Device for in-situ testing of micro-area electrochemical performance of sample under hydrostatic pressure

Abstract

The application discloses a device for in-situ testing of micro-area electrochemical performance of a sample under hydrostatic pressure, comprising: a high-pressure cavity unit, comprising a shell and a high-pressure cavity formed by the shell, the high-pressure cavity being used for at least a sample to be tested; an electrochemical detection unit, used for at least electrochemical measurement on a selected area of the sample to be tested; a sample transmission unit, in transmission cooperation with the sample to be tested, and used for at least driving the sample to be tested to move in the high-pressure cavity, so that the selected area of the sample to be tested corresponds to a probe of the electrochemical detection unit; and a hydrostatic pressure environment unit, used for at least injecting liquid into the high-pressure cavity, so as to form a hydrostatic pressure environment in the high-pressure cavity. The application solves the difficulty that current scanning microelectrochemical testing devices cannot be used for testing under hydrostatic pressure, and realizes scanning microelectrochemical testing under hydrostatic pressure.

Description

Technical Field

[0001] This invention specifically relates to a device for in-situ testing of the micro-region electrochemical performance of a sample under hydrostatic pressure, belonging to the field of electrochemical testing technology. Background Technology

[0002] Micro-area electrochemistry is a technique for testing the electrochemical properties of microscopic regions on a material surface, such as corrosion potential and impedance. Scanning microscopy (SMS) electrochemical measurement devices achieve micro-area measurements by applying electrical perturbations to localized micro-areas of the electrode surface and monitoring changes or by passively acquiring signals. Micro-area electrochemical devices can be used to test localized electrochemical data, such as determining the extent of localized corrosion and predicting corrosion rates, providing technical support for materials performance research. Micro-area electrochemical measurements are increasingly widely used in corrosion science, materials science and engineering, and surface and interface physics and chemistry. Traditional electrochemical measurement devices test the overall electrochemical properties of the electrode surface but cannot perform electrochemical tests on minute localized areas with varying morphology, composition, and structure. Scanning microscopy electrochemical measurement enables this, facilitating more microscopic research into materials.

[0003] However, current micro-area electrochemical measurements place high demands on samples and equipment, especially on micro-probes. Even measurements under normal pressure require precise calibration and demand high-quality sample surfaces. Typically, signals are acquired by scanning the sample surface with the micro-probe. Therefore, micro-area electrochemical measurements under high water pressure place even greater demands on sample size and conductivity, limiting the application and development of micro-area electrochemistry under complex and harsh hydrostatic pressures. In recent years, with the increasing activity in deep-sea environments, new requirements have been placed on the service performance of materials in the deep sea. There is an urgent need to study the microscopic electrochemical mechanisms of materials simulating deep-sea conditions to ensure the reliability of key deep-sea materials. However, the high-pressure chambers used to simulate deep-sea environments limit the development of micro-area electrochemistry, particularly the movement limitations of the probe within the high-pressure chamber. This invention achieves micro-area electrochemical measurements under high pressure, using scanning electrochemical testing to determine the local electrochemical properties of materials under high hydrostatic pressure in the deep sea, providing a new path for mechanism research and predictive evaluation of key deep-sea equipment structures. Summary of the Invention

[0004] The main objective of this invention is to provide a device for in-situ testing of the micro-region electrochemical performance of a sample under hydrostatic pressure, thereby overcoming the shortcomings of the prior art.

[0005] To achieve the aforementioned objectives, the technical solution adopted by this invention includes:

[0006] This invention provides an apparatus for in-situ testing of the micro-region electrochemical performance of a sample under hydrostatic pressure, comprising:

[0007] A high-pressure chamber unit includes a housing and a high-pressure chamber enclosed by the housing, the high-pressure chamber being used at least for the sample to be tested;

[0008] An electrochemical detection unit is used to perform electrochemical measurements on at least a selected area of ​​the sample to be tested;

[0009] A sample delivery unit, which is driven in conjunction with the sample to be tested, and is at least used to drive the sample to be tested to move within the high-pressure chamber so that a selected area of ​​the sample to be tested corresponds to the probe of the electrochemical detection unit;

[0010] A hydrostatic pressure environment unit is used at least to inject liquid into the high-pressure chamber to create a hydrostatic pressure environment within the high-pressure chamber.

