CN116046537A - Stress corrosion micro-area in-situ test device and method - Google Patents
Stress corrosion micro-area in-situ test device and method Download PDFInfo
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- CN116046537A CN116046537A CN202310104313.0A CN202310104313A CN116046537A CN 116046537 A CN116046537 A CN 116046537A CN 202310104313 A CN202310104313 A CN 202310104313A CN 116046537 A CN116046537 A CN 116046537A
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G—PHYSICS
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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Abstract
The invention discloses a stress corrosion micro-area in-situ test device and a method, wherein the test device comprises a stress ring test system, a micro-area scanning electrochemical system and a monitoring system; the micro-area scanning electrochemical system comprises a driving arm, a probe, an auxiliary electrode and a reference electrode, wherein the probe is arranged in a cavity body of the stress ring testing system and is connected with an L-shaped sleeve, and the driving arm is connected with the probe through the L-shaped sleeve and is used for controlling the probe to move relative to a sample to be tested; the auxiliary electrode and the reference electrode respectively penetrate through the upper cover so that one end of the auxiliary electrode and one end of the reference electrode are positioned in the cavity body; the monitoring system is used for monitoring the loading force of the stress ring and the fracture condition of the sample to be tested. The invention can synchronously carry out micro-region scanning electrochemical in-situ test during stress corrosion stretching, achieves the purpose of accurately researching micro-region stress corrosion of the simulated material in the loading process under the corrosive environment, and provides technical support for revealing the stress corrosion mechanism of the metal material in the service environment.
Description
Technical Field
The invention relates to the technical field of material testing, in particular to a stress corrosion micro-area in-situ testing device and method.
Background
In actual production operation, the metal material can generate stress corrosion cracking in the gas phase, liquid phase and gas-liquid multiphase corrosion environment containing corrosive gas, and even can cause casualties when serious, so that the damage is extremely high. In experimental research, in order to solve the stress corrosion cracking performance of metal materials, a uniaxial tension experiment is often adopted for stress corrosion test, and the method is simpler and is convenient to operate and is often adopted. However, the method cannot deeply study the corrosion mechanism of the metal material in the stress corrosion cracking process, and cannot provide technical support for revealing the stress corrosion mechanism of the metal material in the service environment.
Although the prior art discloses some stress corrosion experimental devices, the experimental devices cannot observe stress corrosion of a metal material micro-region, cannot perform in-situ real-time test of stress corrosion of a tensile sample micro-region, cannot clearly understand microscopic changes of stress corrosion of the tensile sample in the tensile process, and accordingly cannot clearly and deeply understand the stress corrosion mechanism of the metal material in the service environment.
Disclosure of Invention
In view of the above, the present invention aims to provide an in-situ testing device and method for stress corrosion micro-areas.
The technical scheme of the invention is as follows:
in one aspect, a stress corrosion micro-area in-situ testing device is provided, comprising a stress ring testing system, a micro-area scanning electrochemical system and a monitoring system;
the stress ring testing system comprises a stress ring and a corrosion medium cavity, wherein the corrosion medium cavity comprises a cavity body, and an upper cover and a lower cover which are detachably connected with the upper end and the lower end of the cavity body respectively; the corrosion medium cavity is provided with an air inlet and an air outlet which can be switched on and off; sample mounting holes are symmetrically formed in the centers of the upper cover and the lower cover, and when a sample to be tested is tested, the sample to be tested passes through the sample mounting holes and is respectively connected with the inner top and the inner bottom of the stress ring; the upper cover is provided with a through hole for installing the L-shaped sleeve, the L-shaped sleeve is arranged in the through hole, and one shorter end of the L-shaped sleeve is positioned in the cavity body;
the micro-area scanning electrochemical system comprises a driving arm, a probe, an auxiliary electrode and a reference electrode, wherein the probe is arranged in the cavity body and is connected with the L-shaped sleeve, and the driving arm is connected with the probe through the L-shaped sleeve and is used for controlling the probe to move relative to the sample to be detected; the auxiliary electrode and the reference electrode respectively penetrate through the upper cover so that one end of the auxiliary electrode and one end of the reference electrode are positioned in the cavity body;
the monitoring system is used for monitoring the loading force of the stress ring and the fracture condition of the sample to be tested.
Preferably, the upper and lower ends of the test sample are connected with the inner top and inner bottom of the stress ring through an upper sample fixing piece and a lower sample fixing piece respectively.
