An ultra-high vacuum compatible electrochemical reaction device

Abstract

This invention relates to an ultra-high vacuum compatible electrochemical reaction device, belonging to the field of electrochemical testing technology. The electrochemical reaction device includes a shell, a reaction vessel, a first transfer component, and a second transfer component. The first transfer component extends from the inlet of the shell to transfer the sample from the ultra-high vacuum system to the transfer chamber. The second transfer component transfers the sample from the transfer chamber to the reaction chamber. An inlet pipe and an outlet pipe are connected within the reaction chamber. In use, a vacuum pump is used to evacuate the transfer chamber and the reaction chamber. The sample is then transferred to the reaction chamber via the first and second transfer components. Electrolyte is introduced into the reaction chamber through the inlet and outlet pipes to conduct electrochemical experiments. After the reaction, the sample can be directly transferred to the ultra-high vacuum system for characterization using the first and second transfer components. This significantly reduces the risk of sample contamination and achieves seamless integration between electrochemical reaction and ultra-high vacuum characterization.

Description

Technical Field

[0001] This utility model relates to the field of electrochemical testing technology, and in particular to an ultra-high vacuum compatible electrochemical reaction device. Background Technology

[0002] To delve into the interfacial structure of reactants and products, the microscopic evolution of electrode surfaces, and the state of key intermediate species during electrochemical reactions, high-resolution and high-precision characterization techniques are required. Techniques such as ultra-high vacuum low-temperature scanning probe microscopy (SPM), X-ray photoelectron spectroscopy (XPS), and Auger electron spectroscopy (AES) are important tools for studying electrode interfacial reaction mechanisms due to their atomic-level spatial resolution and molecular-level chemical sensitivity.

[0003] However, traditional ultra-high vacuum compatible electrochemical reaction devices are independent of the ultra-high vacuum system for sample storage. The sample must first be removed from the ultra-high vacuum system and transferred to a reaction device containing electrolyte for electrochemical reaction, and then the reacted sample must be transferred back to the ultra-high vacuum system for characterization. However, there is a significant pressure difference between the traditional electrochemical reaction environment and the ultra-high vacuum characterization environment. In the past, during the back-and-forth sample transfer process, the sample inevitably came into contact with various impurities, such as moisture, oxygen, and other contaminants in the air. This makes the interface information susceptible to contamination or structural reconstruction during the transfer process, severely limiting the accuracy and timeliness of in-situ or quasi-in-situ characterization. Utility Model Content

[0004] This invention provides an ultra-high vacuum compatible electrochemical reaction device to reduce the risk of sample contamination and achieve seamless integration between electrochemical reaction and ultra-high vacuum characterization.

[0005] This invention provides an ultra-high vacuum compatible electrochemical reaction device, comprising: a shell, the interior of which forms a transfer chamber, and a vacuum pump connected to the shell, the vacuum pump being connected to the transfer chamber; the transfer chamber having an inlet and an outlet, the inlet being for connecting to an ultra-high vacuum system; a reaction vessel connected to the shell, the reaction vessel having a reaction chamber, the reaction chamber being connected to the outlet; a first transfer member connected to the shell, the first transfer member extending from the inlet into the transfer chamber to transfer a sample from the ultra-high vacuum system to the transfer chamber; and a second transfer member connected to the shell, the second transfer member for transferring a sample from the transfer chamber to the reaction chamber; wherein a gate valve is installed at the outlet, and an inlet pipe and a outlet pipe are connected to the reaction chamber, the inlet pipe being for introducing electrolyte into the reaction chamber, and valve bodies are provided at both the inlet pipe and the outlet pipe.

[0006] In one embodiment, the inlet pipeline has an inlet, the valve body of the inlet pipeline is a first stopcock located at the inlet, and the inlet pipeline is connected to a pump body for pumping electrolyte into the inlet pipeline. In one embodiment, the drain line has a drain port, and the valve body at the drain line is a second stopcock located at the drain port. In one embodiment, the reaction vessel includes a tube body, an adapter assembly connected to the upper end of the tube body for communicating with the discharge port, and a base connected to the lower end of the tube body. Both the inlet pipe and the outlet pipe are disposed within the base, and the adapter assembly, the tube body, and the base form a reaction chamber.

[0007] In one embodiment, the tube body is made of a transparent material.

[0008] In one embodiment, the adapter is provided with an air inlet for introducing inert gas into the reaction chamber.

[0009] In one embodiment, a reference electrode and a counter electrode are mounted on the adapter assembly, both of which extend into the tube body.

