CN110455627A - Material and high pressure hydrogen Compatibility Evaluation method and system based on permanent displacement load - Google Patents
Material and high pressure hydrogen Compatibility Evaluation method and system based on permanent displacement load Download PDFInfo
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- CN110455627A CN110455627A CN201910790920.0A CN201910790920A CN110455627A CN 110455627 A CN110455627 A CN 110455627A CN 201910790920 A CN201910790920 A CN 201910790920A CN 110455627 A CN110455627 A CN 110455627A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0001—Type of application of the stress
- G01N2203/0003—Steady
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0073—Fatigue
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Abstract
The embodiment of the invention discloses a kind of materials and high pressure hydrogen Compatibility Evaluation method and system based on permanent displacement load, based on Theory of Fracture Mechanics, compatibility test method for material in static seal isolated environment and high pressure hydrogen, it is carried out using compact tensile specimen (CT sample) and bolt load compact tensile specimen (WOL sample), sample material can be measured by the test method and load critical stress intensity factors value K of the compact tensile specimen in high pressure hydrogen environment in the permanent crackle hydrogen induced cracking (HIC) sensibility being displaced under stress state and boltIHThe material parameter obtained according to the method for the present invention cannot be only used for measuring applicability of the material in high pressure hydrogen environment, the design and manufacture equipped that can also be on active service for hydrogen environment provide necessary design parameter, long-range monitoring can be used in test process, testing crew close contact hydrogen high-pressure test device is avoided, empirical risk is reduced.
Description
Technical field
The present embodiments relate to material mechanical performance tests and characterization technique field, and in particular to based on permanent displacement load
Material and high pressure hydrogen Compatibility Evaluation method and system.
Background technique
Hydrogen has the advantages such as from a wealth of sources, discharge product is pollution-free as following emerging energy.It is directly connect with hydrogen
The hydrogen of touching is produced, storage and transportation, the equipment such as hydrogen is added to be the key equipment of Hydrogen Energy development, and safety is also more and more important, and is used for
After contacting with hydrogen Hydrogen Brittleness Phenomena can occur for metal material, nonmetallic materials in hydrogen warehousing and transportation facilities, in high pressure hydrogen then
It can be more obvious.For this purpose, produced, before storage and transportation plus the design and manufacture of the equipment such as hydrogen carrying out hydrogen, need to carry out material with
Whether the Compatibility Evaluation of hydrogen can be on active service for judgement material in hydrogen gas environment.
The compatibility evaluation test method of existing material and hydrogen has differential experiment, horizontal tension test etc. in environment.Mesh
It is even higher that preceding engineering Hydrogen Vapor Pressure can be divided into 35MPa, 70MPa, 90MPa, 103MPa, since hydrogen has easily leakage, easily
Combustion, explosive characteristic face many technical difficulties when the compatibility evaluation for carrying out material and hydrogen is tested, in real-time loading
Be slidingly sealed difficulty, closely operate dangerous property etc..
Summary of the invention
For this purpose, the embodiment of the present invention provides a kind of material and high pressure hydrogen Compatibility Evaluation side for being displaced load based on perseverance
Method, with the Compatibility Evaluation test that the solves existing material and hydrogen technical difficulties such as that there are dynamic sealings is difficult, test risk is big
The problem of.
To achieve the goals above, the embodiment of the present invention provides the following technical solutions:
According to a first aspect of the embodiments of the present invention, a kind of material based on permanent displacement load is commented with high pressure hydrogen compatibility
Valence method, which comprises
Compact tensile specimen is prepared using material to be tested and bolt loads compact tensile specimen；
Fatigue crack prefabrication is carried out respectively to the compact tensile specimen and bolt load compact tensile specimen；
Loaded load is distinguished to the compact tensile specimen and bolt the load compact tensile specimen of prefabricating fatigue crack；
By the compact tensile specimen and bolt the load compact tensile specimen of loaded load respectively in static seal High Pressure Hydrogen
A period of time is placed in compression ring border to be tested；
The compact tensile specimen and bolt load compact tensile specimen are unloaded after the completion of test；
To after unloading the compact tensile specimen and bolt load compact tensile specimen carry out it is cold short break, measure respectively
And calculate the section crack propagation Δ l of sample before and after the test；
Compact tensile specimen is loaded to the compact tensile specimen, bolt respectively according to the section crack propagation Δ l
It is evaluated with the compatibility of high pressure hydrogen, and calculates critical under hydrogen gas environment of bolt load compact tensile specimen and answer
Power intensity factor value KIH。
Further, described that the compact tensile specimen, bolt are loaded tightly respectively according to the section crack propagation
The compatibility of tensile sample and high pressure hydrogen of gathering is evaluated, and calculates bolt load compact tensile specimen in hydrogen gas environment
Under critical stress intensity factors value KIH, comprising:
For the compact tensile specimen,
If 0≤Δ l≤0.25mm, and meet plane strain and assume criterionThe then examination
Sample material is suitable for the hydrogen environment under test pressure；
If 0≤Δ l≤0.25mm, but be unsatisfactory for plane strain and assume criterionFull
Under the conditions of the not quick-fried first leakage design criteria of foot, then thickness when test can be selected in the sample material is suitable for the hydrogen under test pressure
Environment；
If Δ l > 0.25mm, the sample material are not suitable for the hydrogen environment under the test pressure；
Wherein, Δ l=le-l0, l0For the initial section crack length before specimen test, leFor the termination after specimen test
Section crack length, KI0For the stress intensity factor value for testing preceding sample loaded load, KIeLoad is unloaded for sample after test
Stress intensity factor value, Rp0.2For the yield strength of sample material, B is the thickness of sample, and W is the width of sample.
