CN115032063A - Device and method for testing hydrogen embrittlement sensitivity of material for simulating stress state of gas cylinder - Google Patents
Device and method for testing hydrogen embrittlement sensitivity of material for simulating stress state of gas cylinder Download PDFInfo
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- CN115032063A CN115032063A CN202210165488.8A CN202210165488A CN115032063A CN 115032063 A CN115032063 A CN 115032063A CN 202210165488 A CN202210165488 A CN 202210165488A CN 115032063 A CN115032063 A CN 115032063A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 59
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 59
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000012360 testing method Methods 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000007789 gas Substances 0.000 title claims abstract description 23
- 230000035945 sensitivity Effects 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 15
- 239000010439 graphite Substances 0.000 claims abstract description 15
- 238000007600 charging Methods 0.000 claims abstract description 12
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 6
- 238000013461 design Methods 0.000 claims abstract description 4
- 238000005498 polishing Methods 0.000 claims abstract description 4
- 238000004088 simulation Methods 0.000 claims abstract description 4
- 238000004364 calculation method Methods 0.000 claims abstract description 3
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 231100000572 poisoning Toxicity 0.000 claims description 5
- 230000000607 poisoning effect Effects 0.000 claims description 5
- 230000000977 initiatory effect Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 238000010998 test method Methods 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000012611 container material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010325 electrochemical charging Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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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
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
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Abstract
The invention discloses a material hydrogen embrittlement sensitivity test device for simulating a stress state of a gas cylinder, which comprises a medium tank, a potentiostat, a sample, a test machine, a graphite rod or a lead plate, wherein the sample, the test machine and the graphite rod or the lead plate are arranged in the medium tank; the test method comprises the steps of firstly, determining the maximum stress borne by the gas cylinder material by adopting a calculation or simulation mode according to the design parameters of the gas cylinder; secondly, polishing the sample smoothly, and mounting the sample on a testing machine after ultrasonic cleaning; thirdly, connecting a cathode connecting lead with the sample, and inserting a graphite rod or a lead plate serving as an anode into the medium tank; fourthly, loading the sample by using a testing machine until the maximum stress is reached; adding an electrolytic hydrogen charging solution into the medium groove, and regulating a constant potential rectifier to electrochemically charge the sample; fifthly, unloading the tensile stress after maintaining for a certain time, taking out the sample and observing the surface crack condition of the sample; and sixthly, breaking the test sample on a testing machine to observe whether cracks are initiated and expanded on the fracture.
Description
Technical Field
The invention relates to the technical field of metal material tests, in particular to a device and a method for testing hydrogen brittleness sensitivity of a material for simulating a stress state of a gas cylinder.
Background
Hydrogen embrittlement is the phenomenon that hydrogen enters the metal material to polymerize into hydrogen molecules, and strong internal pressure is generated to cause the initiation and development of microcracks, so that the plasticity of the metal material is obviously reduced, the brittleness is rapidly increased, and the metal material is often damaged after being applied for a period of time under static load lower than the tensile strength of the material.
With the challenge of fossil fuel energy exhaustion and the continuous acceleration of clean energy development, the hydrogen energy industry is rapidly developed, wherein in the hydrogen energy storage and transportation technology, high-pressure hydrogen storage is a hydrogen storage technology with great commercial application prospect, and becomes a main mode of hydrogen energy storage and transportation at present. Under the environment of normal temperature and high pressure hydrogen, the high pressure hydrogen storage container can cause the possibility of hydrogen embrittlement and further failure of the material because hydrogen can be adsorbed, dissolved, diffused and aggregated on the surface of a metal material. To ensure long-term, stable and reliable operation, it is important for the high-pressure hydrogen storage container to study the hydrogen brittleness sensitivity of the material.