Preferably, the inner top and the inner bottom of the stress ring are respectively provided with a threaded column protruding towards the center of the stress ring, and the upper sample fixing piece and the lower sample fixing piece are respectively connected with the threaded columns at the upper end and the lower end of the stress ring in a threaded manner.
Preferably, a groove matched with the sample to be tested is formed in one end, connected with the sample to be tested, of the upper sample fixing piece and the lower sample fixing piece, and the sample to be tested is fixed through a bolt after being inserted into the groove.
Preferably, the lower cover is provided with a containing cavity, and a heating device is arranged in the containing cavity; the monitoring system further comprises a temperature monitoring device, and a detection end of the temperature monitoring device penetrates through the upper cover and stretches into the cavity body.
Preferably, the heating device is a heating rod; the temperature monitoring device is a thermometer.
Preferably, the monitoring system adopts a position finder to monitor the loading force of the stress ring, and adopts a fracture sensor to monitor the fracture condition of the sample to be tested.
Preferably, the air inlet is arranged at the lower part of the cavity body, and the air outlet is arranged on the upper cover.
Preferably, the upper cover and the lower cover are made of stainless steel, the cavity body is made of corrosion-resistant glass, and the L-shaped sleeve is made of polytetrafluoroethylene.
On the other hand, the in-situ test method of the stress corrosion micro-region is also provided, and the in-situ test device of the stress corrosion micro-region is adopted for testing.
The beneficial effects of the invention are as follows:
according to the invention, various different corrosive mediums (gas phase, liquid phase or gas/liquid multiphase) can be introduced into the corrosive medium cavity, so that the actual application working condition environment of the metal material under the coupling action of different corrosive environments and different loading loads is simulated; when the tensile test is carried out on the tensile sample under the simulated corrosion working condition environment, the real-time in-situ micro-area scanning test can be carried out on the sample gauge length section, namely the broken section, and the whole-process test records the micro-area current evolution process when the sample is subjected to stress corrosion, so that a more reliable scientific basis is provided for exploring the stress corrosion cracking reason of the material and revealing the stress corrosion mechanism.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a schematic diagram of an in-situ stress corrosion micro-area testing apparatus according to the present invention;
FIG. 2 is a schematic diagram of the structure of the corrosion medium cavity of the stress corrosion micro-area in-situ test device of the present invention.
In the figure: 1-supporting long rod, 2-movable connecting rod, 3-stressing nut, 4-stress ring, 5-base, 6-position finder, 7-fracture sensor, 8-upper sample fixing piece, 9-sample to be tested, 10-corrosion medium cavity, 10-1-upper cover, 10-2-cavity body, 10-3-lower cover, 11-lower sample fixing piece, 12-reference electrode, 13-temperature monitoring device, 14-auxiliary electrode, 15-driving arm, 16-probe, 17-holding cavity, 18-through hole, 19-connecting probe wire, 20-L-shaped sleeve, 21-air inlet and 22-air outlet.
Detailed Description
The invention will be further described with reference to the drawings and examples. It should be noted that, without conflict, the embodiments and technical features of the embodiments in the present application may be combined with each other. It is noted that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless otherwise indicated. The use of the terms "comprising" or "includes" and the like in this disclosure is intended to cover a member or article listed after that term and equivalents thereof without precluding other members or articles.
In one aspect, as shown in fig. 1-2, the present invention provides a stress corrosion micro-area in-situ test device, which comprises a stress ring test system, a micro-area scanning electrochemical system and a monitoring system;
the stress ring testing system comprises a stress ring 4 and a corrosion medium cavity 10, wherein the corrosion medium cavity 10 comprises a cavity body 10-2, and an upper cover 10-1 and a lower cover 10-3 which are detachably connected with the upper end and the lower end of the cavity body 10-2 respectively; the etching medium cavity 10 is provided with an air inlet 21 and an air outlet 22 which can be switched, optionally, the air inlet 21 is arranged at the lower part of the cavity body 10-2, and the air outlet 22 is arranged on the upper cover 10-1; sample mounting holes are symmetrically formed in the centers of the upper cover 10-1 and the lower cover 10-3, and when a sample 9 to be tested is tested, the sample 9 to be tested is respectively connected with the inner top and the inner bottom of the stress ring 4 through the sample mounting holes; the upper cover 10-1 is provided with a through hole 18 for installing an L-shaped sleeve 20, the L-shaped sleeve 20 is arranged in the through hole 18, and one shorter end of the L-shaped sleeve 20 is positioned in the cavity body 10-2; alternatively, the through hole 18 is provided in a tapered shape with the larger inner diameter end being on.