Further, described that the compact tensile specimen, bolt are loaded tightly respectively according to the section crack propagation
The compatibility of tensile sample and high pressure hydrogen of gathering is evaluated, and calculates bolt load compact tensile specimen in hydrogen gas environment
Under critical stress intensity factors value KIH, comprising:
Compact tensile specimen is loaded for the bolt,
If 0≤Δ l≤0.25mm, and meet plane strain and assume criterionThe then examination
Sample material is suitable for the hydrogen environment under test pressure, KIH=0.5KI0；
If 0≤Δ l≤0.25mm, but be unsatisfactory for plane strain and assume criterionFull
Under the conditions of the not quick-fried first leakage design criteria of foot, then the sample material is suitable for the hydrogen environment under test pressure in the case where testing thickness,
KIH=0.5KI0；
If Δ l > 0.25mm, the sample material are not suitable for the hydrogen environment under the test pressure, KIH=KIe；
Wherein, Δ l=le-l0, l0For the initial section crack length before specimen test, leFor the termination after specimen test
Section crack length, KI0For the stress intensity factor value for testing preceding sample loaded load, KIeLoad is unloaded for sample after test
Stress intensity factor value, Rp0.2For the yield strength of sample material, B is the thickness of sample, and W is the width of sample.
Further, the method also includes:
It is scarce that the bolt load compact tensile specimen carries out load F- before loaded load and after unloading load
The calibration of mouth opening displacement V curve；
According to the load F- notch demarcated before the practical notch opening displacement of sample when loaded load and loaded load
Open position move V curve obtain loaded load, and according to unloading load when sample practical notch opening displacement and unloading load it
The load F- notch opening displacement V curve demarcated afterwards obtains unloading load；
It calculates separately to obtain stress intensity factor value K according to the loaded load and unloading loadI0And stress intensity factor
Value KIe。
Further, the compact tensile specimen and bolt the load compact tensile specimen point to prefabricating fatigue crack
Other loaded load, comprising:
The compact tensile specimen is loaded using wedge block, and the bolt load compact tensile specimen is loaded using bolt.
Further, the compact tensile specimen after described pair of unloading and bolt load compact tensile specimen carry out low temperature
It breaks, before measuring respectively and calculating the section crack propagation Δ l of sample before and after the test, further includes:
The compact tensile specimen and bolt load compact tensile specimen are carried out respectively at coloring treatment or secondary fatigue
Reason.
Further, the compact tensile specimen and bolt the load compact tensile specimen point to prefabricating fatigue crack
Other loaded load, comprising:
It is loaded according to recommending loaded value to load compact tensile specimen to the bolt；
As the yield strength R of bolt load compact tensile specimenp0.2When close to 621MPa, recommend loaded value KIIt is 159
~198；
As the yield strength R of bolt load compact tensile specimenp0.2When close to 759MPa, recommend loaded value KIIt is 93
~159；
As the yield strength R of bolt load compact tensile specimenp0.2When close to 897MPa, recommend loaded value KIIt is 71
~115.
According to a second aspect of the embodiments of the present invention, a kind of material and High Pressure Hydrogen gas phase based on permanent displacement load is proposed
Capacitive test macro, the system comprises:
Sample preparation module, for being tried using material to be tested preparation compact tensile specimen and bolt load compact tension specimen
Sample；
Crackle Prefabricated block, for carrying out fatigue respectively to the compact tensile specimen and bolt load compact tensile specimen
Crackle is prefabricated；
Loading module, for the compact tensile specimen and bolt the load compact tensile specimen point to prefabricating fatigue crack
Other loaded load；
Tentative module, for the compact tensile specimen and bolt the load compact tensile specimen of loaded load to exist respectively
A period of time is placed in static seal hydrogen gas environment to be tested；
Unload module, for being carried out after the completion of test to the compact tensile specimen and bolt load compact tensile specimen
Unloading；
Section survey module, for the compact tensile specimen and bolt load compact tensile specimen progress after unloading
It is cold short to break, it measures respectively and calculates the section crack propagation Δ l of sample before and after the test；
Compatibility Evaluation module is used for according to the section crack propagation Δ l respectively to the compact tensile specimen, spiral shell
Bolt load compact tensile specimen and the compatibility of high pressure hydrogen are evaluated, and calculate bolt load compact tensile specimen in high pressure
Critical stress intensity factors value K under hydrogen environmentIH。
Further, the tentative module includes the high pressure storage for static seal hydrogen gas environment needed for providing test
Hydrogen kettle, the exhaust outlet for hydrogen to be discharged after the completion of testing is provided on the high-pressure hydrogen storing kettle, and the high-pressure hydrogen storing kettle connects
It is connected to the supercharging equipment for hydrogen pressurization, is provided with and is used in the compact tensile specimen and bolt load compact tensile specimen
The detection device of sample deformation information is inspected, the detection device and high-pressure hydrogen storing kettle are all connected with data collection system, the height
Pressure hydrogen storage kettle is connected with tele-control system, monitoring system and alarm system.