[0011] Compared with the prior art, the present invention provides a device for accurately measuring the scanning micro-area electrochemistry of a sample under simulated deep-sea hydrostatic pressure. It has a simple structure, is easy to use and maintain, and solves the difficulty that current scanning micro-electrochemical testing devices cannot perform tests under hydrostatic pressure. It realizes scanning micro-electrochemical testing under hydrostatic pressure, and in particular, realizes the working mode of the probe collecting rotating sample signals in a high-pressure chamber. Attached Figure Description

[0012] Figure 1 This is a schematic diagram of a device for in-situ testing of the micro-region electrochemical performance of a sample under hydrostatic pressure, provided in a typical embodiment of the present invention.

[0013] Figure 2 This is a schematic diagram of the structure of the electrochemical detection unit in a typical embodiment of the present invention, showing the electrode, probe, and sample under test in combination. Detailed Implementation

[0014] In view of the shortcomings of the prior art, the inventors of this invention, through long-term research and extensive practice, have proposed the technical solution of this invention. The following will further explain and illustrate the technical solution, its implementation process, and its principles.

[0015] This invention provides an apparatus for in-situ testing of the micro-region electrochemical performance of a sample under hydrostatic pressure, comprising:

[0016] A high-pressure chamber unit includes an outer shell and a high-pressure chamber enclosed by the outer shell, the high-pressure chamber being used at least to contain the sample to be tested and to provide the closed environment required for electrochemical measurements;

[0017] An electrochemical detection unit is used to perform electrochemical measurements on at least a selected area of ​​the sample to be tested;

[0018] A sample delivery unit, which is driven in conjunction with the sample to be tested, and is at least used to drive the sample to be tested to move within the high-pressure chamber so that a selected area of ​​the sample to be tested corresponds to the probe of the electrochemical detection unit;

[0019] A hydrostatic pressure environment unit is used at least to inject liquid into the high-pressure chamber to create a hydrostatic pressure environment within the high-pressure chamber.

[0020] In some specific implementation cases, the electrochemical detection unit includes an electrochemical workstation and an auxiliary electrode, a probe, and a reference electrode. The auxiliary electrode, probe, and reference electrode are disposed in the high-voltage chamber. The electrochemical workstation is electrically connected to the auxiliary electrode, probe, and reference electrode respectively, and the tip of the probe faces the sample to be tested.

[0021] In some specific implementation cases, the housing is provided with a first sealing connector, a second sealing connector and a third sealing connector, which are sealed to the housing. The auxiliary electrode, probe and reference electrode are electrically connected to the electrochemical workstation via the first sealing connector, the second sealing connector and the third sealing connector, respectively.

[0022] In some specific implementation cases, the probe is also connected to a needle insertion drive mechanism, which is at least used to drive the probe to move in a selected direction to change the distance between the tip of the probe and the sample to be tested. The selected direction is the direction in which the probe points to the sample to be tested.

[0023] In some specific implementation cases, the needle insertion transmission mechanism includes a coarse adjustment knob and a fine adjustment knob located outside the high-pressure chamber, and a push rod partially located inside the high-pressure chamber. The coarse adjustment knob and the fine adjustment knob are connected to the probe via the push rod. By turning either the coarse adjustment knob or the fine adjustment knob, the probe can be moved along the selected direction.

[0024] In some specific implementations, the needle insertion transmission mechanism further includes a micro-displacement brake, which is connected to the probe and is used to drive the probe to move and / or vibrate along the selected direction; for example, the micro-displacement brake can be directly on the probe, and the micro-displacement brake can be a miniature piezoelectric ceramic, etc.

[0025] In some specific implementation cases, an observation window is also provided on the outer shell.

[0026] In some specific implementation cases, the housing is also equipped with a lighting mechanism.

[0027] In some specific implementation cases, the lighting mechanism is located at the observation window.

