CN112945660A - Test method for detecting hydrogen embrittlement sensitivity of steel - Google Patents
Test method for detecting hydrogen embrittlement sensitivity of steel Download PDFInfo
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- CN112945660A CN112945660A CN202110095175.5A CN202110095175A CN112945660A CN 112945660 A CN112945660 A CN 112945660A CN 202110095175 A CN202110095175 A CN 202110095175A CN 112945660 A CN112945660 A CN 112945660A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 132
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 132
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 99
- 239000010959 steel Substances 0.000 title claims abstract description 99
- 230000035945 sensitivity Effects 0.000 title claims abstract description 38
- 238000010998 test method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000009864 tensile test Methods 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 8
- 230000009467 reduction Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910000797 Ultra-high-strength steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000007704 transition Effects 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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention discloses a test method for detecting hydrogen embrittlement sensitivity of steel, which comprises the following steps: performing electrochemical hydrogen charging on a steel sample to be detected, performing a tensile test on the steel sample after hydrogen charging, measuring and obtaining the hydrogen content of the steel sample and the mechanical properties under different hydrogen contents, and drawing a hydrogen content-mechanical property curve, wherein the hydrogen content corresponding to an inflection point of the curve is the critical hydrogen content of the steel, namely the hydrogen embrittlement sensitivity of the steel sample. The test method for detecting the hydrogen embrittlement sensitivity of the steel is simple and high in test speed, and the tensile rate of the tensile test method is 2 orders of magnitude higher than the traditional slow tensile rate, so that the trouble of sample storage after hydrogen charging is eliminated, the problem that hydrogen escapes from steel due to overlong tensile world in the process of slow tensile and quick load is solved, and overall, the requirements of equipment and personnel are reduced, the test detection time is shortened, and the detection cost is reduced.
Description
Technical Field
The present invention relates to the field of determining hydrogen embrittlement sensitivity. More specifically, the invention relates to a test method for detecting hydrogen embrittlement sensitivity of steel.
Background
When the tensile strength of the ultrahigh-strength steel exceeds 1000MPa, the performance of the material is reduced due to a very small amount of hydrogen, so that the hydrogen induced cracking phenomenon occurs. The hydrogen embrittlement of steel which is fractured under mild corrosive environment and the hydrogen induced cracking under atmospheric environment become very significant. Recently, due to the higher requirements of people on energy conservation and emission reduction, materials such as hydrogen energy equipment and high-strength automobile parts are increasingly used, and if the materials generate hydrogen-induced cracking, irremediable consequences can be caused. Different steel materials have different sensibility to hydrogen, so that the sensitivity to hydrogen brittleness of the steel materials is detected, and data support can be provided for the practical application of the steel materials in the actual environment.
The existing method for detecting the hydrogen embrittlement sensitivity of steel mostly adopts a slow tensile testing machine (the tensile rate is about 0.005 mm/min) or a constant load test, and the detection time of each sample generally exceeds 3 days or even 1 week. Therefore, one type of the method is to charge hydrogen directly in the process of a slow stretching or constant load test, the method needs to bind two devices for use, a special test box is needed to be arranged for filling solution while the flexibility is lacked, and insulation treatment is needed between a sample and a clamp; the other is that the constant load time of the stretcher is too long, the surface coating of the sample needs to be prevented from hydrogen escaping after hydrogen is charged, and after the slow stretching or the constant load is finished, the coating needs to be removed so as to measure the hydrogen. If the plating effect is not good, the method is easy to cause error of the test result, and the sample treatment is troublesome. The two methods have high requirements on the technical level of detection personnel and are greatly influenced by human.
Disclosure of Invention
To achieve these objects and other advantages in accordance with the present invention, a test method for detecting hydrogen embrittlement sensitivity of a steel material is provided, which includes the steps of:
carrying out electrochemical hydrogen charging on a steel sample to be detected, charging hydrogen with different contents into the steel sample by adjusting different current values in the electrochemical hydrogen charging process, measuring to obtain the mechanical properties of the steel sample under different hydrogen contents, drawing a hydrogen content-mechanical property curve, wherein the hydrogen content corresponding to the inflection point of the curve is the critical hydrogen content of the steel, and is used for judging the hydrogen brittleness sensitivity of the steel sample: the larger the critical hydrogen content value, the lower the hydrogen embrittlement sensitivity of the steel sample.