Further, the detection device includes foil gauge, extensometer or LVDT displacement sensor.
The embodiment of the present invention has the advantages that
A kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load that the embodiment of the present invention proposes and
System is based on Theory of Fracture Mechanics, for the compatibility test method of material in static seal isolated environment and high pressure hydrogen, uses
Compact tensile specimen (CT sample) and bolt load compact tensile specimen (WOL sample) carry out, and can be weighed by the test method
Sample material is measured in the permanent crackle hydrogen induced cracking (HIC) sensibility being displaced under stress state and bolt load compact tensile specimen in height
Critical stress intensity factors value K in pressure hydrogen environmentIH, the material parameter obtained according to the method for the present invention cannot be only used for measure material
Expect the applicability in high pressure hydrogen environment, the design and manufacture for the equipment that can also be on active service for hydrogen environment provide necessary design parameter,
Static seal is better than dynamic sealing design, and being carried out the Compatibility Evaluation of material and hydrogen under loading environment in the form of static seal is ensured
The stability of test process, reduces the risk of hydrogen gas leakage, long-range monitoring can be used in test process, avoids testing crew close
Distance contact hydrogen high-pressure test device, reduces empirical risk.
Detailed description of the invention
It, below will be to embodiment party in order to illustrate more clearly of embodiments of the present invention or technical solution in the prior art
Formula or attached drawing needed to be used in the description of the prior art are briefly described.It should be evident that the accompanying drawings in the following description is only
It is merely exemplary, it for those of ordinary skill in the art, without creative efforts, can also basis
The attached drawing of offer, which is extended, obtains other implementation attached drawings.
Fig. 1 is a kind of material and high pressure hydrogen Compatibility Evaluation based on permanent displacement load that the embodiment of the present invention 1 provides
The flow diagram of method；
Fig. 2 is a kind of material and high pressure hydrogen Compatibility Evaluation based on permanent displacement load that the embodiment of the present invention 1 provides
The structural schematic diagram of method CT sample；
Fig. 3 is a kind of material and high pressure hydrogen Compatibility Evaluation based on permanent displacement load that the embodiment of the present invention 1 provides
The structural schematic diagram of method WOL sample；
Fig. 4 is a kind of material and high pressure hydrogen Compatibility Evaluation based on permanent displacement load that the embodiment of the present invention 2 provides
The structural schematic diagram of system；
Fig. 5 is a kind of material and high pressure hydrogen Compatibility Evaluation based on permanent displacement load that the embodiment of the present invention 2 provides
The structural schematic diagram of STS system test set.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily, it is clear that described embodiment is the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
As shown in Figure 1, the present embodiment proposes a kind of material and high pressure hydrogen Compatibility Evaluation based on permanent displacement load
Method, method includes the following steps:
Step S110, compact tensile specimen is prepared using material to be tested and bolt loads compact tensile specimen.
Sample preparation and dimensional measurement:
Test is tried using compact tensile specimen (referred to as: CT sample, as shown in Figure 2) and the load compact tension specimen of modified bolt
Sample (referred to as: WOL sample, as shown in Figure 3) carry out, wherein WOL sample is alternatively referred to as bolt loaded type CT sample, with CT sample
Difference be that CT sample is loaded in load using wedge block, and WOL sample is loaded using bolt, first right before test
Specimen surface carries out oil removing, processing of rust removing.The thickness B of sample be it needs to be determined that key parameter, selected sample thickness answers
Design thickness not less than 85% should be commonly used when sampling is not able to satisfy 85% design thickness requirement using maximum sampling thickness
There are 25mm, 20mm, 15mm, 12.5mm, 10mm, 7.5mm, 5mm etc. in the thickness of test.It can be true according to sample thickness B
The width and thickness of width W, the CT sample of sample is determined than recommending are as follows: the width-thickness ratio of 1≤W/B≤2, WOL sample is recommended are as follows: W/B=
2:1 also may be selected 1:1 and carry out.CT sample, WOL sample geomery refer to ASTM E1681-03 (reapproved
2008)ε2《Determine threshold stress intensity factor for environment-assisted
Cracking of metallic materials " in require.
The measurement of specimen size should be accurate to ± 0.02mm or ± 0.2%, accurate thickness B, the width W, machine for measuring sample
Tool notch length a, the other sizes information of sample such as height, physical notches height information should also be recorded.