[0028] In some specific implementation cases, the outer shell is also equipped with a rupture disc.

[0029] In some specific implementations, the sample transfer unit includes a drive mechanism and a sample rod. A portion of the sample rod is disposed inside the high-pressure chamber and sealed to the outer shell, and is used at least to carry the sample to be tested. The drive mechanism is driven to drive the sample rod and is used at least to drive the sample rod to move linearly along its own axis and / or rotate about its own axis.

[0030] In some specific implementation cases, the sample rod is an insulating component, and an electrical connection wire is provided inside the sample rod. The electrical connection wire is electrically connected to the electrochemical workstation, and the electrical connection wire can also be electrically connected to the sample to be tested placed on the sample rod.

[0031] In some specific implementations, the sample rod penetrates the high-pressure chamber.

[0032] In some specific implementation cases, the housing is also provided with a fourth sealing connector and a fifth sealing connector, which are sealed to the housing, and the electrical connection line is electrically connected to the electrochemical workstation via the fourth sealing connector and the fifth sealing connector.

[0033] In some specific implementation cases, the sample rod is sealed to the housing via the fourth sealing connector and the fifth sealing connector.

[0034] In some specific implementations, the sample transfer unit further includes a control mechanism, which is electrically connected to the drive mechanism.

[0035] In some specific implementation examples, the device further includes: a sample spiral shaft and a sample stage transmission device, which are disposed outside the high-pressure chamber. The drive mechanism is connected to the sample stage transmission device, and the sample stage transmission device is connected to the sample spiral shaft. The sample spiral shaft is fixedly connected to the sample rod. The sample spiral shaft is capable of rotating around its own axis and moving linearly along its own axial direction.

[0036] In some specific implementation examples, the hydrostatic pressure environment unit includes a liquid circulation supply mechanism, which comprises a pump body and a sealed water tank. The pump body is connected to the sealed water tank and is also connected to the outer casing via a first pressure-resistant pipeline and a second pressure-resistant pipeline, thereby forming a circulation loop for liquid circulation between the sealed water tank, the first pressure-resistant pipeline, the second pressure-resistant pipeline, and the high-pressure chamber.

[0037] In addition, the first pressure-resistant pipeline is also equipped with a shut-off valve and a pressure gauge for increasing pressure, and the second pressure-resistant pipeline is also equipped with a pressure relief valve and a pressure relief gauge for decreasing pressure.

[0038] In some specific implementation cases, the hydrostatic pressure environment unit further includes a circulating gas supply mechanism, which includes a gas storage container and a gas processing mechanism. The gas storage container is connected to a sealed water tank via a gas guide pipe, and the gas processing mechanism is connected to the sealed water tank via an exhaust pipe.

[0039] In some specific implementation cases, a flow meter is also installed on the air delivery pipe.

[0040] The following will further explain the technical solution, its implementation process and principle in conjunction with the accompanying drawings and specific implementation examples. Unless otherwise specified, the electrochemical workstation, probe, three-electrode system, sealing connector, rupture disc, drive mechanism, controller, pressure gauge, pressure relief valve, pump and other components used in the embodiments of the present invention are all known to those skilled in the art and can be obtained commercially. Their specific structures and product models are not limited here.

[0041] Example

[0042] Please see Figure 1 and Figure 2 A device for in-situ testing of the electrochemical performance of a sample micro-region under hydrostatic pressure, comprising a high-pressure chamber unit, an electrochemical detection unit, a sample transfer unit, and a hydrostatic pressure environment unit.

[0043] The high-pressure chamber unit includes a housing 21 and a high-pressure chamber enclosed by the housing 21. The high-pressure chamber is at least used to contain the sample 24 to be tested and to provide a sealed environment required for electrochemical measurement. The electrochemical detection unit is at least used to perform electrochemical measurement on a selected area of ​​the sample 24 to be tested. The sample transfer unit is driven in conjunction with the sample to be tested and is at least used to drive the sample 24 to be tested within the high-pressure chamber so that the selected area of ​​the sample 24 to be tested corresponds to the probe 27 of the electrochemical detection unit. The hydrostatic pressure environment unit is at least used to inject liquid into the high-pressure chamber to form a hydrostatic pressure environment within the high-pressure chamber.

