CN116642753A - Hydrogen embrittlement sensitivity testing device and method - Google Patents
Hydrogen embrittlement sensitivity testing device and method Download PDFInfo
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- CN116642753A CN116642753A CN202310617018.5A CN202310617018A CN116642753A CN 116642753 A CN116642753 A CN 116642753A CN 202310617018 A CN202310617018 A CN 202310617018A CN 116642753 A CN116642753 A CN 116642753A
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 54
- 239000001257 hydrogen Substances 0.000 title claims abstract description 54
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000012360 testing method Methods 0.000 title claims abstract description 35
- 230000035945 sensitivity Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 14
- 239000003792 electrolyte Substances 0.000 claims abstract description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- 238000007600 charging Methods 0.000 claims description 23
- 238000007789 sealing Methods 0.000 claims description 22
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000012466 permeate Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 20
- 230000000630 rising effect Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 239000011229 interlayer Substances 0.000 description 15
- 238000009434 installation Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 4
- 238000009864 tensile test Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010325 electrochemical charging Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 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
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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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
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/04—Chucks
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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
-
- 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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- Physics & Mathematics (AREA)
- 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)
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- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a hydrogen embrittlement sensitivity testing device and method, comprising the following steps: the bottom electrolytic cell, the cover plate, the inner corrugated pipe, the outer corrugated pipe, the rod sample and the like, when the rod sample is stretched to generate axial elongation, the cover plate rises along with the axial elongation, the outer corrugated pipe and the inner corrugated pipe are driven to be uniformly elongated at the moment, the corrugated folds of the outer corrugated pipe and the inner corrugated pipe are stretched to be long, the liquid surface area is reduced to form a liquid level rising trend, meanwhile, the rod sample is stretched to cause a liquid level extending trend of a gauge length section, the whole process of immersing of the gauge length section of the rod sample in electrolyte can be ensured under the combined action of the liquid level rising trend, the overflow of hydrogen is reduced, and meanwhile, the set current density parameter is ensured to be kept stable.
Description
Technical Field
The invention relates to the field of metal mechanical property detection test equipment and method, in particular to a hydrogen embrittlement sensitivity test device and method.
Background
Hydrogen is very likely to penetrate into the gaps between other atoms and molecules in long-term contact with the hydrogen (mainly referred to as metal materials), so that the properties of the materials are affected, the properties are mainly represented by degradation of various properties, irreversible property damage is generated, and the negative effects on important mechanical properties (mainly toughness and fracture resistance) of the metal materials are called hydrogen embrittlement. In order to explore the fundamental mechanism of hydrogen embrittlement, the law of influence of hydrogen on the mechanical properties of materials and the mechanism of performance degradation are necessary to explore in a laboratory environment, wherein the hydrogen embrittlement sensitivity of the materials obtained by carrying out a slow strain rate uniaxial loading tensile test on the materials is a main evaluation means for researching the hydrogen embrittlement.
In the prior art, the sample is subjected to hydrogen charging treatment before or during a hydrogen embrittlement sensitivity experiment, and the main method comprises the following steps: room temperature gas phase charging, high temperature high pressure charging, chemical corrosion charging and electrochemical charging. Because of a certain danger of gaseous hydrogen charging, the electrochemical hydrogen charging device is simple, convenient to operate, safe and stable, and a great amount of domestic researches are carried out by adopting an electrochemical cathode pre-charging method.
However, a certain time is required between the end of the pre-charging and the completion of the sample installation and the beginning of the tensile test, during which the hydrogen entering the metal sample through the pre-charging can continuously escape, and usually, the slow strain rate tensile test usually needs tens of minutes, the hydrogen inside the metal sample can escape more quickly under the action of tensile stress, particularly, the uniform and stable hydrogen concentration inside the sample cannot be ensured aiming at the metal material with relatively high hydrogen diffusion rate, such as low carbon steel and the like, and the accuracy and the reliability of the test result are seriously affected, so that the sample is considered to be kept in the hydrogen charging environment electrolyte in the whole process before or during the beginning of the tensile test, and the hydrogen escape is reduced, but under the condition, the sample can cause the partial gauge length section to be exposed out of the water surface due to the excessively high elongation rate, so that the current density parameter is changed, and the inaccuracy and the error of the test result are caused.
Disclosure of Invention
The invention aims to overcome the problems in the prior art, and provides a hydrogen embrittlement sensitivity testing device and a hydrogen embrittlement sensitivity testing method which can keep a rod sample in an electrolyte in a hydrogen charging environment and overcome the problem that part of a gauge length section is exposed to the water surface along with the stretching of the sample under the condition.
