A multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction and its application

Abstract

A multifunctional flow-type in-situ spectral detection device for electrocatalytic reactions and its application relate to the field of catalytic analysis. The device includes an in-situ reaction cell and an electrochemical workstation. The in-situ reaction cell includes a light-transmitting sealing window, a first cathode cavity, a second cathode cavity, and a cathode gas chamber; the second cathode cavity and the cathode gas chamber are screwed to the first cathode cavity and the second cathode cavity, respectively; the device is provided with circulation inlets and outlets for the anolyte, cathode electrolyte, and cathode reaction gas, as well as a gas flow channel connecting the second cathode cavity and the cathode gas chamber. In addition, the device also includes a reference electrode, a counter electrode, a working electrode, and an ion exchange membrane, each of which is connected to the electrochemical workstation. The in-situ reaction cell is connected to an in-situ spectrometer, the distance between the working electrode and the light-transmitting sealing window is adjusted by rotating the second cathode cavity, voltage and current are applied through the electrochemical workstation, and the spectral signal during the electrocatalytic reaction is collected using the in-situ spectrometer.

Description

Technical Field

[0001] The present invention relates to the technical field of catalytic analysis, and in particular to a multifunctional flow-type in-situ spectrum detection device for electrocatalytic reactions and applications thereof. Background Art

[0002] With the rapid depletion of fossil energy and increasingly severe environmental pollution, electrocatalytic reaction technology has shown great potential in electrochemical energy conversion and material transformation due to its ability to finely control the energy of electrochemical reaction systems and the direction and progress of reactions at room temperature and pressure. Emerging technologies such as hydrogen-oxygen fuel cells and electrocatalytic carbon dioxide reduction offer innovative solutions to address energy and environmental challenges. However, the core of these technologies lies in the design of efficient catalysts that balance reaction stability, selectivity, and activity.

[0003] In situ spectroscopic techniques play a key role in exploring the mechanisms of electrocatalytic reactions, catalyst evolution, and structural analysis. The in situ cell, a core component for conducting in situ spectroscopic studies of electrocatalysis, has a direct impact on the reliability and practicality of experimental results. However, existing in situ cells are typically only suitable for specific characterization methods, and the applied current is often small, making it difficult to simulate actual reaction conditions, resulting in significant differences between experimental results and actual working conditions.

[0004] Performing multiple characterizations on a single catalyst is essential for a deeper understanding of its performance, optimized design, and application. This integrated characterization approach can provide comprehensive structure-activity relationships, reveal reaction mechanisms, and guide the development of highly efficient catalysts. In particular, performing multiple characterization techniques in the same in situ cell yields comprehensive, consistent, and interrelated data, enabling a deeper understanding of the complex relationships between material properties, structure, and dynamic processes while improving experimental efficiency and data reliability.

[0005] At present, most in-situ cells used for electrocatalytic reactions are limited to a single characterization technology. For example: Chinese patent CN115452800A discloses an in-situ surface-enhanced Raman spectroscopy system for real-time monitoring of the electrocatalytic three-phase interface, but it is limited to in-situ Raman spectroscopy measurements in electrocatalytic reactions. Chinese patent CN112858421A describes an in-situ synchrotron radiation electrolysis cell for electrocatalytic systems, which is specifically used for in-situ synchrotron radiation measurements in electrocatalytic reactions, but the gas can only participate in the reaction after being dissolved, which limits its scope of application. Chinese patent CN117269210A introduces the design and testing method of an in-situ XRD micro-electrolysis cell for foam metal electrodes, but it is only applicable to in-situ XRD tests using foam metal as the working electrode, and does not support gas passage tests.

[0006] Although these existing technologies have their own characteristics, none of them has been able to integrate multiple characterization techniques in a single in-situ cell, and it is difficult to perform in-situ characterization under conditions close to actual working conditions, thus limiting the comprehensive understanding and optimization of the electrocatalytic process.

[0007] Specifically, existing in-situ electrolytic cells face numerous challenges in electrocatalysis research, primarily due to their limited functionality, poor adaptability, complex assembly, insufficient sealing, and limited ability to simulate operating conditions. These design limitations have severely hampered the application and development of in-situ spectroscopic characterization techniques in electrocatalysis, particularly in their ability to comprehensively characterize cells under realistic operating conditions.