[0044] In this embodiment, the electrochemical detection unit includes an electrochemical workstation 20, an auxiliary electrode 23, a probe 27, and a reference electrode 28. The auxiliary electrode 23, the probe 27, and the reference electrode 28 are disposed in the high-voltage chamber. The electrochemical workstation 20 is electrically connected to the auxiliary electrode 23, the probe 27, and the reference electrode 28, respectively. The tip of the probe 27 faces the sample 24 to be tested.

[0045] In this embodiment, the working electrode of the electrochemical workstation is connected to a sleeve and a probe signal is acquired. The electrochemical workstation adopts a three-electrode system measurement connection method, and the reference electrode and the auxiliary electrode are connected through a sealed connector. The electrochemical workstation can be set to scanning vibration electrode mode, local electrochemical impedance spectroscopy mode and scanning electrochemical microscope mode.

[0046] In this embodiment, the outer shell 21 is mainly made of hydrostatic pressure resistant material, and the high-pressure chamber can hold a certain volume of liquid.

[0047] In this embodiment, the outer casing 21 is provided with a first sealing connector 3, a second sealing connector 29, and a third sealing connector 32. The first sealing connector 3, the second sealing connector 29, and the third sealing connector 32 are sealed and fitted with the outer casing 21. The auxiliary electrode 23, the probe 27, and the reference electrode 28 are electrically connected to the first sealing connector 3, the second sealing connector 29, and the third sealing connector 32, respectively. The first sealing connector 3, the second sealing connector 29, and the third sealing connector 32 are electrically connected to the electrochemical workstation 20.

[0048] In this embodiment, the auxiliary electrode 23 can be a platinum mesh electrode, etc., and the reference electrode 28 can be an Ag / AgCl high-pressure reference electrode, etc. The first sealing connector 3, the second sealing connector 29, and the third sealing connector 32 can be obtained directly from commercial sources or assembled from commercially available accessories. The specific product models are not limited here. Furthermore, the first sealing connector 3, the second sealing connector 29, and the third sealing connector 32 all include the same built-in sealing gasket 6. The sealing gasket 6 is mainly used to simultaneously realize the connection of the first sealing connector 3, the second sealing connector 29, and the third sealing connector 32 with the auxiliary electrode 23, the probe 27, and the reference electrode 28, as well as the sealing of the high-pressure chamber.

[0049] For example, the sealing connector can be a ferrule fitting with a threaded straight-through or a spring sealing ring fitting with a threaded straight-through, connected to the cavity through a sealing gasket, thereby achieving the sealing function.

[0050] In this embodiment, the outer shell 21 is further provided with a needle insertion drive mechanism. The needle insertion drive mechanism and the probe 27 are combined to form a scanning microelectrochemical probe system 4. The needle insertion drive mechanism is connected to the probe 27 and is at least used to drive the probe 27 to move in a selected direction to change the distance between the tip of the probe 27 and the sample 24 to be tested. The selected direction is the direction in which the probe 27 points to the sample 24 to be tested.

[0051] In this embodiment, the needle insertion transmission mechanism is located outside the high-pressure chamber and correspondingly located at the second sealing connector 29. The needle insertion transmission mechanism includes a coarse adjustment knob 31 and a fine adjustment knob 30 located outside the high-pressure chamber, and a push rod partially located inside the high-pressure chamber. The push rod is fixedly connected to the probe, and a helical groove is fixedly provided on the push rod. The helical groove is drivenly connected to a helical stator, and the helical stator is connected to the coarse adjustment knob 31 and the fine adjustment knob 30. By turning either the coarse adjustment knob 31 or the fine adjustment knob 30, the push rod and the probe 27 can move together in the selected direction. At the same time, the probe 27 is also electrically connected to the electrochemical workstation through the second sealing connector 29. The structure of the needle insertion transmission mechanism can be referred to as that of a micrometer.