The micro-area scanning electrochemical system comprises a driving arm 15, a probe 16, an auxiliary electrode 14, a reference electrode 12 and a scanning electrochemical microscope control unit connected through a wire, wherein the probe 16 is arranged in the cavity body 10-2 and is connected with the L-shaped sleeve 20, and the driving arm 15 is connected with the probe 16 through the L-shaped sleeve 20 and is used for controlling the probe 16 to move relative to the sample 9 to be detected; the auxiliary electrode 14 and the reference electrode 12 respectively pass through the upper cover 10-1 so that one end of each of the auxiliary electrode and the reference electrode is positioned in the cavity body 10-2;
the monitoring system is used for monitoring the loading force of the stress ring 4 and the fracture condition of the to-be-tested sample 9.
It should be noted that, in the above embodiment, the probe 16 is connected to the driving arm through a connection probe wire 19, the auxiliary electrode 14 and the reference electrode 12 are also connected to the microscope control unit of the micro-area scanning electrochemical system through wires, and the micro-area electrochemical test is performed through the computer control system, so as to obtain the micro-area current information when the surface of the sample is subjected to stress electrochemical corrosion in the loaded stretching process. The principle of performing the micro-area electrochemical test by the micro-area scanning electrochemical system is the prior art, and is not described herein in detail.
In a specific embodiment, the monitoring system uses 6 to monitor the loading force of the stress ring 4 and uses a fracture sensor 7 to monitor the fracture of the test specimen 9. The position finder 6 can indirectly display the loading force, the test result is more accurate, the stability of loading parameters can be ensured, and the fracture sensor 7 can display the fracture time of the sample 9 to be tested, so that the working time of a tester can be greatly reduced, and the tensile state of the sample does not need to be concerned at any time. The above two monitoring devices are both in the prior art, and specific structures are not described herein.
In a specific embodiment, as shown in fig. 1, the stress ring testing system includes, in addition to the stress ring 4 and the corrosive medium cavity 10, a stress nut 3 for applying a force to the stress ring 4, a base 5 for supporting the stress ring 4, a support long rod 1 disposed on the base 5 and located on a side wall of the stress ring 4, and a movable connecting rod 2 disposed on the support long rod 1, where the position finder 6 and the fracture sensor 7 in the monitoring system are disposed on the movable connecting rod 2, and optionally, the movable connecting rod 2 moves up and down on the support long rod 1 by loosening a screw.
In a specific embodiment, the base 5 and the support long rod 1 are welded into a whole, and gaskets are arranged at four corners of the bottom of the base 5, so as to play a role in buffering and adjusting the horizontal plane. The support long rod 1 is positioned right behind the base 5, is vertically fixed on the base 5, is in the same plane with the central symmetry line of the stress ring 4, and is far greater than the radius of the corrosion medium cavity in distance, and is higher than the top of the stress ring.
In a specific embodiment, in order to ensure that the test specimen 9 is tested in a tensile manner on the central axis of the stress ring 4, the corrosive medium cavity 10 needs to be parallel to the platform of the base 5, and in order to ensure that the lower cover 10-3 is sealed and leak-proof, sealing rubber matched with the shape of the test specimen 9 is inlaid in the central position, the test specimen 9 is vertically symmetrical in the corrosive medium cavity, and sealing rubber matched with the shape of the test specimen 9 is inlaid in the center of the upper cover 10-1, so as to ensure that the test specimen 9 is tested in a tensile manner on the central axis.
It should be noted that, the stress ring testing system is in the prior art, and other stress ring testing systems in the prior art besides the stress ring testing system adopted in the embodiment may also be applied to the stress ring testing system disclosed in the prior art, such as CN203811126U, a stress ring deformation detecting device, CN216695824U, and the like.