The existing material hydrogen embrittlement sensitivity test methods mainly comprise two methods, namely, after a sample is electrochemically charged with hydrogen, a slow tensile test is carried out; and secondly, directly performing a slow tensile test in a normal-temperature high-pressure hydrogen environment. The former device is simple and convenient, and is easy to operate, but the hydrogen concentration is difficult to avoid reduction caused by the diffusion of hydrogen; the latter needs to be carried out in a high-pressure cavity, the used medium is high-pressure high-purity hydrogen, and the hydrogen is an explosive hazard source, so that the test has high risk and high price, and is difficult to popularize in domestic laboratories. Meanwhile, both methods can only qualitatively evaluate whether the material has the possibility of hydrogen embrittlement, but cannot explain the hydrogen embrittlement sensitivity degree of the material under the stress state in actual use.
In view of the current situation, it is necessary to invent a hydrogen embrittlement sensitivity test method for a material capable of simulating a stress state of a gas cylinder, and on the premise of ensuring safety, whether a material has a possibility of a destructive vicious accident under a static load lower than the tensile strength of the material in an actual use stress state is evaluated.
Disclosure of Invention
The invention aims to solve the problems and provides a device and a method for testing hydrogen brittleness sensitivity of a material simulating the stress state of a gas cylinder.
The invention is realized by the following technical scheme:
a material hydrogen embrittlement sensitivity test device for simulating the stress state of a gas cylinder comprises a sample capable of being electrochemically charged with hydrogen, a medium tank containing an electrolytic charged hydrogen solution, a testing machine capable of applying tensile stress, a constant potential rectifier and a graphite rod or a lead plate serving as an anode;
the sample, the testing machine and the graphite rod or the lead plate are all arranged in the medium tank, the cathode of the potentiostat is connected with the sample through a connecting lead, and the anode of the potentiostat is connected with the graphite rod or the lead plate.
Further, the electrolytic hydrogen charging solution comprises 0.5mol/L of dilute sulfuric acid solution and 200mg/L of antimony trioxide serving as a poisoning agent.
A method for testing hydrogen brittleness sensitivity of a material for simulating a stress state of a gas cylinder mainly comprises the following steps:
determining the maximum stress borne by a gas cylinder material in a calculation or simulation mode according to the design parameters of the gas cylinder;
polishing the sample smoothly, and mounting the sample on a testing machine which is installed in a medium tank and can apply tensile stress after ultrasonic cleaning;
connecting a cathode connecting lead to the sample, and inserting a graphite rod or a lead plate serving as an anode into the medium tank;
step four, loading the sample by using a testing machine capable of applying tensile stress until the maximum stress determined in the step one is reached; meanwhile, adding an electrolytic hydrogen charging solution into the medium groove, and regulating a constant potential rectifier to perform electrochemical hydrogen charging on the sample;
step five, after the whole system is maintained for a preset time, unloading the tensile stress, taking out the sample, and observing the surface crack condition of the sample;
and step six, breaking the test sample on a testing machine, and observing whether the fracture has crack initiation and expansion.
Furthermore, in the second step, the ultrasonic cleaning is carried out by adopting analytically pure alcohol.
Further, the electrolytic hydrogen-charging solution in the fourth step comprises a dilute sulphuric acid solution of 0.5mol/L and antimony trioxide of 200mg/L as a poisoning agent.
The invention has the beneficial effects that:
by adopting the method for testing the hydrogen embrittlement sensitivity of the material for simulating the stress state of the gas cylinder, the hydrogen content of the material facing a high-pressure hydrogen storage container is simulated by electrochemical hydrogen charging, and the tensile force of the material of the hydrogen storage container under the actual service working condition is simulated by a testing machine capable of applying tensile stress, so that the possible problem that whether the material has a low-stress embrittlement failure damage vicious accident or not in the actual use stress state cannot be evaluated in the hydrogen embrittlement sensitivity research of the existing material is solved, and the method is simple to operate and convenient to use.
Drawings
FIG. 1 is a schematic diagram of the construction of the test apparatus of the present invention;
reference numerals: 1. sample, 2, medium tank, 3, testing machine, 4, lead plate, 5 and constant potential rectifier.