[0052] In this embodiment, a micro piezoelectric ceramic 38 (i.e., a micro-displacement actuator) is also provided in the high-pressure chamber. The micro piezoelectric ceramic 38 is fixedly mounted on the push rod or probe, and the micro piezoelectric ceramic can be controlled by voltage to realize the micro vibration of the sample rod and the probe in the high-pressure chamber, thereby enabling the scanning vibration electrochemical mode to be realized.

[0053] Specifically, the structures of the first, second, and third sealing connectors are all the same. The water seal includes a hollow conduit, a wire located inside the conduit, a sealing filler inside the conduit, and a spring sealing ring sleeved on the outside of the conduit. The wire is located inside the conduit and can be connected to the electrical connection mechanism inside and outside the high-pressure chamber. The sealing filler can achieve sealing inside the conduit. The spring sealing ring is located between the conduit and the outer shell 21 and achieves sealed communication between the conduit and the outer shell 21.

[0054] Specifically, the push rod is disposed inside the catheter. While maintaining a sealed fit with the catheter, the push rod also moves in a movable fit with the catheter. Specifically, the push rod can rotate relative to the catheter about its own axis and move along its own axis. For example, the push rod can fit with the catheter through a sealing ring or the like.

[0055] In this embodiment, the outer shell 21 is also provided with an observation window 5, through which the relative position and distance between the probe 27 and the sample 24 can be observed. The observation window 5 can be a transparent observation window such as quartz.

[0056] In this embodiment, the outer casing 21 is also provided with an illumination mechanism, which is located at the observation window 5. The illumination mechanism is used to illuminate the high-pressure chamber so that the internal environment of the high-pressure chamber (mainly the relative position and distance between the probe 27 and the sample 24) can be observed through the observation window 5. The illumination mechanism can be an LED light or the like.

[0057] In this embodiment, the outer casing 21 is also provided with a rupture disc 7. The rupture disc 7 serves as a protective device and is mainly used to prevent excessive pressure in the high-pressure chamber from causing a safety accident. The rupture disc 7 can be obtained commercially. The connection structure and connection method between the rupture disc 7 and the outer casing 2 can also be implemented using structures and methods known to those skilled in the art, and no specific limitations are made here.

[0058] In this embodiment, the sample transfer unit includes a drive mechanism 1 and a sample rod 2. A portion of the sample rod 2 is disposed inside the high-pressure chamber and sealed to the outer shell 21, and is at least used to carry the sample to be tested 24. The drive mechanism 1 is driven to drive the sample rod 2 to move linearly along its own axis and / or rotate about its own axis, thereby changing the position of the sample to be tested 24 in the high-pressure chamber so that different areas of the sample to be tested 24 correspond to the probe 27, thereby enabling the probe to detect the micro-area signals of different areas of the sample to be tested 24. Specifically, when detecting signals, the probe is opposite to the sample to be tested located on the sample rod 2. The drive mechanism 1 drives the sample rod 2 to rotate so that the sample to be tested and the sample rod move back and forth and rotate together, while the helical shaft of the probe remains stationary, thereby enabling the probe to detect the micro-area signals of different areas of the sample to be tested.

[0059] In this embodiment, the sample rod 2 is a hollow insulating component. An electrical connection wire 26 is provided inside the sample rod 2. The electrical connection wire 26 is electrically connected to the electrochemical workstation 20, and the electrical connection wire 26 can also be electrically connected to the sample 24 to be tested, which is placed on the sample rod 2.

[0060] In this embodiment, the sample rod 2 is a hollow, insulated sample rod, and the electrical connection line 26 is disposed inside the hollow structure of the sample rod 2. One end of the electrical connection line 26 is electrically connected to the electrochemical workstation 20, and the other end is electrically connected to the sample to be tested, so as to collect the working electrode signal. In this embodiment, the interior of the sample rod 2 can be filled with insulating materials such as insulating resin.