Step S120, fatigue crack prefabrication is carried out respectively to compact tensile specimen and bolt load compact tensile specimen.
(1) before carrying out fatigue crack prefabrication, the tensile strength R of material should be obtainedm, yield strength Rp0.2, elastic modulus E ginseng
Number.
(2) crackle initial length, general control a are determined0/ W wants the prefabricated crack length to be between 0.45~0.55
(a0- a), wherein required prefabricated minimum fatigue crack should be greater than 1.3mm or 2.5%W (taking wherein the greater).Example: CT sample B
It is 19mm for 25mm, W 50mm, machining notch length a；If controlling a0/ W is 0.45~0.55, then a0Length should be 22.5~
27.5mm subtracts machining notch length 19mm, then precrack length should be 3.5~8.5mm.
(3) fatigue crack prefabrication should be carried out using the method for load shedding lotus, prefabricated in the last 1.3mm of crackle or 50% crackle
When amount, maximum fatigue precracking power should take formula (1), the low value in (2).
In formula: FtFor the load that should apply in fatigue tester, W is the width of sample, and B is the thickness of sample, a0It is pre-
The length of crackle processed, Rp0.2For yield strength, E is elasticity modulus.Calculating can be calculated by formula (3).
(4) it can be marked on sample, the position of the quasi- extension of label precrack facilitates in crackle prefabrication process
It is observed.Then clamping CT sample or WOL sample, it is noted that concentricity is consistent in clamping process, concentricity can shadow
Ring the propagation direction of crackle and the symmetry of precrack in sample.
(5) the prefabricated of fatigue crack carries out on HF fatigue testing machine, stress ratio 0.1, prefabricating fatigue crack process
Middle maximum fatigue crack prefabrication power should be accurately to ± 2.5%.It sets precrack load and carries out fatigue crack prefabrication.
Step S130, load is loaded respectively to the compact tensile specimen of prefabricating fatigue crack and bolt load compact tensile specimen
Lotus.
Compact tensile specimen is loaded using wedge block, and bolt is loaded compact tensile specimen and loaded using bolt.
Further, this method further include:
Bolt loads compact tensile specimen and carries out load F- notch before loaded load and after unloading load
The calibration of open position shifting V curve；
According to the load F- notch demarcated before the practical notch opening displacement of sample when loaded load and loaded load
Open position move V curve obtain loaded load, and according to unloading load when sample practical notch opening displacement and unloading load it
The load F- notch opening displacement V curve demarcated afterwards obtains unloading load；
It calculates separately to obtain stress intensity factor value K according to loaded load and unloading loadI0With stress intensity factor value
KIe。
One, the load of CT sample
(1) CT sample is loaded using wedge block.
(2) the minimum stress-intensity factor value loaded needed for the load of CT sample will calculate, according to the tensile strength of sample
Rm, it is calculated using following formula:
In formula: KIAPPRefer to institute's stress intensity factor to be loaded, V is the aperture displacement reached needed for sample, and W is sample
Width, B be sample thickness, a0For the length of precrack, E is elasticity modulus.
(3) the CT sample not loaded is carried out opening mouth dimensional measurement, then by CT specimen clamping on universal testing machine,
CT sample is loaded using wedge block, the aperture displacement of control CT sample is greater than the sample that formula (5) are calculated
Aperture displacement completes load.
(4) measurement for opening opening size can carry out on stereomicroscope, and record the notch that load is completed and open position
Move V.
(5) CT sample load example is shown in Table 1.
Minimum aperture displacement needed for the load of table 1CT sample
Two, the load of WOL sample
(1) WOL sample is loaded using bolt, the stress intensity factor value K of WOL sampleIIt calculates and utilizes following formula:
In formula: W is the width of sample, and B is the thickness of sample, and a is crack length, FVFor loaded load.
(2) as the yield strength R of experimental materialp0.2With when yield strength is close in following table, the load of WOL sample KI can be joined
Recommendation in table 2 is loaded, or is loaded according to material property.
The different yield strength R of table 2p0.2Corresponding recommendation loaded value KI
| Yield strength Rp0.2 | Recommend the K of loadI |
| 621MPa | 159~198 |
| 759MPa | 93~159 |
| 897MPa | 71~115 |
(3) WOL sample needs progress load F- notch opening displacement V curve to be demarcated before load, utilizes universal test
Machine stretches WOL sample, installs extensometer in aperture position, records the F-V curve in drawing process.
(4) being determined according to the recommendation in table 1 needs K to be loadedIValue, and be calculated using formula (7) and need to load
Load FV, and the notch opening displacement V loaded needed for being obtained according to the F-V curve of acquisition.
(5) WOL sample is loaded using bolt, the notch opening displacement of sample is recorded when load, until reaching plus
What is carried opens aperture displacement and is recorded as V0。
(6) according to the aperture displacement V of actual loaded0, correspond to the real load F that F-V curve is loadedV0And it records.
Step S140, by the compact tensile specimen of loaded load and bolt load compact tensile specimen respectively in static seal height
A period of time is placed in pressure hydrogen environment to be tested.