[0008] The root causes of these shortcomings can be traced back to several key factors, including limited design concepts, insufficient technological integration, a lack of modular design, a poor understanding of the actual application environment, and inadequate analysis of user needs. The combined effect of these factors makes it difficult for existing in situ electrolytic cells to meet the increasingly diverse and comprehensive demands of electrocatalysis research, highlighting the urgent need to develop new, multifunctional, and highly adaptable in situ electrolytic cells to promote deeper and more comprehensive electrocatalysis research. Summary of the Invention

[0009] The purpose of the present invention is to solve the many limitations of in-situ electrolytic cells in the prior art, and to provide a multifunctional flow-type in-situ spectral detection device for electrocatalytic reactions and its application, which is multifunctional, efficient and flexible; first, by integrating multiple characterization technologies, a single device can simultaneously or alternately perform multiple in-situ spectral detections, thereby providing comprehensive and consistent data; second, a modular design is adopted to improve the adaptability and scalability of the device, so that it can flexibly respond to different experimental needs; third, the sealing performance and working condition simulation capabilities of the device are optimized, so that it can perform efficient in-situ characterization under conditions close to actual reaction conditions. Through these innovations, the present invention aims to provide a powerful tool for the study of electrocatalytic reaction mechanisms, tracking of catalyst evolution processes, and structural analysis, thereby providing key scientific basis and technical support for the development of new catalysts with high performance and high stability.

[0010] In order to achieve the above object, the present invention adopts the following technical solutions:

[0011] A multifunctional flow-type in-situ spectral detection device for electrocatalytic reactions, comprising an in-situ reaction cell and an electrochemical workstation; the in-situ reaction cell comprises, arranged from top to bottom, a first heating plate, a light-transmitting sealing window, a first cathode cavity, a second cathode cavity, a cathode gas chamber, and a second heating plate;

[0012] An anode cavity is provided on the side of the first cathode cavity. The interior of the first cathode cavity is a cylindrical hollow structure with a threaded inner wall. An opening is provided on the side of the first cathode cavity to connect the hollow structure with the anode cavity. The light-transmitting sealing window cover is provided on the hollow structure of the first cathode cavity.

[0013] The second cathode cavity is a columnar structure, with threads on both the outer and inner walls. The second cathode cavity is placed in the lower part of the first cathode cavity and is screwed to the first cathode cavity.

[0014] The cathode gas chamber is a columnar structure with a threaded outer wall. The cathode gas chamber is placed inside the second cathode cavity and is screwed to the second cathode cavity.

[0015] The anode cavity is provided with an anode electrolyte circulation inlet and outlet; the first cathode cavity is provided with a cathode electrolyte circulation inlet and outlet; the cathode gas chamber is provided with a cathode reaction gas inlet and outlet, and a gas flow channel connected to the second cathode cavity; the top of the second cathode cavity is provided with a connecting hole;

[0016] The first heating plate is arranged at the upper part of the first cathode cavity, and the second heating plate is arranged at the lower part of the second cathode cavity;

[0017] The present invention also includes a reference electrode, a counter electrode, a working electrode and an ion exchange membrane;

[0018] One end of the reference electrode is connected to the electrochemical workstation, and the other end is inserted into the hollow structure from the side of the first cathode cavity; the counter electrode and the ion exchange membrane are arranged between the anode cavity and the first cathode cavity, and the ion exchange membrane is close to the first cathode cavity, and the counter electrode is connected to the electrochemical workstation through a conductive part inserted into the anode cavity; the working electrode is arranged between the second cathode cavity and the cathode gas chamber, and the cathode gas chamber is made of conductive material, and the working electrode is connected to the chemical workstation through a conductive part inserted into the cathode gas chamber.

[0019] The present invention further comprises a window cover and a sealing rubber ring, wherein the sealing rubber ring is arranged between the light-transmitting sealing window and the window cover.

[0020] The present invention further comprises a sealing gasket, which is arranged between the first cathode cavity and the anode cavity.

[0021] The anode cavity and the first cathode cavity are connected by bolts.

[0022] A serpentine flow channel communicating with the anode electrolyte circulation inlet and outlet is provided on the inner side of the anode cavity, and the counter electrode is located at the serpentine flow channel.

