Electrochemical reaction tank for hard X-ray absorption spectrum in-situ dual-mode test

Abstract

The utility model discloses an electrochemical reaction tank for a hard X-ray absorption spectrum in-situ dual-mode test. The electrochemical reaction tank comprises a reaction tank body, a working electrode, a reference electrode and a graphite counter electrode, the front plate is provided with a working electrode window, and the upper plate is provided with a reference electrode hole and a graphite counter electrode hole. The working electrode is arranged at the window of the front plate and is tightly attached to the reaction tank body through a polyimide adhesive tape, and the reference electrode and the graphite counter electrode are arranged on the two sides of the reaction tank body and are respectively connected with an external electrochemical working platform. The distance between the working electrode window and the rear plate is controlled, and the working electrode is coupled with synchrotron radiation X-ray incident light, a fluorescence signal and a transmission signal to form an X-ray dual-mode test channel. The advantages of a synchrotron radiation X-ray absorption spectrum measuring platform are fully utilized, a real in-situ electrochemical detection environment is simulated, and reliable fluorescence and transmission signals are collected at the same time.

Description

Technical Field

[0001] This invention relates to the field of electrocatalytic reaction characterization technology, and in particular to an electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy. Background Technology

[0002] The composition and structure of energy materials directly affect their energy conversion efficiency. During energy conversion, precise characterization of surface structures and accurate identification of intermediate products enable a more accurate understanding of the dynamic processes of chemical reactions, allowing for in-depth research into reaction mechanisms and providing theoretical basis and technical support for improving energy conversion efficiency and product selectivity. However, while traditional offline structural characterization techniques can provide static structural information about materials, they are significantly insufficient in capturing dynamic structural changes under actual service conditions. These techniques often cannot monitor in real time the instantaneous changes in the surface composition and structure of materials caused by external conditions (such as electric field, light field, temperature, and pressure), greatly limiting our comprehensive understanding and in-depth exploration of energy conversion mechanisms. Synchrotron radiation hard X-ray absorption spectroscopy, as an advanced in-situ characterization technique, can provide detailed information about the electronic structure and coordination environment of absorbing atoms by analyzing the changes in the absorption coefficients of specific elements in the material. In electrochemical energy conversion processes, this technique not only reflects the true state of energy materials but also reveals the intrinsic relationship between the microstructure of the material's active centers and its electrochemical performance, opening up new avenues for exploring structure-activity relationships.

[0003] Existing technologies disclose many in-situ electrochemical reaction cells, such as the electrocatalytic reaction cell proposed by the University of Science and Technology of China for in-situ testing of hard X-ray absorption spectroscopy (CN208399425U), and the in-situ photoelectrocatalytic electrolysis cell and its application in X-ray absorption spectroscopy proposed by ShanghaiTech University (CN117589920A), which realize in-situ (photo)electrochemical testing. However, all of them acquire the signal generated by the sample in a single mode of transmission or fluorescence. The acquisition of X-ray absorption spectroscopy in transmission mode has high requirements for the content of the analyte element in the sample and the thickness of the electrolyte that has penetrated. For fluorescence measurement mode, the advantage is that the content requirement of the analyte element is lower, but the existence of self-absorption effect may cause misleading in the data analysis process. Therefore, it is necessary to comprehensively optimize the design of in-situ electrochemical reaction cells based on the synchrotron radiation hard X-ray absorption spectroscopy testing mode. Utility Model Content

[0004] The main technical problems to be solved by this utility model are as follows: solving the problems of single testing mode, low testing efficiency and poor spectrum quality of traditional in-situ electrochemical reaction cells; and simultaneously acquiring sample signals in fluorescence and transmission modes to obtain effective hard X-ray absorption spectra.

[0005] In view of this, the present invention provides an electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy. This reaction cell can restore the state of electrochemical testing to the greatest extent. By controlling the thickness of the electrolyte layer on the surface of the working electrode and the distance and angle between the working electrode and the fluorescence detector, in-situ dual-mode testing can be achieved.

[0006] The technical solution adopted by this utility model to solve its technical problem is:

[0007] An electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy includes a reaction cell body, a working electrode, a reference electrode, and a graphite counter electrode.

[0008] The reaction tank includes an upper plate, a bottom plate, a front plate and a rear plate of different shapes arranged in parallel, and a pair of side plates arranged in parallel. The front plate, rear plate and side plates are vertically arranged between the upper plate and the bottom plate. The front plate includes a first front plate body, a second front plate body and a third front plate body connected in sequence. The rear plate includes a first rear plate body, a second rear plate body and a third rear plate body connected in sequence. A working electrode window is provided on the second front plate body of the front plate.