[0010] In one embodiment, the adapter assembly includes a connecting flange, one side of the gate valve is connected to the discharge port, and the other side of the gate valve is connected to the connecting flange.

[0011] In one embodiment, an observation window is provided on the housing.

[0012] In one embodiment, the second transfer element is a linear inlet.

[0013] Compared with the prior art, the advantage of this utility model is that the reaction vessel and the first and second transfer components for transferring samples are integrated into one device, which can directly transfer samples stored in the ultra-high vacuum system to the reaction vessel for reaction, reducing the risk of sample contamination.

[0014] Because the housing is connected to a vacuum pump, the gas in the reaction chamber and transfer chamber can be extracted before transfer to prevent residual gas from contaminating the sample. Then, the first transfer device transfers the sample from the ultra-high vacuum system to the transfer chamber, and the second transfer device transfers the sample from the transfer chamber to the reaction chamber within the reaction vessel. Electrolyte is introduced into the reaction chamber by controlling the valves in the inlet and outlet pipes, achieving contact between the electrolyte and the sample to initiate the electrochemical reaction. After the reaction is complete, the liquid in the reaction chamber is drained through the outlet pipe, and the vacuum pump removes impurities from the reaction chamber and transfer chamber for the next reaction. Attached Figure Description

[0015] The present invention will be described in more detail below based on embodiments and with reference to the accompanying drawings.

[0016] Figure 1 This is a schematic diagram of the main structure of the ultra-high vacuum compatible electrochemical reaction device in an embodiment of this utility model; Figure 2 This is a schematic diagram of the main structure of an electrochemical reaction device with a transparent tube in an embodiment of this utility model; Figure 3 This is a schematic diagram of the structure of the first transfer member in an embodiment of this utility model; Figure 4 This is a schematic diagram of the structure of the second transfer member in an embodiment of this utility model; Figure 5 This is a schematic diagram of the structure of the second transfer member in an embodiment of this utility model from another perspective.

[0017] Figure label: 1. Second transfer component; 2. Housing; 3. Gate valve; 4. Adapter assembly; 5. Tube body; 6. Base; 7. First interface; 8. Second interface; 9. Third interface; 10. Air inlet; 11. Liquid inlet; 12. Liquid outlet; 13. Feed inlet; 14. Sample transfer rod interface; 15. Counter electrode; 16. Reference electrode; 17. Sample; 18. Electrical connection. Detailed Implementation

[0018] The present invention will be further described below with reference to the accompanying drawings.

[0019] See Figures 1 to 3 As shown, this utility model provides an ultra-high vacuum compatible electrochemical reaction device, which includes: The shell 2, the reaction vessel, the first transfer member and the second transfer member 1, wherein the reaction vessel, the first transfer member and the second transfer member 1 are all connected to the shell 2.

[0020] A transfer chamber is formed inside the housing 2, and a vacuum pump (not shown in the figure) is also connected to the housing 2. The vacuum pump is connected to the transfer chamber. The transfer chamber has an inlet 13 and an outlet, and the inlet 13 is used to connect to an ultra-high vacuum system.

[0021] The reaction vessel is connected to the discharge port of the shell 2, and a reaction chamber is formed inside the reaction vessel.

[0022] An ultra-high vacuum system refers to a system that creates an ultra-high vacuum environment. Items requiring a high degree of cleanliness are often stored in ultra-high vacuum systems to prevent contamination from airborne impurities. The sample 17 to be reacted in this application will also be stored in an ultra-high vacuum system before the reaction.

[0023] The first transfer member is connected to the housing 2 and can extend out of the inlet 13 of the transfer chamber. When the inlet 13 is connected to the ultra-high vacuum system, the first transfer member can be extended into the ultra-high vacuum system through the inlet 13 to transfer the sample 17 from the ultra-high vacuum system into the transfer chamber. The first transfer member can also be used to transfer the reacted sample 17 from the transfer chamber into the ultra-high vacuum system.

[0024] The second transfer member 1 is connected to the housing 2. The second transfer member 1 can move the sample 17 in the transfer chamber from the outlet and extend it into the reaction chamber, thereby transferring the sample 17 in the transfer chamber to the reaction chamber.

[0025] A gate valve 3 is installed at the discharge port of the shell 2. By controlling the opening and closing of the gate valve 3, the transfer chamber and the reaction chamber can be connected or isolated.