[0061] In this embodiment, the sample rod 2 extends through both ends of the high-pressure chamber, that is, the two ends of the sample rod 2 are located outside the high-pressure chamber, and the middle part is located inside the high-pressure chamber. The sample rod 2 is movably fitted and sealed with the outer shell 21. The first sealing connector 3, the second sealing connector 29, and the third sealing connector 32 are located on the side of the sample rod 2. The sample rod 2 can achieve a movable fit and sealing structure with the outer shell 21 through a threaded connection.

[0062] In this embodiment, the sample to be tested 24 may be a cylindrical or similar structure, and the sample to be tested 24 may extend through the sample rod 2.

[0063] In this embodiment, the outer casing 21 is further provided with a fourth sealing connector 34 and a fifth sealing connector 35. The fourth sealing connector 34 and the fifth sealing connector 35 are sealed and fitted with the outer casing 21. The electrical connection line 26 is electrically connected to the electrochemical workstation 20 via the fourth sealing connector 34 and the fifth sealing connector 35.

[0064] In this embodiment, the sample rod 2 is sealed to the outer shell 21 via the fourth sealing connector 34 and the fifth sealing connector 35.

[0065] In this embodiment, the device further includes a sample spiral shaft 36 and a sample stage transmission device 37. The sample spiral shaft 36 and the sample stage transmission device 37 are disposed outside the high-pressure chamber. The drive mechanism 1 is connected to the sample stage transmission device 37, and the sample stage transmission device 37 is connected to the sample spiral shaft 36. The sample spiral shaft 36 is fixedly connected to the sample rod 2. The sample spiral shaft 36 can rotate around its own axis and move linearly along its own axial direction.

[0066] In this embodiment, the sample transfer unit further includes a control mechanism 22, which is electrically connected to the drive mechanism 1. The drive mechanism 1 can be a rotary drive motor, which drives the sample rod 2 to rotate. Due to the threaded connection structure between the sample rod 2 and the outer shell, the rotational motion of the sample rod 2 can be converted into linear motion of the sample rod 2 along its own axis, thereby realizing the linear motion drive and rotational motion drive of the sample to be tested. The control mechanism 22 is used to control the rotational speed and working state of the drive mechanism 1, and thereby adjust the rotational speed and position of the sample to be tested. For example, the control mechanism 22 can be a PLC controller, etc. The control mechanism 22 and the control software it uses can be obtained commercially.

[0067] In this embodiment, the electrochemical workstation 20 is connected to the reference electrode 28, the auxiliary electrode 23, the probe 27, and the sample to be tested 24. The working modes of the electrochemical workstation are scanning vibration electrode mode, local electrochemical impedance spectroscopy mode, and scanning electrochemical microscope mode. After connecting the circuit and adjusting the probe to the test distance, the position of the sample to be tested is changed by the drive mechanism, thereby realizing the probe to detect the micro-area signal of different regions of the sample to be tested.

[0068] In this embodiment, the hydrostatic pressure environment unit includes a liquid circulation supply mechanism, which comprises a pump body 11 and a sealed water tank 12. The pump body 11 is connected to the sealed water tank 12, and the pump body 11 is also connected to the outer casing 21 via a first pressure-resistant pipe 8 and a second pressure-resistant pipe 19, thereby forming a circulation loop for liquid circulation between the sealed water tank 12, the first pressure-resistant pipe 8, the second pressure-resistant pipe 19, and the high-pressure chamber.

[0069] Furthermore, the first pressure-resistant pipeline 8 is also equipped with a shut-off valve 9 and a pressure boosting gauge 10, and the second pressure-resistant pipeline 19 is also equipped with a pressure relief valve 33 and a pressure relief gauge 18. The pressure regulation of the high-pressure chamber environment can be achieved through the pump body 11, the pressure relief valve 33, the pressure relief gauge 18, the shut-off valve 9 and the pressure boosting gauge 10.

[0070] In this embodiment, the hydrostatic pressure environment unit further includes a circulating gas supply mechanism, which is at least used to inject gas into the liquid in the sealed water tank 12 to adjust the amount of gas dissolved in the liquid in the sealed water tank 12 and the environmental pressure in the high-pressure chamber.