In a specific embodiment, the upper and lower ends of the test specimen 9 are connected to the inner top and inner bottom of the stress ring 4 through upper and lower specimen holders 8 and 11, respectively. Optionally, the inner top and the inner bottom of the stress ring 4 are respectively provided with a threaded column protruding towards the center of the stress ring 4, and the upper sample fixing piece 8 and the lower sample fixing piece 11 are respectively connected with the threaded columns at the upper end and the lower end of the stress ring 4 in a threaded manner. Optionally, a groove matched with the sample 9 to be tested is formed in one end, connected with the sample 9 to be tested, of the upper sample fixing piece 8 and the lower sample fixing piece 11, and the sample 9 to be tested is fixed through a bolt after being inserted into the groove.
In order to test the corrosion mechanism of the corrosion medium to the material under different temperatures, in a specific embodiment, the lower cover 10-3 is provided with a containing cavity 17, and a heating device is arranged in the containing cavity 17; the monitoring system further comprises a temperature monitoring device 13, and a detection end of the temperature monitoring device 13 penetrates through the upper cover 10-1 and stretches into the cavity body 10-2. Optionally, the heating device is a heating rod; the temperature monitoring device is a thermometer. It should be noted that the above embodiment is only for providing the corrosive medium cavity with a heating function, and other related heating structure arrangements in the prior art may also be suitable for the present invention.
In a specific embodiment, the upper cover 10-1 and the lower cover 10-3 are made of stainless steel, the chamber body 10-2 is made of corrosion-resistant glass or transparent and durable polypropylene, and the L-shaped sleeve 20 is made of polytetrafluoroethylene. In this embodiment, the cavity body 10-2 is made of corrosion-resistant glass or transparent and durable polypropylene, which can make the corrosion process visible, so that an observer can observe the sample directly at any time.
On the other hand, the in-situ test method of the stress corrosion micro-region is also provided, and the in-situ test device of the stress corrosion micro-region is adopted for testing. In a specific embodiment, when the stress corrosion micro-area in-situ testing device is used for testing, the working principle is as follows:
firstly, the corrosive medium cavity 10 is disassembled, the sample 9 to be tested is inlaid and fixed on the lower cover 10-3 through sealing rubber, the sample 9 to be tested is connected with the lower sample fixing piece 11, the L-shaped sleeve 20 is installed by utilizing the through hole on the upper cover 10-1, the probe 16 is installed, the distance between the tip of the probe 16 and the sample 9 to be tested is adjusted, the probe is prevented from being damaged by bumping on the surface of the tensile sample when the upper cover 10-1 is installed, the final position of the probe 16 is adjusted under the software interface condition of the micro-scanning electrochemical system, the tip of the electronic probe 16 is positioned at the optimal position of the surface of the sample 9 to be tested, the sample 9 to be tested is fixed by utilizing the central through hole of the upper cover 10-1, the corrosive medium cavity 10 is installed into a whole body to be placed in the center of a stress ring by utilizing a screw and a nut, the upper sample fixing piece 8 and the sample 9 to be tested are connected, the corrosive medium cavity 10 is screwed and fixed on the central axis of the stress ring through the upper sample fixing piece 8 and the lower sample fixing piece 11, the position of the position finder 6 is adjusted, the displacement count is 0 at the moment, the stress nut 3 is loosened, the stress ring 4 is restored to deform, a constant load force is applied to the sample 9 to be tested, the reading size of the position finder 6 is converted into the load force through consulting relevant standards, the test force size is set through adjusting the stress nut 3, the position of the fracture sensor 7 is adjusted, a stress ring test system is utilized for switching, after the whole device is installed, corrosive liquid is added, if heating is needed, a heating rod is inserted into the accommodating cavity 17, if the gas environment is needed to be tested, the gas outlet 22 is closed, the gas inlet 21 is opened, then the stress corrosion test system is utilized for starting a stress corrosion test by inserting the reference electrode 12, the thermometer 13 and the auxiliary electrode 14 into the corrosive medium cavity 10, and meanwhile, the relevant temperature parameters are well regulated, in the whole testing process, the testing position of the probe 16 can be regulated by a microscope control unit of the micro-area scanning electrochemical system to carry out micro-area scanning electrochemical testing, the current change morphology trend of the stress corrosion micro-area of the sample under the action of multiple environments is measured, the microscopic change of the stress corrosion of the sample is synchronously observed in real time, and the stress corrosion mechanism is further revealed.
In summary, the invention is based on the existing stress ring test system, and the micro-area scanning electrochemical system is arranged to test the micro-area current evolution process when the sample is subjected to stress corrosion, so as to explore the cause of stress corrosion cracking of the material and reveal the stress corrosion mechanism. Compared with the prior art, the method has obvious progress.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalents and modifications can be made to the above-mentioned embodiments without departing from the scope of the invention.