[0026] An inlet pipe and an outlet pipe are connected within the reaction chamber. The inlet pipe is used to introduce electrolyte into the reaction chamber, and both the inlet and outlet pipes are equipped with valves. Because of the presence of both inlet and outlet pipes, and the valves at both ends, the timing and amount of electrolyte introduced into the reaction chamber can be flexibly controlled.

[0027] In use, first open gate valve 3 to connect the transfer chamber and the reaction chamber. Then close the valve of the inlet pipe and open the valve of the outlet pipe to drain the residual electrolyte in the reaction chamber. After that, close inlet 13 and turn on the vacuum pump to extract the gas from the reaction chamber and the transfer chamber, and also extract any remaining electrolyte. This completes the preparation work before the experiment.

[0028] Then, the ultra-high vacuum compatible electrochemical reaction device is connected to the ultra-high vacuum system containing sample 17, so that the inlet 13 of the transfer chamber is connected to the ultra-high vacuum system. The first transfer member is controlled to extend, so that the end of the first transfer member extends out of the inlet 13 and enters the ultra-high vacuum system. The sample 17 in the ultra-high vacuum system is taken out by the first transfer member and transferred to the transfer chamber.

[0029] After sample 17 is transferred to the transfer chamber, the first transfer element is controlled to transfer sample 17 from the outlet to the reaction chamber. By controlling the valve body with the re-inlet pipeline and the valve body with the re-outlet pipeline, an appropriate amount of electrolyte is introduced into the reaction chamber to conduct an electrochemical reaction experiment.

[0030] Because the gas in both the reaction chamber and the transfer chamber is extracted by a vacuum pump during the transfer process, contamination of sample 17 by impurities remaining in the transfer chamber and reaction chamber is avoided, achieving seamless integration between electrochemical reaction and ultra-high vacuum characterization. Furthermore, since the reaction chamber is connected to both inlet and outlet pipes, electrolyte can be introduced into the reaction chamber, and the amount of electrolyte can be flexibly controlled via a control valve. This makes the reaction process relatively convenient.

[0031] After the reaction, the sample 17 can be transferred to the transfer chamber using the second transfer device, and then the sample 17 can be transferred to the ultra-high vacuum system for characterization using the first transfer device. This greatly reduces the probability of the sample 17 coming into contact with contaminants during the transfer process, and allows for better measurement of the changes in the sample before and after the reaction.

[0032] See Figure 1 and Figure 2 As shown, in some implementations, the liquid inlet pipeline has a liquid inlet 11, the valve body of the liquid inlet pipeline is not provided with a first stopcock at the liquid inlet 11, the liquid inlet pipeline is connected to a pump body, and the pump body is used to pump electrolyte into the liquid inlet pipeline.

[0033] In use, first connect the inlet 11 of the inlet pipe to the container storing the required electrolyte, and control the opening and closing of the inlet 11 by rotating the first stopcock. When it is necessary to add electrolyte to the reaction chamber, first open the inlet 11 by rotating the first stopcock, and then use the pump to pump the electrolyte into the inlet pipe, allowing the electrolyte to flow into the reaction chamber. The pump can be a miniature peristaltic pump, which can continue to pump electrolyte in even after the electrolyte in the reaction chamber has been completely drained. After adding electrolyte, the pump can be turned off, and the inlet 11 can be closed by rotating the first stopcock.

[0034] See Figure 1 and Figure 2 As shown, in some implementations, the drain pipe has a drain port 12, and the valve body at the drain pipe is a second stopcock located at the drain port 12. By rotating the second stopcock, the opening and closing of the drain port 12 can be controlled, achieving flexible control of the drain.

[0035] In some implementations, the reaction vessel includes a tube body 5, with a transfer assembly 4 connected to the upper end of the tube body 5 for communicating with the discharge port, and a base 6 connected to the lower end of the tube body 5. The transfer assembly 4, the tube body 5, and the base 6 form a reaction chamber, and the liquid inlet pipe and the liquid outlet pipe are both located inside the base 6.

[0036] In other words, the reaction vessel in this application is connected to the shell 2 via the adapter component 4, and the electrolyte is introduced and discharged from the base 6 at the bottom of the tube 5. Compared to setting a drain pipe at a higher elevation, the electrolyte in the reaction chamber can be discharged more thoroughly using the drain pipe, reducing electrolyte residue. Furthermore, the liquid level rises gradually during the process of introducing electrolyte into the reaction chamber, making it easier to control the amount of electrolyte.

[0037] In some implementations, the tube 5 is made of a transparent material, allowing the amount of electrolyte in the reaction chamber to be seen through the tube 5, thus enabling more accurate control of the electrolyte flow rate. The tube 5 can be made of glass. Glass is not only transparent, facilitating control of the electrolyte amount, but also chemically stable, thus not affecting the electrochemical reaction.