According to a preferred embodiment of the present invention, the electrochemical hydrogen charging process of the steel sample comprises: and the platinum electrode and the steel sample are respectively connected to the anode and the cathode of a power supply, and are placed in a hydrogen charging solution to electrify the connected loop.
According to a preferred embodiment of the present invention, the mechanical properties of the steel sample are measured using a tensile test;
wherein, the hydrogen content of the steel sample is measured, which specifically comprises the following steps: sampling the fracture position of the steel sample which is broken in the tensile test, and measuring the hydrogen content of the sampling sample, namely the hydrogen content of the steel sample.
According to a preferred embodiment of the present invention, the sampled sample is subjected to acetone dehydration and absolute ethanol washing after sampling.
According to a preferred embodiment of the present invention, the hydrogen content of the sampled sample is measured by a hydrogen meter, and the measurement temperature is maintained at 600-800 ℃.
According to a preferred embodiment of the present invention, the maximum tensile force is not less than 5KN and the minimum tensile rate is 1mm/min in the tensile test.
According to a preferred embodiment of the invention, the time interval between the removal of the steel sample after the hydrogen charging and the tensile test should not be greater than 6 hours.
According to a preferred embodiment of the invention, the power supply is a constant current power supply, and the resolution of the power supply is up to 0.1 mA.
According to a preferred embodiment of the invention, the mechanical property is in particular the area reduction ratio.
The invention at least comprises the following beneficial effects:
1. the test method for detecting the hydrogen embrittlement sensitivity of the steel is simple and high in test speed, and the tensile rate of the tensile test method is 2 orders of magnitude higher than the traditional slow tensile rate, the trouble of sample storage after hydrogen charging is eliminated, the problem that hydrogen escapes from steel due to overlong tensile world in the process of slow tensile and quick constant load is solved, and overall, the requirements of equipment and personnel are reduced, the test detection time is shortened, and the detection cost is reduced.
2. The test method for detecting the hydrogen embrittlement sensitivity of the steel obtains the specific critical hydrogen content value of the steel sample according to the prepared hydrogen content-surface shrinkage curve, namely the method can quantitatively calculate the hydrogen embrittlement sensitivity of the steel sample, and quantitatively judge the hydrogen embrittlement sensitivity of the steel only according to manual experience (for example, judging the hydrogen embrittlement sensitivity to be strong or weak according to the shape of a fracture after stretching) compared with the conventional method, so that the test method plays a better guiding role in the precision use of the steel.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
Fig. 1 is a schematic diagram of an electrochemical hydrogen charging process involved in the present invention.
FIG. 2 is a schematic diagram of the tensile test process involved in the present invention.
Fig. 3 is a schematic structural view of a hydrogen meter according to the present invention.
FIG. 4 is a graph of hydrogen content versus area reduction ratio in an embodiment of the present invention.
1: a constant current power supply; 2: a wire; 3: a steel sample; 4: a beaker; 5: a platinum electrode; 6, electrolyte; 7: a tensile testing machine; 8: a sample heating device; 9: a gas sampler; 10: a gas chromatograph.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art. The basic principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
As shown in FIGS. 1-4, a preferred embodiment of the present invention provides a test method for detecting hydrogen embrittlement sensitivity of a steel material, comprising the steps of:
the electrochemical hydrogen filling is carried out on a steel sample to be detected, hydrogen with different contents is filled into the steel sample by adjusting different current values in the electrochemical hydrogen filling process, the mechanical properties of the steel sample under different hydrogen contents are obtained through measurement (specifically, the mechanical property measurement is carried out through a tensile test), a hydrogen content-mechanical property curve is drawn, and the hydrogen content corresponding to the inflection point of the curve is the critical hydrogen content of the steel, namely the hydrogen brittleness sensitivity of the steel sample.