[0071] In this embodiment, the circulating gas supply mechanism includes a gas storage container 15 and a gas processing mechanism 17. The gas storage container 15 is connected to a sealed water tank 12 via a gas guide pipe 14, and the gas processing mechanism 17 is connected to the sealed water tank 12 via an exhaust pipe 16. A flow meter 13 is also provided on the gas guide pipe 14. Specifically, the gas in the gas storage container 15 is fed into the liquid in the sealed water tank 12 through the gas guide pipe 14 connected to the flow meter 13. The flow rate of the gas can be controlled by controlling the flow meter 13, and the amount of gas dissolved in the solution can be controlled by controlling the ventilation time and flow rate. Undissolved gas can be discharged into the gas processing mechanism 17 through the exhaust pipe 16. It should be noted that the gas storage container 15 can be a gas storage bottle, and the gas processing mechanism 17 can be a gas processing pool, etc. The process methods and reagents used by the gas processing mechanism to process the gas are all known to those skilled in the art and are not limited here. The gas can be a common gas known to those skilled in the art and is not specifically limited here.

[0072] The present invention provides a device for accurately measuring the scanning micro-area electrochemistry of a sample under simulated deep-sea hydrostatic pressure. The device has a simple structure and is easy to use and maintain. It solves the problem that current scanning micro-electrochemical testing devices cannot perform tests under hydrostatic pressure, and thus realizes scanning micro-electrochemical testing under hydrostatic pressure. In particular, it realizes the working mode of the probe collecting rotating sample signals in a high-pressure chamber.

[0073] It should be understood that the above embodiments are merely illustrative of the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement it accordingly. They should not be construed as limiting the scope of protection of the present invention. All equivalent changes or modifications made in accordance with the spirit and essence of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A device for testing the electrochemical properties of a micro-area of a sample in situ under hydrostatic pressure, characterized in that, include: The high-pressure chamber unit includes a housing (21) and a high-pressure chamber enclosed by the housing (21), the high-pressure chamber being used at least to contain the sample to be tested (24) and to provide a closed environment required for electrochemical measurements; An electrochemical detection unit is used at least for electrochemical measurement of a selected area of ​​the sample to be tested (24). The electrochemical detection unit includes an electrochemical workstation (20), an auxiliary electrode (23), a probe (27), and a reference electrode (28). The auxiliary electrode (23), the probe (27), and the reference electrode (28) are disposed in the high-voltage chamber. The electrochemical workstation (20) is electrically connected to the auxiliary electrode (23), the probe (27), and the reference electrode (28), respectively. The tip of the probe (27) faces the sample to be tested (24). The probe (27) is also connected to a needle insertion drive mechanism. The needle insertion drive mechanism is used at least to drive the probe (27) to move in a selected direction to change the distance between the tip of the probe (27) and the sample to be tested (24). The selected direction is the direction in which the probe (27) points to the sample to be tested (24). The sample transfer unit is used at least to fix the sample to be tested (24) and drive the sample to be tested (24) to move within the high-pressure chamber so that a selected area of ​​the sample to be tested (24) corresponds to the probe (27) of the electrochemical detection unit. A hydrostatic pressure environment unit is used at least to inject liquid into the high-pressure chamber to form a hydrostatic pressure environment in the high-pressure chamber. The hydrostatic pressure environment unit includes a liquid circulation supply mechanism and a circulating gas supply mechanism. The liquid circulation supply mechanism includes a pump body (11) and a sealed water tank (12). The pump body (11) is connected to the sealed water tank (12). The pump body (11) is also connected to the outer shell (21) via a first pressure-resistant pipeline (8) and a second pressure-resistant pipeline (19), thereby establishing a hydrostatic pressure environment between the sealed water tank (12), the first pressure-resistant pipeline (8), the second pressure-resistant pipeline (19), and the high-pressure chamber. A circulation loop is formed between the two, which allows the liquid to circulate. The first pressure-resistant pipeline (8) is also equipped with a shut-off valve (9) and a pressure gauge (10), and the second pressure-resistant pipeline (19) is also equipped with a pressure relief valve (33) and a pressure relief gauge (18). The circulating gas supply mechanism includes a gas storage container (15) and a gas processing mechanism (17). The gas storage container (15) is connected to the sealed water tank (12) via a gas guide pipe (14), and the gas processing mechanism (17) is connected to the sealed water tank (12) via an exhaust pipe (16). A flow meter (13) is also provided on the gas guide pipe (14).