Using high-pressure hydrogen storing kettle provide test needed for static seal hydrogen gas environment, test before first to high-pressure hydrogen storing kettle into
Horizontal high voltage is flushed with hydrogen, and specific processing step is as follows:
(1) high-pressure hydrogen storing kettle is cleaned out, it is ensured that the impurity such as free from dust, oil-free.
(2) sample of loaded is fixed in sample frame, is put into high-pressure hydrogen storing kettle, then carry out fit sealing.
(3) cleaning displacement is carried out to high-pressure hydrogen storing kettle using high pure nitrogen (99.999%) after fastening, is after nitrogen displacement
Oxygen content of uniting is no more than 3%.High-pressure hydrogen storing kettle is vacuumized, vacuum degree is not more than 3Pa.
(4) hydrogen pressurization is carried out to high-pressure hydrogen storing kettle, hydrogen purity is after pressure stabilisation to start to try not less than 99.999%
Test timing.If requiring test temperature, high-pressure hydrogen storing kettle should be carried out after reaching test temperature being pressurized to test pressure.
(5) to ferritic steel, the test period of High pressure filling hydrogen is at least 1000h；The time of stainless steel High pressure filling hydrogen recommends
For 5000h.
Step S150, compact tensile specimen and bolt load compact tensile specimen are unloaded after the completion of test.
The CT sample finished will be flushed with hydrogen, WOL specimen clamping unloads on universal testing machine, wherein WOL sample is unloading
The variation of its notch opening displacement should be recorded when load and is recorded as Ve, after completion of discharge should again the F-V curve to WOL sample into
Rower is fixed, and utilizes VeThe load F born when the unloading of WOL sample is calculatedVe。
Step S160, to after unloading compact tensile specimen and bolt load compact tensile specimen carry out it is cold short break, point
It does not measure and calculates the section crack propagation Δ l of sample before and after the test.
Further, before step step S160 further include: load compact tensile specimen to compact tensile specimen and bolt
Coloring treatment or secondary fatigue processing are carried out respectively.
The measurement of sample section crackle: the CT sample of completion of discharge, WOL sample are subjected to coloring or secondary fatigue is handled, mesh
Be to discriminate between crackle caused by hydrogen induced cracking (HIC).Coloring can be heated to 300 DEG C of heat preservation 1h to sample by high temperature furnace and realize, secondary
Fatigue, which refers to, carries out 3~5min of fatigue crack prefabrication to sample on fatigue tester, and test load should be significantly greater or less than
Load when initial crack is prefabricated.Sample is broken followed by low temperature, its section crack is measured.
Prefabricated fatigue crack region has clearly boundary, can be easily discriminated prefabricating fatigue crack area and hydrogen induced cracking
The difference in area, but topographical difference is smaller between cracked zone caused by hydrogen induced cracking area and artificial low-temperature brittle fracture, it is difficult to it distinguishes, leads to
It crosses before brittle failure and carries out coloring treatment or secondary fatigue processing, hydrogen induced cracking area being marked clearly can be made into hydrogen
Cause cracked zone and it is artificial caused by generate apparent boundary between cracked zone, to distinguish hydrogen induced cracking area, calculate hydrogen cause it is disconnected
Face crack extension.
The measurement of section crack should utilize tool microscope or digit microscope, be carried out using 9 methods, and survey calculation obtains
Initial section crack length a before to specimen test0And the termination section crack length a after teste。
Step S170, compact tensile specimen is loaded to compact tensile specimen, bolt respectively according to section crack propagation Δ l
It is evaluated with the compatibility of high pressure hydrogen, and calculates critical under hydrogen gas environment of bolt load compact tensile specimen and answer
Power intensity factor value KIH。
For the Compatibility Evaluation rule of compact tensile specimen:
(1) if 0≤Δ l≤0.25mm, and meet plane strain assume criterionThen
The sample material is suitable for the hydrogen environment under test pressure；
(2) if 0≤Δ l≤0.25mm, but be unsatisfactory for plane strain assume criterion
Under the conditions of meeting not quick-fried first leakage design criteria, then thickness when test can be selected in the sample material is suitable under test pressure
Hydrogen environment；
(3) if Δ l > 0.25mm, the sample material are not suitable for the hydrogen environment under the test pressure；
Wherein, Δ l=le-l0, l0For the initial section crack length before specimen test, leFor the termination after specimen test
Section crack length, KI0For the stress intensity factor value for testing preceding sample loaded load, KIeLoad is unloaded for sample after test
Stress intensity factor value, Rp0.2For the yield strength of sample material, B is the thickness of sample, and W is the width of sample.