[0038] In some implementations, substrate 6 is made of polytetrafluoroethylene (PTFE), which not only has high strength but also excellent chemical stability against acids, alkalis, and organic solvents. This makes it suitable for electrochemical experiments using various electrolyte systems.

[0039] In some implementations, the adapter 4 is provided with an inlet 10 for introducing inert gas into the reaction chamber. After evacuation and before introducing electrolyte into the reaction chamber, inert gas can be introduced into the reaction chamber through the inlet 10 to regulate the gas pressure inside the reaction chamber and prevent the electrolyte from being introduced into the reaction chamber too quickly due to the vacuum environment. Argon gas, or other types of inert gas, can be introduced into the reaction chamber through the inlet 10.

[0040] In addition, by introducing inert gas into the reaction chamber through the air inlet 10, a slight positive pressure environment can be formed in the reaction chamber and the transfer chamber, thereby blocking the intrusion of external impurities such as oxygen and water vapor to the greatest extent and ensuring the purity of sample 17.

[0041] Of course, after the test is completed, the airflow blown out of the air inlet 10 can be used to purge the sample 17, thereby removing the residual liquid on the surface of the sample 17. Then, the purged sample 17 is transferred to the ultra-high vacuum system through the cooperation of the first transfer member and the second transfer member 1.

[0042] See Figure 1 as well as Figure 2 In some implementations, a reference electrode 16 and a counter electrode 15 are mounted on the adapter 4, and both the reference electrode 16 and the counter electrode 15 extend into the tube body 5.

[0043] When introducing electrolyte into the reaction chamber, sample 17, counter electrode 15, and reference electrode 16 must all be immersed in the electrolyte to form a three-electrode structure, with sample 17 serving as the working electrode in the three-electrode system. By controlling the current and voltage of reference electrode 16 and counter electrode 15, various electrochemical reactions of sample 17 can be tested. This enables various electrochemical reaction tests, such as linear sweep voltammetry and cyclic voltammetry.

[0044] The adapter component 4 is equipped with two BNC interfaces. One BNC interface (second interface 8) is used to connect the reference electrode 16 to an external control circuit, and the other BNC interface (third interface 9) is used to connect the counter electrode 15 to an external control circuit. The voltage and current control of the reference electrode 16 and the counter electrode 15 are realized through the two BNC interfaces.

[0045] See Figure 1 as well as Figure 2 As shown, in some implementations, the adapter 4 includes a connecting flange, one side of the gate valve 3 is connected to the discharge port, and the other side of the gate valve 3 is connected to the connecting flange. In this application, the reaction vessel and the gate valve 3 are connected through the connecting flange. The reaction vessel can be easily removed by disassembling and assembling the connecting flange to facilitate cleaning or maintenance of the shell 2 or the reaction vessel. Compared with an integrated design, this reduces the difficulty of subsequent cleaning and maintenance.

[0046] See Figure 2 As shown, in some implementations, the connecting flange is a reducing flange, and the diameter of the side of the connecting flange connected to the gate valve 3 is smaller than the diameter of the side of the connecting flange connected to the pipe body 5. This allows for the use of a larger diameter pipe body 5 to complete the electrochemical reaction test, and also allows for adaptation to the size of the gate valve 3.

[0047] In some implementations, an observation window is provided on the housing 2. The internal condition of the transfer cavity can be directly observed through the observation window of the housing 2. During the process of transferring the sample 17 using the first transfer member and the second transfer member 1, the position of the sample 17 can be seen intuitively through the observation window, and the position of the sample 17 can be accurately adjusted.

[0048] An observation window can be provided on both the front and rear sides of the housing 2. It is understandable that the observation windows are made of a transparent material, which can meet the requirements for observing the internal environment of the reaction chamber while preventing foreign objects from entering the transfer chamber through the observation windows.