[0023] The cathode gas chamber is made of titanium or stainless steel.

[0024] The working electrode includes a gas diffusion electrode, a glassy carbon electrode and a metal foil.

[0025] The multifunctional flow-type in-situ spectral detection device for electrocatalytic reactions is applied by connecting the in-situ reaction cell to the in-situ spectrometer, adjusting the distance between the working electrode and the light-transmitting sealing window by rotating the second cathode cavity, applying voltage and current through the electrochemical workstation, and using the in-situ spectrometer to collect spectral signals during the electrocatalytic reaction.

[0026] The spectral signals include X-ray diffraction spectral signals, synchrotron radiation spectral signals or Raman spectral signals to meet different in-situ characterization requirements.

[0027] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0028] 1. This paper designs a multifunctional flow-based in-situ spectroscopic detection device specifically for studying electrocatalytic reactions involving cathode gas under realistic operating conditions. This device can conduct reactions over long periods of time at high current densities, enabling in-depth analysis of reaction mechanisms, catalyst evolution, and catalyst structure, thereby facilitating the design of highly efficient catalysts.

[0029] 2. The present invention allows replacement of windows of different materials according to different requirements of the detection light source. At the same time, the distance between the window and the cathode working electrode is adjustable to adapt to different types of detection instruments, thereby enhancing the adaptability and flexibility of the device.

[0030] 3. The present invention offers a variety of working electrode options, including gas diffusion electrodes, glassy carbon electrodes, and metal foils, to meet diverse experimental needs. These electrodes all maintain excellent electrical conductivity, ensuring efficient electrocatalytic reactions.

[0031] 4. The ingenious assembly design of the present invention achieves excellent gas-liquid sealing and ensures stability during the experiment. In addition, the controllable reaction temperature further enhances the performance of the device, making it adaptable to various reaction conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 Schematic diagram of the overall structure of the in-situ reaction pool of the present invention;

[0033] Figure 2 This is one of the schematic diagrams of the decomposition structure of the in-situ reaction tank of the present invention;

[0034] Figure 3 This is the second schematic diagram of the decomposition structure of the in-situ reaction tank of the present invention.

[0035] Figure numerals: first heating plate 1, window cover 2, light-transmitting sealing window 3, sealing rubber ring 4, first cathode cavity 5, second cathode cavity 6, working electrode 7, cathode gas chamber 8, second heating plate 9, anode cavity 10, ion exchange membrane 11, counter electrode 12, sealing gasket 13, anode conductive copper column 14, cathode conductive copper column 15, reference electrode 16, cathode electrolyte circulation inlet and outlet 51, 52, opening 53, reference electrode mounting hole 54, connecting hole 61, gas flow channel 81, working electrode mounting hole 82, cathode reaction gas inlet and outlet 83, 84, anode electrolyte circulation inlet and outlet 101, 102, counter electrode mounting hole 103, serpentine flow channel 104. DETAILED DESCRIPTION

[0036] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer and more understandable, the present invention is further described in detail below with reference to the accompanying drawings and embodiments.

[0037] Example 1

[0038] The device of the invention comprises an in-situ reaction cell and an electrochemical workstation.

[0039] See also Figures 1 to 3 The in-situ reaction cell of the present invention comprises a first heating plate 1, a window cover 2, a sealing rubber ring 4, a light-transmitting sealing window 3, a first cathode cavity 5, a second cathode cavity 6, a cathode gas chamber 8 and a second heating plate 9, which are arranged in sequence from top to bottom;

[0040] An anode cavity 10 is provided on the side of the first cathode cavity 5. The interior of the first cathode cavity 5 is a cylindrical hollow structure with a threaded inner wall. An opening 53 is provided on the side of the first cathode cavity 5 to connect the hollow structure with the anode cavity 10. The light-transmitting sealing window 3 is covered on the hollow structure of the first cathode cavity 5.

[0041] The second cathode cavity 6 is a columnar structure, and its outer wall and inner wall are both provided with threads. The second cathode cavity 6 is placed in the lower part of the first cathode cavity 5 and is screwed to the first cathode cavity 5;

[0042] The cathode gas chamber 8 is a columnar structure with a threaded outer wall. The cathode gas chamber 8 is placed inside the second cathode cavity 6 and is screwed to the second cathode cavity 6.