Compact tensile specimen is loaded for bolt, according to following Compatibility Evaluation rule and is calculated:
(1) if 0≤Δ l≤0.25mm, and meet plane strain assume criterionThen
The sample material is suitable for the hydrogen environment under test pressure, KIH=0.5KI0；
(2) if 0≤Δ l≤0.25mm, but be unsatisfactory for plane strain assume criterion
Under the conditions of meeting not quick-fried first leakage design criteria, then the sample material is suitable for the hydrogen ring under test pressure in the case where testing thickness
Border, KIH=0.5KI0；
(3) if Δ l > 0.25mm, the sample material are not suitable for the hydrogen environment under the test pressure, KIH=KIe；
Wherein, Δ l=le-l0, l0For the initial section crack length before specimen test, leFor the termination after specimen test
Section crack length, KI0For the stress intensity factor value for testing preceding sample loaded load, KIeLoad is unloaded for sample after test
Stress intensity factor value, Rp0.2For the yield strength of sample material, B is the thickness of sample, and W is the width of sample.
A kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load that the present embodiment proposes, based on disconnected
Theory of mechanics is split, for the compatibility test method of material in static seal isolated environment and high pressure hydrogen, is tried using compact tension specimen
Sample (CT sample) and bolt load compact tensile specimen (WOL sample) carry out, and can measure sample material by the test method
In the permanent crackle hydrogen induced cracking (HIC) sensibility being displaced under stress state and bolt load compact tensile specimen in high pressure hydrogen environment
Critical stress intensity factors value KIH, the material parameter obtained according to the method for the present invention cannot be only used for measure material in High Pressure Hydrogen
The design and manufacture of applicability in environment, the equipment that can also be on active service for hydrogen environment provide necessary design parameter, and static seal wants excellent
It is designed in dynamic sealing, carries out the Compatibility Evaluation of material and hydrogen under loading environment in the form of static seal and ensure test process
Stability, reduce the risk of hydrogen gas leakage.
Embodiment 2
It is corresponding with above-described embodiment 1, as shown in figure 4, the present embodiment proposes a kind of material based on permanent displacement load
Material and high pressure hydrogen compatibility test system, the system include:
Sample preparation module 210, for loading compact tension specimen using material to be tested preparation compact tensile specimen and bolt
Sample.
Crackle Prefabricated block 220, for carrying out fatigue respectively to compact tensile specimen and bolt load compact tensile specimen
Crackle is prefabricated.
Loading module 230, for the compact tensile specimen and bolt load compact tensile specimen point to prefabricating fatigue crack
Other loaded load.
Tentative module 240, for the compact tensile specimen of loaded load and bolt load compact tensile specimen to exist respectively
A period of time is placed in static seal hydrogen gas environment to be tested.
As shown in figure 5, the experimental rig that tentative module 240 is related to includes for static seal High Pressure Hydrogen needed for providing test
The high-pressure hydrogen storing kettle 241 in compression ring border is provided with heating device 2411 outside high-pressure hydrogen storing kettle 241, is arranged on high-pressure hydrogen storing kettle 241
There is the exhaust outlet 242 for hydrogen to be discharged after the completion of testing, high-pressure hydrogen storing kettle 241 is connected by nitrogen or hydrogen pipeline 2431
There is the supercharging equipment 243 for hydrogen pressurization, is provided in compact tensile specimen and bolt load compact tensile specimen for examining
The detection device of sample deformation information, detection device and high-pressure hydrogen storing kettle 241 connect data acquisition system by data cable
System 244, high-pressure hydrogen storing kettle 241 are connected with tele-control system 245, monitoring system and alarm system, and monitoring system includes prison
Camera 246 is controlled, alarm system includes hydrogen alarm 247.
Further, detection device includes foil gauge, extensometer or LVDT displacement sensor.It can be using in sample crackle
Tip nearby pastes foil gauge 248, sample aperture position and installs the modes such as extensometer 249 or LVDT displacement sensor, will try
Deformation information during testing is converted to electric signal transmission to data collection system, record the deformation information on test material surface with
Monitoring test progress.
Specific test process is as follows:
(1) high-pressure hydrogen storing kettle 241 is cleaned, it is ensured that put the sample of loaded to high pressure without dust, oil stain, water inside
Hydrogen storage kettle 241 sample frame can be used when necessary, sample is fixed；It, should be by number if being equipped with foil gauge, extensometer or LVDT
It is connected at data-interface according to line；
(2) 241 tele-control system of high-pressure hydrogen storing kettle, data collection system, monitoring system and alarm system are opened, it is ensured that
System is working properly；
(3) fastening high hydrogen storage kettle 241, it is ensured that sealing element is correctly installed, and carries out high pure nitrogen purging using pressure charging system,
3 purgings are at least carried out, the nitrogen pressure of purging is greater than 2MPa.
(4) it is vacuumized after purging, then carries out hydrogen pressurization, if test temperature is higher than room temperature, should be reached
Hydrogen pressurization is carried out after test temperature again, until reaching test pressure.
(5) system starts timing after stablizing, and is detected using long-range control, monitoring, alarm system to equipment state, number
Test temperature, pressure, deformation information are acquired and are recorded according to acquisition system.
(6) pressure release is carried out after testing, hydrogen is discharged by exhaust outlet 242 (flame-retardant device), followed by high pure nitrogen
It is purged, it is ensured that hydrogen-free gas medium in autoclave opens high-pressure hydrogen storing kettle 241, completes test.