In the embodiment, three process systems of electrochemical hydrogen charging, tensile test and hydrogen measurement are creatively combined together, the test method for quickly and efficiently obtaining hydrogen embrittlement sensitivity is realized, the method is simple, the test speed is high, the trouble of sample storage after hydrogen charging is eliminated, and the problem that hydrogen escapes from steel due to overlong tensile world in the process of slow stretching and quick load is solved.
As shown in fig. 4, the vertical axis surface reduction ratio is a ratio of a surface reduction ratio of the steel sample after the hydrogen charging to a surface reduction ratio of the steel sample before the hydrogen charging, the surface reduction ratio is a test characterization value of "strength and plasticity", and the larger the critical hydrogen content in the curve is, the lower the hydrogen embrittlement sensitivity of the steel sample is. And (3) obtaining the surface shrinkage of the steel sample through a tensile test, and finally drawing a relation curve of the surface shrinkage and the hydrogen content measured by a hydrogen measuring instrument, wherein the inflection point of the curve is the critical hydrogen content. Wherein, in the tensile test, the maximum tensile force is not less than 5KN, and the minimum tensile rate is 1 mm/min.
Specifically, the shape of the steel sample is not limited, and may be various shapes, such as a round bar shape, a length of 30mm, a diameter of 6mm, and a transition arc radius R of 10mm, when the steel sample is in the above shape and size, the corresponding hydrogen content-face reduction curve is prepared by the above method, wherein the critical hydrogen content of the steel sample is 1.5ppm, that is, the method of the present invention can quantitatively calculate the hydrogen embrittlement sensitivity of the steel sample, and quantitatively judge the hydrogen embrittlement sensitivity of the steel sample only according to manual experience (for example, judge the hydrogen embrittlement sensitivity of the steel by the fracture shape after stretching), which can better guide the precision use of the steel.
Wherein, the hydrogen content of the steel sample is measured by a hydrogen measuring instrument, as shown in fig. 3, the hydrogen measuring instrument consists of three major parts, namely a sample heating device 8, a gas sampler 9 and a gas chromatograph 10; after a steel sample to be detected is fractured in a tensile test, taking a sample near the fracture site of the tensile test, wherein the length of the sample is 10mm, putting the sample into a sample heating device, heating at the speed of 100 ℃/h, and obtaining the hydrogen content of the sample through a gas sampler 9 and a gas chromatograph 10;
in another preferred embodiment of the present invention, as shown in fig. 1, the electrochemical hydrogen charging process specifically includes: the electrochemical hydrogen charging process comprises the steps that the constant current power supply 1 is connected with a platinum electrode 5 and a steel sample 3 which are soaked in the electrolyte 6 through the lead 2, the platinum electrode 5 and the steel sample 3 are respectively connected with the anode and the cathode of the power supply, the electrolyte 6 is placed in a container, the beaker 4 can be adopted during actual use, and H ionized from the electrolyte 6 can be achieved by applying a certain current (namely, the power supply is switched on) through the beaker 4+Adsorbed on the surface of a steel sample 3, wherein a part of H+After the electrons are obtained, the hydrogen atoms are diffused into the steel sample 3, and the steel sample can be taken out after the hydrogen is filled for a certain time.
It is emphasized that, in order to prevent the hydrogen gas in the steel material sample from diffusing away from the steel for the tensile test with time, the time interval from the taking out of the steel material sample after the charging to the tensile test should be not more than 6 hours.
In another preferred embodiment of the invention, after the electrochemical hydrogen charging of the steel sample is finished, the steel sample is arranged on a tensile testing machine, and a tensile test is carried out at a tensile rate of 1mm/min until the steel sample is broken, so as to obtain the strength and the plasticity of the steel sample. After the steel sample is fractured, taking a sample near the fracture site, wherein the length of the sample is 10mm, putting the sample into a sample heating device, heating at the speed of 100 ℃/h, and obtaining the hydrogen content of the sample through a gas sampler and a gas chromatograph;
in another preferred embodiment of the present invention, in the test method for detecting hydrogen embrittlement sensitivity of steel, the method for measuring and obtaining hydrogen content of a steel sample by using TDS hydrogen measurement method specifically includes:
sampling the fracture position of the steel sample which is broken in the tensile test, and measuring the hydrogen content of the sampling sample, namely the hydrogen content of the steel sample.