Detailed Description
The technical solution in the embodiments of the present invention is clearly and completely described below with reference to the accompanying drawings.
Example 1
As shown in the figure, the material hydrogen embrittlement sensitivity test device for simulating the stress state of the gas cylinder comprises a sample 1 capable of being electrochemically charged, a medium tank 2 containing an electrolytic charging solution, a testing machine 3 capable of applying tensile stress, a potentiostat 5 and a graphite rod or lead plate 4 serving as an anode;
the sample 1, the testing machine 3 and the graphite rod or the lead plate 4 are all arranged in the medium tank 2, the cathode of the constant potential rectifier 5 is connected with the sample 1 through a connecting lead, and the anode of the constant potential rectifier 5 is connected with the graphite rod or the lead plate 4.
The invention discloses a method for testing hydrogen brittleness sensitivity of a material for simulating the stress state of a gas cylinder, which comprises the following steps:
1) according to the design parameters of the gas cylinder, the maximum stress level born by the simulated 50MPa high-pressure hydrogen storage container material 4130X is 350 MPa;
2) polishing the working section of the sample 1 smoothly, putting the sample into analytically pure alcohol, performing ultrasonic cleaning for about 15min to remove dirt such as surface grease and the like, and then installing the sample on a testing machine 3 which is installed in a medium tank 2 and can apply tensile stress;
3) connecting a cathode connecting lead to the sample 1, and inserting a graphite rod or a lead plate 4 as an anode into the medium tank 2;
4) loading the sample 1 by using a testing machine 3 capable of applying tensile stress until the determined maximum stress is 350 MPa;
5) adding electrolytic hydrogen solution (0.5 mol/L dilute sulfuric acid solution containing 200mg/L poisoning agent antimony trioxide) into the medium tank 2, and adjusting the potentiostat 5 to 10mA/cm 2 Electrochemical charging of sample 1 with current density of (a);
6) after the whole system is maintained for 240 hours, unloading the tensile stress, taking out the sample 1, and observing the surface crack condition of the sample 1, wherein according to the earlier test, the hydrogen content in the sample 1 is about 3.6 ppm;
7) the test sample 1 is pulled off on a testing machine, and crack initiation and propagation are not observed in the fracture, which shows that the 4130X material has lower hydrogen brittleness sensitivity in the stress state and is suitable for being used as a 50MPa high-pressure hydrogen storage container material.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (5)
1. The utility model provides a material hydrogen embrittlement sensitivity test device of simulation gas cylinder stress state which characterized in that: comprises a sample (1) capable of being electrochemically charged, a medium tank (2) containing an electrolytic hydrogen charging solution, a testing machine (3) capable of applying tensile stress, a constant potential rectifier (5) and a graphite rod or lead plate (4) as an anode;
the sample (1), the testing machine (3) and the graphite rod or the lead plate (4) are all arranged in the medium tank (2), the cathode of the potentiostat (5) is connected with the sample (1) through a connecting lead, and the anode of the potentiostat (5) is connected with the graphite rod or the lead plate (4).
2. The device for testing the hydrogen embrittlement sensitivity of the material for simulating the stress state of the gas cylinder according to claim 1, is characterized in that: the electrolytic hydrogen charging solution comprises 0.5mol/L of dilute sulphuric acid solution and 200mg/L of poisoning agent antimony trioxide.
3. The method for testing hydrogen embrittlement sensitivity of materials simulating stress states of gas cylinders, according to claim 1, is characterized in that: the method mainly comprises the following steps:
determining the maximum stress born by a gas cylinder material in a calculation or simulation mode according to the design parameters of the gas cylinder;
polishing the sample smoothly, and mounting the sample on a testing machine which is installed in a medium tank and can apply tensile stress after ultrasonic cleaning;
connecting a cathode connecting lead to the sample, and inserting a graphite rod or a lead plate serving as an anode into the medium tank;
step four, loading the sample by using a testing machine capable of applying tensile stress until the maximum stress determined in the step one is reached; meanwhile, adding an electrolytic hydrogen charging solution into the medium groove, and adjusting a constant potential rectifier to perform electrochemical hydrogen charging on the sample;
step five, after the whole system is maintained for a preset time, unloading the tensile stress, taking out the sample, and observing the surface crack condition of the sample;
and step six, breaking the test sample on a testing machine, and observing whether the fracture has crack initiation and expansion.