Unload module 250, for being carried out after the completion of test to compact tensile specimen and bolt load compact tensile specimen
Unloading.
Section survey module 260, for the compact tensile specimen and bolt load compact tensile specimen progress after unloading
It is cold short to break, it measures respectively and calculates the section crack propagation Δ l of sample before and after the test.
Compatibility Evaluation module 270, for being added respectively to compact tensile specimen, bolt according to section crack propagation Δ l
The compatibility for carrying compact tensile specimen and high pressure hydrogen is evaluated, and calculates bolt load compact tensile specimen in high pressure hydrogen
Critical stress intensity factors value K under environmentIH。
In a kind of material and high pressure hydrogen Compatibility Evaluation system based on permanent displacement load provided in an embodiment of the present invention
Function performed by each component has been discussed in detail in above-described embodiment 1, therefore does not do excessively repeat here.
A kind of material and high pressure hydrogen Compatibility Evaluation system based on permanent displacement load that the embodiment of the present invention proposes, base
In Theory of Fracture Mechanics, for the compatibility test method of material in static seal isolated environment and high pressure hydrogen, using compact drawing
It stretches sample (CT sample) and bolt load compact tensile specimen (WOL sample) carries out, sample can be measured by the test method
Material is in the permanent crackle hydrogen induced cracking (HIC) sensibility being displaced under stress state and bolt load compact tensile specimen in High Pressure Hydrogen ring
Critical stress intensity factors value K in borderIH, the material parameter obtained according to the present invention cannot be only used for measure material in High Pressure Hydrogen
The design and manufacture of applicability in environment, the equipment that can also be on active service for hydrogen environment provide necessary design parameter, high-pressure hydrogen storing kettle
Static seal be better than dynamic sealing design, in the form of static seal carry out loading environment under the Compatibility Evaluation of material and hydrogen it is true
The stability for having protected test process, reduces the risk of hydrogen gas leakage, test process can be used long-range monitoring, avoid testing crew
Close contact hydrogen high-pressure test device, reduces empirical risk.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (10)
1. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load, which is characterized in that the method packet
It includes:
Compact tensile specimen is prepared using material to be tested and bolt loads compact tensile specimen；
Fatigue crack prefabrication is carried out respectively to the compact tensile specimen and bolt load compact tensile specimen；
Loaded load is distinguished to the compact tensile specimen and bolt the load compact tensile specimen of prefabricating fatigue crack；
By the compact tensile specimen and bolt the load compact tensile specimen of loaded load respectively in static seal High Pressure Hydrogen compression ring
A period of time is placed in border to be tested；
The compact tensile specimen and bolt load compact tensile specimen are unloaded after the completion of test；
To after unloading the compact tensile specimen and bolt load compact tensile specimen carry out it is cold short break, measure and count respectively
Calculate the section crack propagation Δ l of sample before and after the test；
According to the section crack propagation Δ l respectively to the compact tensile specimen, bolt load compact tensile specimen and height
The compatibility of pressure hydrogen is evaluated, and it is strong to calculate limit stress of the bolt load compact tensile specimen under hydrogen gas environment
Spend factor values KIH。
2. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load according to claim 1,
It is characterized in that, it is described that the compact tensile specimen, bolt load compact tension specimen are tried respectively according to the section crack propagation
The compatibility of sample and high pressure hydrogen is evaluated, and it is critical under hydrogen gas environment to calculate bolt load compact tensile specimen
Stress intensity factor value KIH, comprising:
For the compact tensile specimen,
If 0≤Δ l≤0.25mm, and meet plane strain and assume criterionThe then sample material
Material is suitable for the hydrogen environment under test pressure；
If 0≤Δ l≤0.25mm, but be unsatisfactory for plane strain and assume criterionMeeting not
Under the conditions of quick-fried first leakage design criteria, then thickness when test can be selected in the sample material is suitable for the hydrogen ring under test pressure
Border；
If Δ l > 0.25mm, the sample material are not suitable for the hydrogen environment under the test pressure；
Wherein, Δ l=le-l0, l0For the initial section crack length before specimen test, leIt is split for the termination section after specimen test
Line length, KI0For the stress intensity factor value for testing preceding sample loaded load, KIeThe stress for unloading load for sample after test is strong
Spend factor values, Rp0.2For the yield strength of sample material, B is the thickness of sample, and W is the width of sample.
3. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load according to claim 1,
It is characterized in that, it is described that the compact tensile specimen, bolt load compact tension specimen are tried respectively according to the section crack propagation
The compatibility of sample and high pressure hydrogen is evaluated, and it is critical under hydrogen gas environment to calculate bolt load compact tensile specimen
Stress intensity factor value KIH, comprising:
Compact tensile specimen is loaded for the bolt,
If 0≤Δ l≤0.25mm, and meet plane strain and assume criterionThe then sample material
Material is suitable for the hydrogen environment under test pressure, KIH=0.5KI0；
If 0≤Δ l≤0.25mm, but be unsatisfactory for plane strain and assume criterionMeeting not
Under the conditions of quick-fried first leakage design criteria, then the sample material is suitable for the hydrogen environment under test pressure, K in the case where testing thicknessIH=
0.5KI0；
If Δ l > 0.25mm, the sample material are not suitable for the hydrogen environment under the test pressure, KIH=KIe；
Wherein, Δ l=le-l0, l0For the initial section crack length before specimen test, leIt is split for the termination section after specimen test
Line length, KI0For the stress intensity factor value for testing preceding sample loaded load, KIeThe stress for unloading load for sample after test is strong
Spend factor values, Rp0.2For the yield strength of sample material, B is the thickness of sample, and W is the width of sample.
4. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load according to claim 1,
It is characterized in that, the method also includes:
The bolt load compact tensile specimen carries out load F- notch before loaded load and after unloading load
The calibration of open position shifting V curve；
Position is opened according to the load F- notch demarcated before the practical notch opening displacement of sample when loaded load and loaded load
V curve acquisition loaded load is moved, and according to mark after the practical notch opening displacement and unloading load of sample when unloading load
Fixed load F- notch opening displacement V curve obtains unloading load；
It calculates separately to obtain stress intensity factor value K according to the loaded load and unloading loadI0With stress intensity factor value KIe。
5. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load according to claim 1,
It is characterized in that, the compact tensile specimen and bolt the load compact tensile specimen to prefabricating fatigue crack loads load respectively
Lotus, comprising:
The compact tensile specimen is loaded using wedge block, and the bolt load compact tensile specimen is loaded using bolt.
6. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load according to claim 1,
It being characterized in that, the compact tensile specimen and bolt load compact tensile specimen after described pair of unloading carry out low temperature and break, point
Before not measuring and calculating the section crack propagation Δ l of sample before and after the test, further includes:
Coloring treatment or secondary fatigue processing are carried out respectively to the compact tensile specimen and bolt load compact tensile specimen.
7. a kind of material and high pressure hydrogen Compatibility Evaluation method based on permanent displacement load according to claim 1,
It is characterized in that, the compact tensile specimen and bolt the load compact tensile specimen to prefabricating fatigue crack loads load respectively
Lotus, comprising:
It is loaded according to recommending loaded value to load compact tensile specimen to the bolt；
As the yield strength R of bolt load compact tensile specimenp0.2When close to 621MPa, recommend loaded value KIFor 159~
198；
As the yield strength R of bolt load compact tensile specimenp0.2When close to 759MPa, recommend loaded value KIFor 93~
159；
As the yield strength R of bolt load compact tensile specimenp0.2When close to 897MPa, recommend loaded value KIFor 71~
115。
8. a kind of material and high pressure hydrogen compatibility test system based on permanent displacement load, which is characterized in that the system packet
It includes:
Sample preparation module, for loading compact tensile specimen using material to be tested preparation compact tensile specimen and bolt；
Crackle Prefabricated block, for carrying out fatigue crack respectively to the compact tensile specimen and bolt load compact tensile specimen
It is prefabricated；
Loading module adds respectively for the compact tensile specimen and bolt the load compact tensile specimen to prefabricating fatigue crack
Carry load；
Tentative module, for the compact tensile specimen and bolt of loaded load to be loaded compact tensile specimen respectively quiet close
A period of time is placed in envelope hydrogen gas environment to be tested；
Unload module, for being unloaded after the completion of test to the compact tensile specimen and bolt load compact tensile specimen
It carries；
Section survey module, for after unloading the compact tensile specimen and bolt load compact tensile specimen carry out it is cold short
It breaks, measure respectively and calculates the section crack propagation Δ l of sample before and after the test；
Compatibility Evaluation module, for being added respectively to the compact tensile specimen, bolt according to the section crack propagation Δ l
The compatibility for carrying compact tensile specimen and high pressure hydrogen is evaluated, and calculates bolt load compact tensile specimen in high pressure hydrogen
Critical stress intensity factors value K under environmentIH。
9. a kind of material and high pressure hydrogen compatibility test system based on permanent displacement load according to claim 8,
It is characterized in that, the tentative module includes the high-pressure hydrogen storing kettle for static seal hydrogen gas environment needed for providing test, institute
The exhaust outlet being provided on high-pressure hydrogen storing kettle for hydrogen to be discharged after the completion of testing is stated, the high-pressure hydrogen storing kettle, which is connected with, to be used for
It is provided in the supercharging equipment of hydrogen pressurization, the compact tensile specimen and bolt load compact tensile specimen and becomes for inspecting sample
The detection device of shape information, the detection device and high-pressure hydrogen storing kettle are all connected with data collection system, the high-pressure hydrogen storing kettle
It is connected with tele-control system, monitoring system and alarm system.
10. a kind of material and high pressure hydrogen compatibility test system based on permanent displacement load according to claim 9,
It is characterized in that, the detection device includes foil gauge, extensometer or LVDT displacement sensor.
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