements document, T at the time of record gas filling terminates1
(6) pressure maintaining to the reading that density of hydrogen detection device measures is not zero, and records this moment T2;According to sample thickness, Density of hydrogen and time (T2-T1), hydrogen diffusion coefficient is calculated using Fick diffusion second law;
(7) the reading Y of two-way foil gauge at this time is recorded1, loading axis is reduced, until two-way foil gauge reading is-Y1, to set Determine the reciprocal loading axis of frequency cycle, makes two-way foil gauge reading in Y1~-Y1Between change, to piece sample apply cyclic loading, Increased until density of hydrogen detection device is read with 1.5 times of the rate that variation each second is former reading;Remember during the test Record the strain and displacement at sample center;
(8) the fatigue life cycle F undergone before specimen broke is recorded1, using vacuum pump to experimental enviroment case and attachment tube Road is evacuated to setting vacuum degree, closes vacuum pump;It is replaced several times using argon gas, separation top environment cabinet is under Portion's environment cabinet takes out sample;
(9) step (2), (3) are repeated, the residual air of experimental enviroment case and air-channel system, Zhi Daozhen are taken out with vacuum pump Reciprocal of duty cycle reaches setting value;It carries out argon gas to low pressure buffer tank to fill, until argon pressure reaches step (5) in low pressure buffer tank Middle hydrogen/natural gas gaseous mixture charge pressure;High pressure argon gas is carried out to high-pressure buffering pot using Pneumatic booster pump to fill, until After argon pressure reaches setting value in high-pressure buffering pot;The argon gas in high-pressure buffering pot is set to enter proving ring by valve control In the case of border, until air pressure reaches test requirements document;It repeats step (7), the fatigue that record sample is undergone before rupturing in an argon atmosphere Cycle-index F2;Calculate the ratio (F of fatigue life cycle twice1/F2), which is the fatigue damage index of sample.
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 perseverance The fatigue test of hydrogen loading natural gas is pressed, the hydrogen loading gas pressure for keeping disk sheet metal specimens to be born during test is constant, but Circulation change occurs for its load born, thus the corresponding fatigue behaviour of test material, and recording disc sheet metal specimens respectively The fatigue life cycle undergone before rupture in hydrogen loading natural gas environment and in ar gas environment, is calculated disk sheet metal specimens Fatigue damage index.Data acquired can be used to evaluate performance damage of the 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 fatigue failure that can accelerate disk sheet metal specimens by increasing the force frequency of loading axis, can shorten in this way Test period greatly improves 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 environmental cabinet Body 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, Top heat exchange jacket 25, lower part heat exchange jacket 26, heating agent return line 27, steel ball 28, two-way foil gauge 29, lead-in wire sealing dress Set 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, 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 environmental cabinet Lower part environment cabinet on body 14 is into (row) port 32;It is connected to pressure reducing valve 4 all the way, is then chromatograph 5.Utilize color Spectrum analysis instrument 5 can measure each component content in hydrogen/natural oxygen mixture, and then adjust each component in mixed gas and contain Ratio is measured, realizes the accurate proportion of hydrogen/natural oxygen mixture.Flow control valve 17, displacement are provided in above-mentioned pipeline Pipeline 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 rate;Argon bottle group 21 and lower part environment cabinet are connected into (row) port dedicated for the replacement piping 20 of gas displacement 32, argon gas purging lower part environment cabinet 14 can be directly carried out, to achieve the purpose that gas displacement;From lower part environment cabinet The blowdown piping 9 for being directly connected to low pressure buffer tank 3, high-pressure buffering pot 7 and vacuum pump 11 is equipped with into (row) port 32, starting is true Sky pump 11 is opened low pressure buffer tank 3, high-pressure buffering pot 7 and lower part environment cabinet and is connect into (row) port 32 with vacuum pump 11 Valve on pipeline 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.Entire system System is controlled by control system 19.