Claims (10)
1. The in-situ stress corrosion micro-area testing device is characterized by comprising a stress ring testing system, a micro-area scanning electrochemical system and a monitoring system;
the stress ring testing system comprises a stress ring and a corrosion medium cavity, wherein the corrosion medium cavity comprises a cavity body, and an upper cover and a lower cover which are detachably connected with the upper end and the lower end of the cavity body respectively; the corrosion medium cavity is provided with an air inlet and an air outlet which can be switched on and off; sample mounting holes are symmetrically formed in the centers of the upper cover and the lower cover, and when a sample to be tested is tested, the sample to be tested passes through the sample mounting holes and is respectively connected with the inner top and the inner bottom of the stress ring; the upper cover is provided with a through hole for installing the L-shaped sleeve, the L-shaped sleeve is arranged in the through hole, and one shorter end of the L-shaped sleeve is positioned in the cavity body;
the micro-area scanning electrochemical system comprises a driving arm, a probe, an auxiliary electrode and a reference electrode, wherein the probe is arranged in the cavity body and is connected with the L-shaped sleeve, and the driving arm is connected with the probe through the L-shaped sleeve and is used for controlling the probe to move relative to the sample to be detected; the auxiliary electrode and the reference electrode respectively penetrate through the upper cover so that one end of the auxiliary electrode and one end of the reference electrode are positioned in the cavity body;
the monitoring system is used for monitoring the loading force of the stress ring and the fracture condition of the sample to be tested.
2. The stress corrosion micro-area in-situ test device according to claim 1, wherein the upper and lower ends of the test specimen are connected to the inner top and inner bottom of the stress ring by upper and lower specimen holders, respectively.
3. The stress corrosion micro-area in-situ test device according to claim 2, wherein the inner top and the inner bottom of the stress ring are respectively provided with a threaded column protruding towards the center of the stress ring, and the upper sample fixing piece and the lower sample fixing piece are respectively connected with the threaded columns at the upper end and the lower end of the stress ring in a threaded manner.
4. The stress corrosion micro-area in-situ test device according to claim 3, wherein a groove matched with the test sample is formed in one end, connected with the test sample, of the upper test sample fixing piece and the lower test sample fixing piece, and the test sample is fixed through a bolt after being inserted into the groove.
5. The stress corrosion micro-area in-situ test device according to claim 1, wherein the lower cover is provided with a containing cavity, and a heating device is arranged in the containing cavity; the monitoring system further comprises a temperature monitoring device, and a detection end of the temperature monitoring device penetrates through the upper cover and stretches into the cavity body.
6. The stress corrosion micro-area in-situ test device of claim 5, wherein the heating device is a heating rod; the temperature monitoring device is a thermometer.
7. The stress corrosion micro-area in-situ test device according to claim 1, wherein the monitoring system monitors the loading force of the stress ring by using a position finder and monitors the fracture condition of the test sample by using a fracture sensor.
8. The stress corrosion micro-area in-situ test device according to claim 1, wherein the air inlet is arranged at the lower part of the cavity body, and the air outlet is arranged on the upper cover.
9. The stress corrosion micro-area in-situ test device according to any one of claims 1 to 8, wherein the upper cover and the lower cover are made of stainless steel, the cavity body is made of corrosion-resistant glass, and the L-shaped sleeve is made of polytetrafluoroethylene.
10. An in-situ test method for stress corrosion micro-areas, which is characterized in that the in-situ test device for stress corrosion micro-areas is adopted for testing according to any one of claims 1-9.
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| CN202310104313.0A CN116046537A (en) | 2023-02-13 | 2023-02-13 | Stress corrosion micro-area in-situ test device and method |
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| CN202310104313.0A CN116046537A (en) | 2023-02-13 | 2023-02-13 | Stress corrosion micro-area in-situ test device and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116539512A (en) * | 2023-05-12 | 2023-08-04 | 北京科技大学 | Stress corrosion simulation experiment equipment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116539512A (en) * | 2023-05-12 | 2023-08-04 | 北京科技大学 | Stress corrosion simulation experiment equipment |
| CN116539512B (en) * | 2023-05-12 | 2023-12-22 | 北京科技大学 | Stress corrosion simulation experiment equipment |
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