In one aspect, the present invention provides a hydrogen embrittlement sensitivity test device comprising:
the electrolytic cell comprises a bottom plate and a barrel body, wherein the barrel body is arranged on the bottom plate, the outer diameter of the bottom plate is larger than that of the barrel body, a connecting channel is formed in the bottom plate, one end of the connecting channel is provided with a first opening on the upper surface of the bottom plate, the first opening is positioned in the barrel body, the other end of the connecting channel is provided with a second opening on the upper surface of the bottom plate, the second opening is positioned outside the barrel body, the inside of the barrel body is used for containing electrolyte, the bottom plate can be connected with the bottom of a rod sample, and the rod sample is positioned in the barrel body;
the cover plate is positioned above the cylinder body, an air outlet is formed in the cover plate, and the cover plate can be connected with the top of the rod sample;
the inner corrugated pipe is arranged between the bottom plate and the cover plate, and the cylinder body is sleeved in the inner corrugated pipe;
the outer corrugated pipe is arranged between the bottom plate and the cover plate, the inner corrugated pipe is sleeved in the outer corrugated pipe, an interlayer space is arranged between the inner corrugated pipe and the outer corrugated pipe, the second opening is arranged between the inner corrugated pipe and the outer corrugated pipe, the connecting channel is communicated with the interlayer space, and the air outlet is communicated with the interlayer space.
Further, the installation base is provided with a groove, the bottom plate is arranged in the groove, the middle part of the bottom plate is provided with a first through hole, the middle part of the bottom plate is provided with an installation groove, the bottom end of the rod sample is provided with a lower fixing part, the lower fixing part penetrates through the first through hole to enter the installation groove, and the lower fixing part is detachably connected in the installation groove.
Further, the lower end of the mounting base is provided with a clamping end, and the clamping end is used for clamping by external clamping equipment.
Further, the outer side wall of the lower fixing part is provided with a first external thread, the inner side wall of the mounting groove is provided with a first internal thread matched with the first external thread, and the lower fixing part is detachably connected with the mounting groove in a threaded connection mode.
Further, the method further comprises the following steps: the annular sealing plug is arranged between the outer side wall of the lower fixing part and the inner side wall of the first through hole.
Further, the annular sealing plug is fixedly sleeved on the outer side of the lower fixing part, a second external thread is arranged on the outer side wall of the annular sealing plug, a second internal thread matched with the second external thread is arranged on the inner side wall of the first through hole, and the annular sealing plug is detachably connected in the first through hole of the bottom plate in a threaded connection mode.
Further, the upper ends of the outer corrugated pipe and the inner corrugated pipe are detachably connected to the lower surface of the cover plate in a buckling connection mode.
Further, the upper end of the rod sample is connected with an upper fixing part which is detachably connected with the cover plate.
Further, the second through hole has been seted up to the central part of apron, and go up the fixed part and pass the second through hole, and threaded connection has fastening nut on the lateral wall of last fixed part, and fastening nut is located the below of apron, and fastening nut is used for realizing the detachable relation of connection between fixed part and the apron.
On the other hand, the invention also provides a hydrogen embrittlement sensitivity test method, which is suitable for the hydrogen embrittlement sensitivity test device of any one of the above, and comprises the following steps:
and 1, polishing the rod sample to more than 1000 meshes, confirming a gauge length section and a connecting section connected with a bottom plate and a cover plate on the rod sample, and performing nickel plating or wax sealing treatment on the parts except the gauge length section and the connecting section.
Step 2, the sample is arranged between the cover plate and the bottom plate and is connected with the anode of an external direct current power supply, the cathode of the external direct current power supply is connected with an external platinum electrode, the lower end of the platinum electrode also stretches into the electrolytic cell,
and 3, installing the inner corrugated pipe and the outer corrugated pipe between the cover plate and the bottom plate.
Step 4, injecting electrolyte into the electrolytic cell, placing the rod sample and the platinum electrode into the electrolytic cell, enabling the electrolyte to permeate the gauge length section of the rod sample,
step 5, clamping and fixing the rod sample by using an external lifting device and a clamping system, preparing to apply vertical up-and-down tensile load to the rod sample, and determining the hydrogen charging current I according to the following formula:
I＝π×d×L×a，
where d is the diameter of the rod specimen, L is the gauge length, and a is the charging current density as determined by the test requirements.
And starting an external direct current power supply, and starting electrochemical hydrogen charging operation.