[0049] See Figure 1 , Figure 4 as well as Figure 5As shown, in some implementations, the second transfer element 1 is a linear inlet, capable of linear movement. The linear actuator is used for the linear movement of the sample 17 within the vacuum chamber of the vacuum equipment. The internal dynamic seal employs a welded bellows structure, resulting in smoother linear drive, better sealing performance, and more precise position control, suitable for ultra-high vacuum environments. As shown in the figure, the second transfer element 1 in this application is installed above the housing 2, enabling vertical transfer of the sample 17. It can transfer the sample 17 from the outlet at the bottom of the transfer chamber to the reaction chamber, or retrieve the sample 17 from the reaction chamber back into the transfer chamber. See also... Figure 1 , Figure 4 as well as Figure 5 As shown, the second transfer member 1 is provided with an electrical connection part 18. When the second transfer member 1 comes into contact with the sample 17, the sample is electrically connected to the electrical connection part 18 provided on the second transfer member 1. Furthermore, the electrical connection part 18 in this application is connected to a BNC interface (first interface 7) provided on the top of the second transfer member 1 via a wire. By connecting the first interface 7 to a controller, the current and voltage of the electrical connection part 18 on the second transfer member 1 can be adjusted or measured, thereby ensuring that the sample is in a suitable electrochemical environment when immersed in the electrolyte, and thus completing the corresponding electrochemical reaction.

[0050] In some implementations, the first transfer element is a sample transfer rod, see [link to relevant documentation]. Figure 2 As shown, it is installed on the left side of the housing 2 and inserted into the sample transfer rod interface 14 of the housing 2. The sample transfer rod can extend into the transfer chamber and can extend out from the feed port 13 on the right side of the transfer chamber. When the feed port 13 is connected to the ultra-high vacuum system, the sample transfer rod extending out of the feed port 13 can extend into the ultra-high vacuum system and take out the sample 17 in the ultra-high vacuum system and transfer it to the transfer chamber.

[0051] Although the present invention has been described with reference to preferred embodiments, various modifications can be made thereto and components can be replaced with equivalents without departing from the scope of the invention. In particular, the technical features mentioned in the various embodiments can be combined in any manner, provided there is no structural conflict. The present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. An ultrahigh vacuum compatible electrochemical reaction device, characterized by, It includes: The housing has a transfer chamber inside, and the housing is also connected to a vacuum pump. The vacuum pump is connected to the transfer chamber, and the transfer chamber has an inlet and an outlet. The inlet is used to connect to an ultra-high vacuum system. A reaction vessel connected to the shell, the reaction vessel having a reaction chamber connected to the discharge port; A first transfer member is connected to the housing and is used to extend from the inlet into the transfer cavity to transfer the sample from the ultra-high vacuum system into the transfer cavity. as well as The second transfer member is connected to the housing and is used to transfer the sample in the transfer chamber to the reaction chamber. The discharge port is equipped with a gate valve, and the reaction chamber is connected to an inlet pipe and a outlet pipe. The inlet pipe is used to introduce electrolyte into the reaction chamber, and both the inlet pipe and the outlet pipe are equipped with valve bodies.

2. The ultra-high vacuum compatible electrochemical reaction device according to claim 1, characterized in that, The liquid inlet pipeline has a liquid inlet, and the valve body of the liquid inlet pipeline is a first stopcock located at the liquid inlet. The liquid inlet pipeline is connected to a pump body, which is used to pump electrolyte into the liquid inlet pipeline.

3. The ultra-high vacuum compatible electrochemical reaction device according to claim 2, characterized in that, The drain pipe has a drain port, and the valve body at the drain pipe is a second stopcock located at the drain port.

4. The ultra-high vacuum compatible electrochemical reaction apparatus according to any one of claims 1-3, characterized in that, The reaction vessel includes a tube body, the upper end of which is connected to a transfer assembly for communicating with the discharge port, and the lower end of which is connected to a base. The liquid inlet pipe and the liquid outlet pipe are both disposed within the base. The transfer assembly, the tube body, and the base form the reaction chamber.

5. The ultra-high vacuum compatible electrochemical reaction device according to claim 4, characterized in that, The tube body is made of transparent material.

6. The ultra-high vacuum compatible electrochemical reaction device according to claim 4, characterized in that, The adapter assembly is provided with an air inlet, which is used to introduce inert gas into the reaction chamber.

7. The ultra-high vacuum compatible electrochemical reaction device according to claim 4, characterized in that, The adapter assembly is equipped with a reference electrode and a counter electrode, both of which extend into the tube body.

8. The ultra-high vacuum compatible electrochemical reaction device according to claim 4, characterized in that, The adapter assembly includes a connecting flange, one side of the gate valve is connected to the discharge port, and the other side of the gate valve is connected to the connecting flange.

9. The ultra-high vacuum compatible electrochemical reaction apparatus according to any one of claims 1-3, characterized in that, An observation window is provided on the housing.

10. The ultra-high vacuum compatible electrochemical reactor of any one of claims 1-3, wherein, the second transfer member is a linear inductor.

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