2. The apparatus according to claim 1, characterized in that: The outer shell (21) is provided with a first sealing connector (3), a second sealing connector (29), and a third sealing connector (32). The first sealing connector (3), the second sealing connector (29), and the third sealing connector (32) are sealed to the outer shell (21). The auxiliary electrode (23), the probe (27), and the reference electrode (28) are electrically connected to the electrochemical workstation (20) via the first sealing connector (3), the second sealing connector (29), and the third sealing connector (32), respectively.

3. The apparatus according to claim 2, characterized in that: The needle insertion transmission mechanism includes a coarse adjustment knob (31) and a fine adjustment knob (30) located outside the high-pressure chamber, and a push rod partially located inside the high-pressure chamber. The coarse adjustment knob (31) and the fine adjustment knob (30) are connected to the probe (27) via the push rod. By turning either the coarse adjustment knob (31) or the fine adjustment knob (30), the probe (27) can be moved along the selected direction.

4. The apparatus according to claim 2, characterized in that: The needle insertion transmission mechanism also includes a micro-displacement brake (38), which is connected to the probe (27) and is used to drive the probe (27) to move and / or vibrate along the selected direction.

5. The apparatus according to claim 1, characterized in that: The outer casing (21) is also provided with an observation window (5).

6. The apparatus according to claim 5, characterized in that: The outer casing (21) is also provided with a lighting mechanism.

7. The apparatus according to claim 6, characterized in that: The lighting mechanism is correspondingly located at the observation window (5).

8. The apparatus according to claim 1 or 5, characterized in that: The outer casing (21) is also provided with a rupture disc (7).

9. The apparatus according to claim 1, characterized in that: The sample transfer unit includes a drive mechanism (1) and a sample rod (2). A portion of the sample rod (2) is disposed inside the high-pressure chamber and is sealed to the outer shell (21), and is used at least to carry the sample to be tested (24). The drive mechanism (1) is driven to the sample rod (2), and is used at least to drive the sample rod (2) to make linear motion along its own axis and / or rotate around its own axis.

10. The apparatus according to claim 9, characterized in that: The sample rod (2) is a hollow insulating component. An electrical connection wire (26) is provided inside the sample rod (2). The electrical connection wire is electrically connected to the electrochemical workstation (20), and the electrical connection wire (26) can also be electrically connected to the sample to be tested (24) set on the sample rod (2).

11. The apparatus according to claim 10, characterized in that: The sample rod (2) passes through the high-pressure chamber.

12. The apparatus according to claim 10, characterized in that: The outer casing (21) is also provided with a fourth sealing connector (34) and a fifth sealing connector (35). The fourth sealing connector (34) and the fifth sealing connector (35) are sealed to the outer casing (21). The electrical connection line (26) is electrically connected to the electrochemical workstation (20) via the fourth sealing connector (34) and the fifth sealing connector (35).

13. The apparatus according to claim 12, characterized in that: The sample rod (2) is sealed to the outer shell (21) via the fourth sealing connector (34) and the fifth sealing connector (35).

14. The apparatus according to claim 10, characterized in that: The sample transfer unit also includes a control mechanism (22), which is electrically connected to the drive mechanism (1).

15. The apparatus according to claim 10, characterized in that, Also includes: The sample spiral shaft (36) and sample stage transmission device (37) are located outside the high-pressure chamber. The drive mechanism (1) is connected to the sample stage transmission device (37). The sample stage transmission device (37) is connected to the sample spiral shaft (36). The sample spiral shaft (36) is fixedly connected to the sample rod (2). The sample spiral shaft (36) can rotate around its own axis and move linearly along its own axial direction.

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