And 6, after 2 minutes, observing whether the hydrogen charging operation is stable or not, and using an external lifting device and a clamping system to stretch the rod sample to start the hydrogen embrittlement sensitivity test.
Compared with the prior art, the invention has the beneficial effects that: when the rod sample is stretched to generate axial elongation, the cover plate is connected with the upper end of the rod sample, the cover plate is lifted along with the rod sample, the outer corrugated pipe and the inner corrugated pipe are driven to be uniformly elongated, an interlayer space between the outer corrugated pipe and the inner corrugated pipe is also stretched and deformed along with the inner corrugated pipe, the corrugated folds of the outer corrugated pipe and the inner corrugated pipe are stretched and lengthened, the liquid surface area of the interlayer space is reduced, the liquid surface area is reduced to form a liquid level rising trend, and meanwhile, the rod sample is stretched to lead to a liquid level extending trend of a gauge length section, and under the combined action of the liquid level rising trend, the whole process of immersing of the gauge length section of the rod sample in electrolyte is ensured, so that the overflow of hydrogen is reduced, and meanwhile, the set current density parameter is kept stable.
Drawings
FIG. 1 is a front cross-sectional view of an overall structure of one embodiment of the present invention;
fig. 2 is a schematic top view of a part of a structure of an embodiment of the present invention.
Reference numerals illustrate:
1. a bar sample; 2. a cover plate; 3. an outer bellows; 4. an inner bellows; 5. a cylinder; 6. a bottom plate; 7. a mounting base; 8. a clamping end; 9. an annular sealing plug; 10. a connection channel; 11. a platinum electrode; 12. a fastening nut; 15. an external DC power supply.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a hydrogen embrittlement sensitivity test device and a method.
In one aspect, the present invention provides a hydrogen embrittlement sensitivity test device comprising: the electrolytic cell comprises a bottom plate 6 and a barrel 5, wherein the barrel 5 is arranged on the bottom plate 6, the outer diameter of the bottom plate 6 is larger than that of the barrel 5, a connecting channel 10 is formed in the bottom plate 6, one end of the connecting channel 10 is provided with a first opening on the upper surface of the bottom plate 6, the first opening is positioned in the barrel 5, the other end of the connecting channel 10 is provided with a second opening on the upper surface of the bottom plate 6, the second opening is positioned outside the barrel 5, the inside of the barrel 5 is used for containing electrolyte, the bottom plate 6 can be connected with the bottom of one rod sample 1, and the rod sample 1 is positioned in the barrel 5; the cover plate 2 is positioned above the cylinder body, an air outlet is formed in the cover plate, and the cover plate 2 can be connected with the top of the rod sample 1; the inner corrugated pipe 4 is arranged between the bottom plate 6 and the cover plate 2, and the cylinder 5 is sleeved inside the inner corrugated pipe 4; the outer corrugated pipe 3 is arranged between the bottom plate 6 and the cover plate 2, the inner corrugated pipe 4 is sleeved in the outer corrugated pipe 3, an interlayer space is arranged between the inner corrugated pipe 4 and the outer corrugated pipe 3, the second opening is arranged between the inner corrugated pipe 4 and the outer corrugated pipe 3, the connecting channel 10 is communicated with the interlayer space, and the air outlet is communicated with the interlayer space.
Specifically, please refer to fig. 1 and 2, when an online electrochemical hydrogen embrittlement sensitivity test is performed, an external stretching clamping device can generate an up-down stretching load in a vertical direction at the upper end and the lower end of the rod sample 1, when the rod sample 1 is stretched to generate an axial extension, the cover plate 2 is also lifted up along with the upper end of the rod sample 1, the outer corrugated tube 3 and the inner corrugated tube 4 are driven to be uniformly stretched at the moment, an interlayer space between the outer corrugated tube 3 and the inner corrugated tube 4 is also stretched and deformed along with the interlayer space, a solution is simultaneously communicated with the inside of the cylinder 6 through the connecting channel 10, the liquid level is consistent with the liquid level in the interlayer space, and the corrugated folds of the outer corrugated tube 3 and the inner corrugated tube 4 are stretched to be lengthened in the stretching and deforming process, so that the liquid level surface area of the interlayer space is reduced, which is equivalent to the liquid level surface area of a communicating vessel formed by the interlayer space and the cylinder 6 is reduced, the liquid level surface area is reduced to form a liquid level rising trend under the condition that the volume of the solution is unchanged, meanwhile, the liquid level is led to be stretched by the liquid level 1 and the liquid level is stretched out of the liquid level and the high level is kept under the condition that the high gradient of the electrolyte is set, the overall current is guaranteed, and the overall current is also stable, and the current is guaranteed, and the overall current is stable, and the parameter is guaranteed.