4. The method for testing hydrogen embrittlement sensitivity of materials simulating stress states of gas cylinders, according to claim 3, is characterized in that: and in the second step, the ultrasonic cleaning is carried out by adopting analytically pure alcohol.
5. The method for testing hydrogen embrittlement sensitivity of materials simulating stress states of gas cylinders, according to claim 3, is characterized in that: the electrolytic hydrogen-charging solution in the fourth step comprises 0.5mol/L of dilute sulphuric acid solution and 200mg/L of antimony trioxide serving as a poisoning agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210165488.8A CN115032063A (en) | 2022-02-23 | 2022-02-23 | Device and method for testing hydrogen embrittlement sensitivity of material for simulating stress state of gas cylinder |
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| CN202210165488.8A CN115032063A (en) | 2022-02-23 | 2022-02-23 | Device and method for testing hydrogen embrittlement sensitivity of material for simulating stress state of gas cylinder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117110053A (en) * | 2023-10-23 | 2023-11-24 | 中铝材料应用研究院有限公司 | Method for testing hydrogen embrittlement sensitivity of aluminum alloy material in simulated high-pressure hydrogen environment |
| CN117629741A (en) * | 2023-10-19 | 2024-03-01 | 合肥通用机械研究院有限公司 | Characterization method for hydrogen embrittlement sensitivity parameter of hydrogen energy storage and transportation equipment material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180248A (en) * | 1996-10-02 | 1998-04-29 | 日本电池株式会社 | Enclosed lead accumulator and its manufacturing method |
| JP2009069004A (en) * | 2007-09-13 | 2009-04-02 | Nippon Steel Corp | Device and method for evaluating hydrogen embrittlement of thin steel sheet |
| CN105987847A (en) * | 2015-03-04 | 2016-10-05 | 天津市海王星海上工程技术股份有限公司 | Steel hydrogen embrittlement test device under cathode protection in marine environment and test method |
| CN107764663A (en) * | 2016-08-23 | 2018-03-06 | 张宇 | A kind of hydrogen embrittlement evaluation method |
-
2022
- 2022-02-23 CN CN202210165488.8A patent/CN115032063A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180248A (en) * | 1996-10-02 | 1998-04-29 | 日本电池株式会社 | Enclosed lead accumulator and its manufacturing method |
| JP2009069004A (en) * | 2007-09-13 | 2009-04-02 | Nippon Steel Corp | Device and method for evaluating hydrogen embrittlement of thin steel sheet |
| CN105987847A (en) * | 2015-03-04 | 2016-10-05 | 天津市海王星海上工程技术股份有限公司 | Steel hydrogen embrittlement test device under cathode protection in marine environment and test method |
| CN107764663A (en) * | 2016-08-23 | 2018-03-06 | 张宇 | A kind of hydrogen embrittlement evaluation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117629741A (en) * | 2023-10-19 | 2024-03-01 | 合肥通用机械研究院有限公司 | Characterization method for hydrogen embrittlement sensitivity parameter of hydrogen energy storage and transportation equipment material |
| CN117110053A (en) * | 2023-10-23 | 2023-11-24 | 中铝材料应用研究院有限公司 | Method for testing hydrogen embrittlement sensitivity of aluminum alloy material in simulated high-pressure hydrogen environment |
| CN117110053B (en) * | 2023-10-23 | 2023-12-19 | 中铝材料应用研究院有限公司 | Method for testing hydrogen embrittlement sensitivity of aluminum alloy material in simulated high-pressure hydrogen environment |
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