In another preferred embodiment of the invention, in the test method for detecting the hydrogen embrittlement sensitivity of steel, after sampling, the sampled sample is subjected to acetone dehydration and absolute ethanol cleaning, and impurities on the surface of the sampled sample are cleaned, so that the subsequent measurement is prevented from being influenced.
According to a preferred embodiment of the present invention, in the test method for detecting hydrogen embrittlement sensitivity of steel, a hydrogen content measurement is performed on the sample by using a hydrogen measuring instrument, and the measurement temperature is maintained at 600-.
According to a preferred embodiment of the present invention, in the test method for detecting hydrogen embrittlement sensitivity of steel, the power supply is a constant current power supply, and the resolution ratio thereof should reach 0.1 mA.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (9)
1. A test method for detecting hydrogen embrittlement sensitivity of steel is characterized by comprising the following steps:
the method comprises the steps of performing electrochemical hydrogen charging on a steel sample to be detected, charging hydrogen with different contents into the steel sample by adjusting different current values in the electrochemical hydrogen charging process, measuring mechanical properties of the steel sample under different hydrogen contents, drawing a hydrogen content-mechanical property curve, determining the hydrogen content corresponding to an inflection point of the curve as the critical hydrogen content of the steel, and judging the hydrogen brittleness sensitivity of the steel sample according to the critical hydrogen content.
2. The test method for detecting hydrogen embrittlement sensitivity of steel products according to claim 1, wherein the electrochemical hydrogen charging process of the steel product sample is specifically as follows: and the platinum electrode and the steel sample are respectively connected to the anode and the cathode of a power supply, and are placed in a hydrogen charging solution to electrify the connected loop.
3. A test method for detecting hydrogen embrittlement sensitivity of steel products as claimed in claim 1, wherein the mechanical properties of the steel product after hydrogen charging are measured by tensile test;
wherein, the hydrogen content of the steel sample is measured, which specifically comprises the following steps: sampling the fracture position of the steel sample which is broken in the tensile test, and measuring the hydrogen content of the sampling sample, namely the hydrogen content of the steel sample.
4. A test method for detecting hydrogen embrittlement sensitivity of steel products according to claim 3, wherein the sampled sample is subjected to acetone dehydration and absolute ethanol washing after sampling.
5. The test method for detecting the hydrogen embrittlement sensitivity of steel products as claimed in claim 3, wherein the hydrogen content of the sampled sample is measured by a hydrogen measuring instrument, and the measurement temperature is maintained at 600-800 ℃.
6. A test method for detecting hydrogen embrittlement sensitivity of steel products as claimed in claim 3, wherein the maximum tensile force in the tensile test is not less than 5KN and the minimum tensile rate is 1 mm/min.
7. A test method for detecting hydrogen embrittlement sensitivity of a steel material as claimed in claim 3, wherein the time interval between the taking out of the steel material sample after charging with hydrogen and the performing of the tensile test is not more than 6 hours.
8. A test method for detecting hydrogen embrittlement sensitivity of steel products as claimed in claim 2, wherein the power supply is a constant current power supply, and the resolution is 0.1 mA.
9. A test method for detecting hydrogen embrittlement sensitivity of steel products according to claim 1, wherein the mechanical properties are surface shrinkage after the breaking of the sample.
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Cited By (3)
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| CN115017694A (en) * | 2022-05-31 | 2022-09-06 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | Test method for simulating hydrogen embrittlement of buried pipeline under interference current and constant-pull load |
| CN115480039A (en) * | 2022-09-26 | 2022-12-16 | 江苏锡信工程检测有限公司 | Detection method and system for detecting hydrogen embrittlement sensitivity of steel |
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