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 is between the two 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 The diameter D of sheet metal specimens 34Y=DK+ 30mm, the adjustable temperature range of heating agent is -80~150 DEG C in refrigerating and heating machine 15.Examination The loading axis for testing machine has the function of that slow strain rate single load, 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 in low pressure buffer tank 3 in 0~60MPa, The blowing pressure range in high-pressure buffering pot 7 is 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;Pass through tongue and groove between top environment cabinet 13 and lower part environment cabinet 14 Positioning blending bolt 31 is attached, and junction is sealed using O-ring sealing element 24;12 diameter D of loading axisJWith top 13 cavity passage diameter D of environment cabinetkIt is 50~80mm and is between the two clearance fit, 12 end of loading axis is in inverted " V " Font, the angle of two bevel edges are 60~80 °;Disk sheet metal specimens 34 with a thickness of 0.5~2mm, diameter DY=DK+30mm; Two-way foil gauge 29 can be installed before on-test at 34 lower surface center of disk sheet metal specimens, arrange lead sealing equipment After 30, disk sheet metal specimens 34 are mounted in the groove of lower part environment cabinet 14, are being tested with measuring disk sheet metal specimens 34 Corresponding strain parameter variation in the process, the corresponding displacement Parameters variation data of disk sheet metal specimens 34 during the test can Loading axis 12 is monitored by control system 19 to obtain;Steel ball 28 is arranged in 34 upper surface of disk sheet metal specimens, and steel ball 28 is in top loop It in the cavity passage of border cabinet 13, is fabricated by high-strength steel, to be able to bear the load of the application of loading axis 12 and then to disk Sheet metal specimens 34 can apply enough pressure, and the diameter range of steel ball 28 is 30~60mm, ensure that its replacement is convenient;Load Between axis 12 and top environment cabinet 13, between disk sheet metal specimens 34 and top environment cabinet 13, disk sheet metal specimens 34 and lower part O-ring sealing element 24 is respectively provided between environment cabinet 14 to be sealed;Refrigerating and heating machine 15 connects heating agent feed line 22 and heat Matchmaker's return line 27 is controlled test gas within the scope of test required temperature by control 23 temperature of heating agent;By top loop The confined space lining that border cabinet 13, disk sheet metal specimens 34 and loading axis 12 are constituted sets density of hydrogen detection device 33, is used to Hydrogen gas leakage detection is carried out, to judge whether disk sheet metal specimens 34 rupture.
Utilize the material fatigue damage test method of hydrogen loading natural gas environmentally conscious materials performance Damage Evaluation device:
Firstly, measuring and recording the thickness of disk sheet metal specimens 34, loading axis 12 is dropped to higher than top environment cabinet At 13, top environment cabinet 13 and lower part environment cabinet 14 are separated, is arranged at 34 lower surface center of disk sheet metal specimens two-way After foil gauge 29, the disk sheet metal specimens 34 equipped with two-way foil gauge 29 are placed in the groove of lower part environment cabinet 14, cloth After having set lead sealing equipment 30, it is aligned the tongue and groove of top environment cabinet 13 and lower part environment cabinet 14 respectively, by top loop Border cabinet 13 and lower part environment cabinet 14 engage, and blending bolt 31 is attached;Secondly, in the cavity of top environment cabinet 13 Steel ball 28 is placed in the upper surface of channel inner disk sheet metal specimens 34, and loading axis 12 is dropped to the place of slightly above steel ball 28, benefit The heating agent 23 of certain temperature is set to flow into top heat exchange jacket 25 and lower part heat exchange from heating agent feed line 22 with refrigerating and heating machine 15 It in collet 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 divided using dalton Voltage division formulas in law: PB=PAlwaysVB/VAlwaysAnd the accounting size of hydrogen total pressure in experimental condition calculates needed for hydrogen Pressure size, the residual air in experimental rig and subsidiary pipeline is taken out using vacuum pump 11, until vacuum degree reaches in system To 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 Natural gas charging is carried out to low pressure buffer tank 3, until natural gas/hydrogen gas mixture pressure reaches setting in low pressure buffer tank 3 After value, terminate gas filling, the pressure reducing valve 4 of connection low pressure buffer tank 3 is opened, using chromatograph 5 to low pressure buffer tank 3 Interior mixed gas carries out the measurement of each component content, if hydrogen, natural Gas content that measurement obtains meet experimental condition, Next step is carried out, if being unsatisfactory for experimental condition, is adjusted correspondingly according to measurement result until measuring obtained hydrogen Gas, 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 Number is not zero, and records this moment T2, 34 thickness of disk sheet metal specimens, density of hydrogen and the time (T that are obtained according to measurement2-T1), Hydrogen diffusion coefficient is calculated using Fick diffusion second law;Record the reading Y of two-way foil gauge 29 at this time1, reduce loading axis 12, until two-way foil gauge 29 reading is-Y1, to test the reciprocal loading axis 12 of frequency cycle of setting, make two-way foil gauge 29 Reading is in Y1~-Y1Between change, and then cyclic loading is applied to disk sheet metal specimens 34, until density of hydrogen detection device 33 Reading is increased with 1.5 times of the rate that variation each second is former reading, and during the test in recording disc sheet metal specimens 34 Strain and displacement at the heart;The fatigue life cycle F that recording disc sheet metal specimens 34 are undergone before rupturing1, right using vacuum pump 11 Lower part environment cabinet 14 and its attached pipeline carry out being evacuated to setting vacuum degree, then close vacuum pump 11;Use argon gas The hydrogen in experimental enviroment case and pipeline/natural gas gaseous mixture is carried out after replacing several times by replacement piping 20, in separation Portion's environment cabinet 13 and lower part environment cabinet 14 take out disk sheet metal specimens 34.So far, hydrogen loading natural gas environment lower disc is thin The constant pressure hydrogen loading natural gas fatigue test of piece sample 34 terminates.In an argon atmosphere tired of disk sheet metal specimens 34 is carried out below Labor 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 Pressure settings before argon pressure reaches in tank 3 in hydrogen loading natural gas environmental testing, hydrogen loading natural gas later are also complete All become argon gas;The fatigue life cycle F that recording disc sheet metal specimens 34 are undergone before rupturing in an argon atmosphere2, tired twice Ratio (the F of cycle-index1/F2) be disk sheet metal specimens 34 fatigue damage index.