[0009] The upper plate of the reaction tank is provided with a through reference electrode hole and a graphite counter electrode hole.

[0010] The working electrode is disposed at the working electrode window, the reference electrode is disposed in the reference electrode hole, and the graphite counter electrode is disposed in the graphite counter electrode hole.

[0011] In the above technical solution, the second front panel is set at a 135-degree angle to the first front panel, the second front panel is set at a 135-degree angle to the third front panel, and the first front panel and the third front panel are set in parallel.

[0012] In the above technical solution, the second rear plate is set at a 135-degree angle to the first rear plate, the second rear plate is set at a 135-degree angle to the third rear plate, and the first rear plate and the third rear plate are set in parallel.

[0013] In the above technical solution, the graphite counter electrode is disposed between the first front plate and the first rear plate.

[0014] In the above technical solution, the reference electrode is disposed between the third front plate and the third rear plate.

[0015] In the above technical solution, the upper plate, bottom plate, front plate, rear plate and side plate are made of polymethyl methacrylate.

[0016] In the above technical solution, the diameter of the working electrode window is 16 mm, the diameter of the reference electrode hole is 16 mm, and the size of the graphite electrode hole is 10 mm × 8 mm.

[0017] Beneficial effects:

[0018] An electrochemical reaction cell for in-situ dual-mode hard X-ray absorption spectroscopy employs conductive materials such as carbon cloth or carbon paper as the working electrode substrate. The sample is coated or directly grown on the substrate. The other side is attached to the working electrode window of the reaction cell body using polyimide tape. One end of the substrate is connected to conductive tape to extract the electrical signal. Assembly, disassembly, and cleaning are simple and convenient. The working electrode is easy to replace, has good sealing, and is internally insulated. Without affecting mass transfer, the distance between the working electrode window and the rear plate of the reaction cell body is shortened, reducing the absorption and scattering of X-rays by the electrolyte and improving the data quality obtained in transmission mode. The angle between the working electrode and both the X-ray and fluorescence detectors is 45 degrees, and the distance between the working electrode window and the fluorescence detector must be at the detector's optimal focusing distance to ensure efficient collection of the fluorescence signal generated by the sample in the fluorescence ionization chamber. The working electrode couples with the synchrotron radiation X-ray incident light, fluorescence signal, and transmission signal to form an X-ray dual-mode testing channel. Once the electrochemical reaction cell is assembled, it can simulate a real in-situ electrochemical detection environment, simultaneously obtaining hard X-ray absorption spectra of samples under different bias voltages, currents, and electrolyte conditions, in both fluorescence and transmission modes. This invention overcomes the problems of existing similar devices, such as limited measurement modes and complex operation, and can be used for in-situ studies of various electrochemical reactions. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the main components of an electrochemical reaction cell used for in-situ dual-mode testing of hard X-ray absorption spectroscopy.

[0020] Figure 2 This is a front view of the reaction tank of this utility model.

[0021] Figure 3 This is a top view of the reaction tank of this utility model.

[0022] Figure 4 This is a schematic diagram of the bottom plate structure of the reaction tank of this utility model.

[0023] In the figure, 1 is the reaction cell body, 2 is the working electrode, 3 is the reference electrode, 4 is the graphite counter electrode, 5 is the first front plate, 6 is the second front plate, 7 is the third front plate, 8 is the working electrode window, 9 is the first rear plate, 10 is the second rear plate, 11 is the third rear plate, 12 is the upper plate, 13 is the reference electrode hole, 14 is the graphite counter electrode hole, and 15 is the bottom plate. Detailed Implementation

[0024] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. However, the following embodiments are only for explaining the present invention, and the scope of protection of the present invention should include all the contents of the claims. Moreover, through the description of the following embodiments, those skilled in the art can fully implement all the contents of the claims of the present invention.

[0025] Example 1:

[0026] like Figure 1 As shown in Figure 2, this utility model provides an electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy. The reaction cell body adopts a shape suitable for synchrotron radiation hard X-ray absorption spectroscopy testing equipment, including a reaction cell body 1, a working electrode 2, a reference electrode 3, and a graphite counter electrode 4. To ensure the acquisition quality of transmission and fluorescence signals, polymethyl methacrylate is selected as the material of the reaction cell body. The second front plate 6 is at a 135-degree angle to the first front plate 5, and the second front plate 6 is at a 135-degree angle to the third front plate 7. The first front plate 5 and the third front plate 7 are parallel. The second rear plate 10 is at a 135-degree angle to the first rear plate 9, and the second rear plate 10 is at a 135-degree angle to the third rear plate 11. The first rear plate 9 and the third rear plate 11 are parallel. The second front plate 6 and the second rear plate 10 are parallel and the distance between them is 3~7 mm. mm, the second front plate 6 is provided with a working electrode window 8, and the working electrode 2 is tightly attached to the reaction tank body with polyimide tape; the upper plate 12 is provided with a reference electrode hole 13 and a graphite counter electrode hole 14 for placing the reference electrode 3 and the counter electrode 4 respectively.