Further, the installation base 7 is provided with a groove, the bottom plate 6 is arranged in the groove, the middle part of the bottom plate 6 is provided with a first through hole, the middle part of the bottom plate 6 is provided with an installation groove, the bottom end of the rod sample 1 is provided with a lower fixing part, the lower fixing part penetrates through the first through hole to enter the installation groove, and the lower fixing part is detachably connected in the installation groove. The bottom of excellent sample 1 can be fixed to installation base 7 to be convenient for clamping equipment comes fixed connection installation base 7, thereby cooperates external stretching equipment to stretch excellent sample 1.
Further, the lower end of the mounting base 7 is provided with a clamping end 8, and the clamping end 8 is used for being clamped by external clamping equipment. The clamping end 8 enables the device to have higher compatibility with the rod sample 1, can use standard samples, does not need to specially customize the size of the samples, and has low requirements on the samples.
Further, the outer side wall of the lower fixing part is provided with a first external thread, the inner side wall of the mounting groove is provided with a first internal thread matched with the first external thread, and the lower fixing part is detachably connected with the mounting groove in a threaded connection mode. The threaded connection mode is more convenient for the installation and the disassembly of the rod sample 1.
Further, the method further comprises the following steps: the annular sealing plug 9, the annular sealing plug 9 is located between the lateral wall of lower fixed part and the inside wall of first through-hole. The annular sealing plug 9 can be inserted between the first through hole and the lower fixing portion for realizing sealing between the rod sample 1 and the first through hole, preventing the electrolyte from leaking to contact the mounting base 7.
Further, the annular sealing plug 9 is fixedly sleeved on the outer side of the lower fixing portion, a second external thread is arranged on the outer side wall of the annular sealing plug 9, a second internal thread matched with the second external thread is arranged on the inner side wall of the first through hole, and the annular sealing plug 9 is detachably connected in the first through hole of the bottom plate 6 in a threaded connection mode. Thereby facilitating the mounting and dismounting of the rod sample 1 and the annular sealing plug 9.
Further, the upper ends of the outer corrugated pipe 3 and the inner corrugated pipe 4 are detachably connected to the lower surface of the cover plate 2 in a buckling connection mode, so that the outer corrugated pipe 3 and the inner corrugated pipe 4 are convenient to detach and install.
Further, an upper fixing portion is connected to the upper end of the rod sample 1, and the upper fixing portion is detachably connected to the cover plate 2. The cover plate 2 is made of organic glass, so that the observation is convenient, and the cover plate can well splash the solution in the electrolytic cell.
Further, a second through hole is formed in the center portion of the cover plate 2, the upper fixing portion penetrates through the second through hole, a fastening nut 12 is connected to the outer side wall of the upper fixing portion in a threaded mode, the fastening nut 12 is located below the cover plate 2, and the fastening nut 12 is used for achieving detachable connection between the upper fixing portion and the cover plate 2. Thereby facilitating the installation and the disassembly of the upper fixing part and the cover plate 2
On the other hand, the invention also provides a hydrogen embrittlement sensitivity test method, which is suitable for the hydrogen embrittlement sensitivity test device of any one of the above, and comprises the following steps:
step 1, polishing the rod sample 1 to more than 1000 meshes, confirming a gauge length section and a connecting section connected with the bottom plate 6 and the cover plate 2 on the rod sample 1, and performing nickel plating or wax sealing treatment on the parts except the gauge length section and the connecting section.
Step 2, the sample is arranged between the cover plate 2 and the bottom plate 6, and is connected with the positive electrode of an external direct current power supply 15, the negative electrode of the external direct current power supply 15 is connected with an external platinum electrode 11, the lower end of the platinum electrode 11 also stretches into the electrolytic cell,
and 3, installing the inner corrugated pipe 4 and the outer corrugated pipe 3 between the cover plate 2 and the bottom plate 6.
Step 4, injecting electrolyte into the electrolytic cell, placing the rod sample 1 and the platinum electrode 11 into the electrolytic cell, enabling the electrolyte to permeate the gauge length section of the rod sample 1,
step 5, clamping and fixing the rod sample 1 by using an external lifting device and a clamping system, preparing to apply vertical up-down tensile load to the rod sample 1, and determining the charging current I according to the following formula:
I＝π×d×L×a，
where d is the diameter of the rod sample 1, L is the gauge length, and a is the charging current density as determined by the test requirements.