As described above, forcing in steel ball 28 using loading axis 12 with the frequency of setting and then being applied to disk sheet metal specimens 34 The load for adding 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 the sealing of static seal O type circle Element 24 is avoided using high pressure dynamic sealing element, can be reduced the probability that hydrogen leaks, be improved the reliability of device And safety;Density of hydrogen detection device 33, strain detection testing device 29, displacement monitor, that is, control system 19 in device It is not influenced by high pressure hydrogen/natural gas, signal stabilization;23 temperature of heating agent is controlled using refrigerating and heating machine 15, thus guarantee test Temperature in the process keeps constant and meets test temperature requirement, while can carry out influence test of the temperature to hydrogen embrittlement;Utilize color Spectrum analysis instrument 5 can analyze the measurement of each component content in hydrogen/natural oxygen mixture, and then adjust each in mixed gas The content of component is, it can be achieved that the accurate proportion of hydrogen/natural oxygen mixture;It can be right using density of hydrogen detection device 33 The confined space that top environment cabinet 13, disk sheet metal specimens 34 and loading axis 12 are constituted carries out hydrogen gas leakage detection, conveniently sentences Whether disconnected disk sheet metal specimens 34 rupture.
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 fatigue damage 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 hydrogen/natural gas gaseous mixture to high-pressure buffering pot using Pneumatic booster pump to fill, until high-pressure buffering pot internal pressure Power reaches setting value;Then gaseous mixture is made to set rate and enter in the environment cabinet of lower part by valve control, experimental enviroment case Intracorporal T at the time of air pressure reaches test requirements document, and record gas filling terminates1
(6) pressure maintaining to the reading that density of hydrogen detection device measures is not zero, and records this moment T2;It is dense according to sample thickness, hydrogen Degree and time (T2-T1), hydrogen diffusion coefficient is calculated using Fick diffusion second law;
(7) the reading Y of two-way foil gauge at this time is recorded1, loading axis is reduced, until two-way foil gauge reading is-Y1, to set frequency Rate cyclic load axis makes two-way foil gauge reading in Y1~-Y1Between change, cyclic loading is applied to piece sample, until hydrogen Gas concentration detection device reading is increased with 1.5 times of the rate that variation each second is former reading;Sample is recorded during the test Strain and displacement at center;
(8) the fatigue life cycle F undergone before specimen broke is recorded1, experimental enviroment case and associated ping are taken out using vacuum pump true Empty extremely setting vacuum degree, closes vacuum pump;It is replaced several times using argon gas, separates top environment cabinet and lower part environmental cabinet Body takes out sample;
(9) step (2), (3) are repeated, the residual air of experimental enviroment case and air-channel system are taken out with vacuum pump, until vacuum degree Reach setting value;It carries out argon gas to low pressure buffer tank to fill, until argon pressure reaches hydrogen in step (5) in low pressure buffer tank Gas/natural gas gaseous mixture charge pressure;It carries out high pressure argon gas to high-pressure buffering pot using Pneumatic booster pump to fill, until high pressure is slow It rushes in tank after argon pressure reaches setting value;Enter the argon gas in high-pressure buffering pot in experimental enviroment case by valve control, Until air pressure reaches test requirements document;It repeats step (7), the fatigue life cycle that record sample is undergone before rupturing in an argon atmosphere F2;Calculate the ratio (F of fatigue life cycle twice1/F2), which is the fatigue damage index of sample.
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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