[0027] Example 2:

[0028] exist Figure 3 In the reaction cell, the upper plate is provided with a reference electrode hole 13 with a diameter of 16 mm and a graphite counter electrode hole 14 with a length × width of 10 mm × 8 mm. The reference electrode 3 and the graphite counter electrode 4 are inserted into the reaction cell from above. A conductive material such as carbon cloth or carbon paper is used as the substrate for the working electrode. A powder sample prepared in the form of ink is coated or directly grown on one side of the substrate. One end of the substrate is connected to a conductive material such as copper tape or carbon tape to extract the electrical signal. The second front plate 6 is provided with a working electrode window 8 with a diameter of 16 mm. To prevent the solution in the reaction cell from flowing out, a polyimide tape with a thickness of 0.05 mm and resistant to acid, alkali and high temperature is used to tightly attach the working electrode 2 to the reaction cell at the window. The lead wire of the working electrode is led out along the upper plate 12. Figure 4A schematic diagram of the bottom plate structure of the reaction cell is provided. The angle between the second front plate 6 and the third front plate 7, which are perpendicular to the bottom plate 15, is 135 degrees, ensuring that the fluorescence ionization chamber efficiently collects the fluorescence signal generated by the sample. To reduce the interference of the electrolyte layer on the transmission signal without affecting mass transfer, the distance between the second front plate 6 and the second rear plate 10 is 3-7 mm. Before testing, the electrolyte is injected to just cover the upper edge of the working electrode window. The reaction cell of this invention is then placed on the corresponding synchrotron radiation hard X-ray absorption spectroscopy testing device. The angle between the working electrode and the X-ray and fluorescence detectors is 45 degrees, and the distance to the fluorescence detector must be at the optimal focusing distance of the detector. The working electrode 2, the reference electrode 3, and the graphite counter electrode 4 are connected to form a complete three-electrode electrochemical reaction in-situ cell system, which can then begin in-situ hard X-ray absorption spectroscopy testing, while simultaneously collecting experimental data of the sample's fluorescence and transmission test modes.

[0029] The above description is merely a specific embodiment of this application, enabling those skilled in the art to understand or implement this application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of this application. Therefore, this application is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features claimed herein.

Claims

1. An electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy, characterized in that: This includes the reaction cell body, working electrode, reference electrode, and graphite counter electrode; The reaction tank includes an upper plate, a bottom plate, a front plate and a rear plate of different shapes arranged in parallel, and a pair of side plates arranged in parallel. The front plate, rear plate and side plates are vertically arranged between the upper plate and the bottom plate. The front plate includes a first front plate body, a second front plate body and a third front plate body connected in sequence. The rear plate includes a first rear plate body, a second rear plate body and a third rear plate body connected in sequence. A working electrode window is provided on the second front plate body of the front plate. The upper plate of the reaction tank is provided with a through reference electrode hole and a graphite counter electrode hole. The working electrode is disposed at the working electrode window, the reference electrode is disposed in the reference electrode hole, and the graphite counter electrode is disposed in the graphite counter electrode hole.

2. The electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy according to claim 1, characterized in that: The second front panel is set at a 135-degree angle to the first front panel, the second front panel is set at a 135-degree angle to the third front panel, and the first front panel and the third front panel are set in parallel.

3. The electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy according to claim 1, characterized in that: The second rear plate is set at a 135-degree angle to the first rear plate, the second rear plate is set at a 135-degree angle to the third rear plate, and the first rear plate and the third rear plate are set in parallel.

4. The electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy according to claim 1, characterized in that: The graphite counter electrode is disposed between the first front plate and the first rear plate.

5. The electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy according to claim 1, characterized in that: The reference electrode is disposed between the third front plate and the third rear plate.

6. The electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy according to claim 1, characterized in that: The upper plate, bottom plate, front plate, rear plate and side plate are made of polymethyl methacrylate.

7. The electrochemical reaction cell for in-situ dual-mode testing of hard X-ray absorption spectroscopy according to claim 1, characterized in that: The working electrode window has a diameter of 16 mm, the reference electrode hole has a diameter of 16 mm, and the graphite electrode hole has a size of 10 mm × 8 mm.

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