The external dc power supply 15 is started and the electrochemical charging operation is started.
And 6, after 2 minutes, observing whether the hydrogen charging operation is stable or not, and using an external lifting device and a clamping system to stretch the rod sample 1 to start a hydrogen embrittlement sensitivity test.
In one embodiment, the bar sample 1 of the standard piece polished step by step in 100#, 200#, 400#, 600#, 800#, 1000# is subjected to nickel plating treatment in a watt plating solution on the portions other than the gauge length section and the upper and lower fixing portions, and then the upper ends thereof are fixed in the second through hole and the electrode hole of the cover plate 2 together with the platinum electrode 11, respectively, and put into the electrolytic cell 5. The cover plate 2 is made of organic glass, so that the observation is convenient. The lower end of the rod specimen 1 is fitted with an annular sealing plug 9 of a suitable size according to the diameter outside the lower fixing portion and screwed to the specimen mount base 7 through the first through hole, and the first through hole in the center of the bottom plate 5 is sealed with the annular sealing plug 9.
The lower ends of the outer corrugated pipe 3 and the inner corrugated pipe 4 are arranged at the part of the bottom plate 5, which is positioned outside the cylinder 6, and the part is in the shape of an outer edge platform, so that the outer opening of the connecting channel 10 is ensured to be in an interlayer space between the outer corrugated pipe 3 and the inner corrugated pipe 4, 0.5% sodium hydroxide electrolyte is injected into the interlayer, and the electrolyte can enter the cylinder 6 until the standard distance section of the rod sample 1 is completely exceeded. The positive electrode of the dc power supply 15 was connected to the platinum electrode 11, and the negative electrode was connected to the rod sample 1.
In the test, the upper fixing part of the rod sample 1 penetrating out of the second through hole and the clamping end 8 of the mounting base 7 are connected with an external pulling-up device and a clamping system, so that the rod sample 1 can be stretched.
Setting the charging current and starting an external direct current power supply. After uniform and stable bubbles can be generated, parameters are input into an external pulling-up device, the pulling-up rate is set, the external pulling-up device is started, and a pulling-up curve is recorded. The bar sample 1 breaks and the test ends.
According to the invention, the liquid level of the electrolyte can be automatically regulated, so that the gauge length section of the rod sample 1 is immersed in the electrolyte in the whole course of the test, and the data accuracy is improved. The invention has simple structure and small size, can effectively prevent electrolyte from splashing, is suitable for laboratory use and operation, has convenient sample clamping and accurate experimental data, and can be compatible with standard samples and various clamp chucks.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A hydrogen embrittlement sensitivity test device, comprising:
the electrolytic cell, electrolytic cell upper portion opening, electrolytic cell includes bottom plate (6) and barrel (5), barrel (5) are located on bottom plate (6), the external diameter of bottom plate (6) is greater than barrel (5) external diameter, connecting channel (10) have been seted up to inside bottom plate (6), connecting channel (10)'s one end has first opening in bottom plate (6) upper surface, first opening is located the inside of barrel (5), connecting channel (10)'s the other end has the second opening in bottom plate (6) upper surface, the second opening is located the outside of barrel (5), the inside of barrel (5) is used for holding electrolyte, bottom plate (6) can connect the bottom of a stick sample (1) and stick sample (1) are located the inside of barrel (5).
The cover plate (2) is positioned above the cylinder (5), an air outlet is formed in the cover plate (2), and the cover plate (2) can be connected with the top of the rod sample (1);
the inner corrugated pipe (4) is arranged between the bottom plate (6) and the cover plate (2), and the cylinder (5) is sleeved inside the inner corrugated pipe (4);
the outer corrugated pipe (3), outer corrugated pipe (3) are located between bottom plate (6) and apron (2), interior ripple pipe (4) are overlapped in the inside of outer corrugated pipe (3), have the intermediate layer space between interior ripple pipe (4), outer corrugated pipe (3), the second opening is located between interior ripple pipe (4) and outer corrugated pipe (3), connecting channel (10) are linked together with the intermediate layer space, the gas outlet is linked together with the intermediate layer space.
2. The hydrogen embrittlement sensitivity test device according to claim 1, wherein the mounting base (7) is provided with a groove, the bottom plate (6) is arranged in the groove, a first through hole is formed in the middle of the bottom plate (6), a mounting groove is formed in the middle of the bottom plate (6), a lower fixing portion is arranged at the bottom end of the rod sample (1), the lower fixing portion penetrates through the first through hole to enter the mounting groove, and the lower fixing portion is detachably connected in the mounting groove.
3. A hydrogen embrittlement sensitivity test device according to claim 2, characterized in that the lower end of the mounting base (7) is provided with a clamping end (8), the clamping end (8) being adapted to be clamped by an external clamping device.
4. A hydrogen embrittlement sensitivity test device according to claim 3, wherein the outer side wall of the lower fixing portion is provided with a first external thread, the inner side wall of the mounting groove is provided with a first internal thread matched with the first external thread, and the lower fixing portion is detachably connected with the mounting groove in a threaded connection manner.
5. The hydrogen embrittlement sensitivity test device of claim 4, further comprising: the annular sealing plug (9) is arranged between the outer side wall of the lower fixing part and the inner side wall of the first through hole.
6. The hydrogen embrittlement sensitivity test device according to claim 5, wherein the annular sealing plug (9) is fixedly sleeved on the outer side of the lower fixing portion, a second external thread is arranged on the outer side wall of the annular sealing plug (9), a second internal thread matched with the second external thread is arranged on the inner side wall of the first through hole, and the annular sealing plug (9) is detachably connected in the first through hole of the bottom plate (6) in a threaded connection mode.
7. The hydrogen embrittlement sensitivity test device according to claim 6, wherein the upper ends of the outer bellows (3) and the inner bellows (4) are detachably connected to the lower surface of the cover plate (2) by means of snap connection.
8. A hydrogen embrittlement sensitivity test device according to claim 7, wherein the upper end of the rod specimen (1) is connected to an upper fixing portion detachably connected to the cover plate (2).
9. The hydrogen embrittlement sensitivity test device according to claim 8, wherein the central portion of the cover plate (2) is provided with a second through hole, the upper fixing portion passes through the second through hole, a fastening nut (12) is screwed on the outer side wall of the upper fixing portion, the fastening nut (12) is located below the cover plate (2), and the fastening nut (12) is used for realizing a detachable connection relationship between the upper fixing portion and the cover plate (2).
10. A hydrogen embrittlement susceptibility testing method, suitable for use in a hydrogen embrittlement susceptibility testing device according to any one of claims 1 to 9, comprising:
and 1, polishing the rod sample (1) to more than 1000 meshes, confirming a gauge length section and a connecting section connected with the bottom plate (6) and the cover plate (2) on the rod sample (1), and carrying out nickel plating or wax sealing treatment on the parts except the gauge length section and the connecting section.
Step 2, a sample is arranged between the cover plate (2) and the bottom plate (6) and is connected with the positive electrode of an external direct current power supply (15), the negative electrode of the external direct current power supply (15) is connected with an external platinum electrode (11), the lower end of the platinum electrode (11) also stretches into the electrolytic cell,
and 3, installing the inner corrugated pipe (4) and the outer corrugated pipe (3) between the cover plate (2) and the bottom plate (6).
Step 4, injecting electrolyte into the electrolytic cell, placing the rod sample (1) and the platinum electrode (11) into the electrolytic cell, enabling the electrolyte to permeate the gauge length section of the rod sample (1),
step 5, clamping and fixing the rod sample (1) by using an external lifting device and a clamping system, preparing to apply vertical up-and-down tensile load to the rod sample (1), and determining the charging current I according to the following formula:
I＝π×d×L×a，
where d is the diameter of the rod specimen (1), L is the gauge length, and a is the charging current density as determined by the test requirements.
An external DC power supply (15) is started to start electrochemical hydrogen charging operation.
And 6, after 2 minutes, observing whether the hydrogen charging operation is stable or not, and using an external lifting device and a clamping system to stretch the rod sample (1) to start a hydrogen embrittlement sensitivity test.
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| CN117723608A (en) * | 2024-02-07 | 2024-03-19 | 江苏龙城精锻集团有限公司 | Material hydrogen embrittlement detection device and method based on electrochemical hydrogen charging test |
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| CN117723608A (en) * | 2024-02-07 | 2024-03-19 | 江苏龙城精锻集团有限公司 | Material hydrogen embrittlement detection device and method based on electrochemical hydrogen charging test |
| CN117723608B (en) * | 2024-02-07 | 2024-05-10 | 江苏龙城精锻集团有限公司 | Material hydrogen embrittlement detection device and method based on electrochemical hydrogen charging test |
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