[0043] The anode chamber 10 is provided with an anode electrolyte circulation inlet and outlet 101, 102; the first cathode chamber 5 is provided with a cathode electrolyte circulation inlet and outlet 51, 52; the cathode gas chamber 8 is provided with a cathode reaction gas inlet and outlet 83, 84, and a gas flow channel 81 connected to the second cathode chamber 6; the top of the second cathode chamber 6 is provided with a connecting hole 61;

[0044] The first heating plate 1 is provided at the upper portion of the first cathode cavity 5, and the second heating plate 9 is provided at the lower portion of the second cathode cavity 6;

[0045] This embodiment further includes a reference electrode 16, a counter electrode 12, a working electrode 7 and an ion exchange membrane 11;

[0046] One end of the reference electrode 16 is connected to the electrochemical workstation, and the other end is inserted into the hollow structure from the side of the first cathode cavity 5; the counter electrode 12 and the ion exchange membrane 11 are arranged between the anode cavity 10 and the first cathode cavity 5, and the ion exchange membrane 11 is close to the first cathode cavity 5, and the counter electrode 12 is connected to the electrochemical workstation through a conductive part inserted into the anode cavity 10; the working electrode 7 is arranged between the second cathode cavity 6 and the cathode gas chamber 8, and the cathode gas chamber 8 is made of conductive material. The working electrode 7 is connected to the chemical workstation through a conductive part inserted into the cathode gas chamber 8.

[0047] The sealing rubber ring 4 is arranged between the light-transmitting sealing window 3 and the window pressing cover 2 .

[0048] The anode chamber 10 and the first cathode chamber 5 are connected by bolts.

[0049] A serpentine flow channel 104 communicating with the anode electrolyte circulation inlet and outlet 101 , 102 is provided on the inner side of the anode cavity 10 , and the counter electrode 12 is located at the serpentine flow channel 104 .

[0050] The working electrode 7 includes a gas diffusion electrode, a glassy carbon electrode and a metal foil.

[0051] In this embodiment, the first cathode chamber 5, window gland 2, and connector are made of polyetheretherketone. The anode chamber 10 and cathode gas chamber 8 are made of titanium. The sealing gasket 13 is made of polytetrafluoroethylene, and the sealing rubber ring 4 is made of nitrile rubber. The heater is made of ceramic.

[0052] In this embodiment, the working electrode 7 is placed between the second cathode cavity 6 and the cathode gas chamber 8, and the fixing of the working electrode 7 and the sealing of the second cathode cavity 6 and the cathode gas chamber 8 are achieved by tightly screwing in the threads;

[0053] The second cathode cavity 6 and the first cathode cavity 5 are tightly screwed into the fitting threads to adjust the distance between the working electrode 7 and the light-transmitting sealing window 3 and seal the second cathode cavity 6 and the first cathode cavity 5;

[0054] A sealing gasket 13 is installed between the anode cavity 10 and the first cathode cavity 5, and a counter electrode 12 and an ion exchange membrane 11 are installed in the sealing gasket 13. The corresponding sealing screws are installed through the sealing screw holes on the anode cavity 10 and the first cathode cavity 5 to achieve a tight seal between the anode cavity 10 and the first cathode cavity 5.

[0055] Specifically, the anode cavity 10 is provided with an electrode mounting hole 103 and a sealing screw hole. The anode electrolyte circulating liquid inlet and outlet 101, 102 are screwed into the joints, and the pipeline is connected to realize electrolyte circulation; the anode conductive copper column 14 is installed in the electrode mounting hole 103 and is conductively connected to the electrode 12 to realize the conductivity of the anode electrode 12 and the sealing of the electrode mounting hole 103.

[0056] The first cathode chamber 5 is provided with a reference electrode mounting hole 54 and a mounting slot; the reference electrode mounting hole 54 communicates with the hollow structure. The reference electrode 16 is wrapped with sealing tape and screwed into the first cathode chamber 5 for installation and sealing. The mounting slot is stepped. First, the light-transmitting sealing window 3 is installed and a sealing rubber ring 4 is placed on top of the light-transmitting sealing window 3. Finally, the window gland 2 is installed to complete the installation and sealing of the light-transmitting sealing window 3. The cathode electrolyte circulation inlet and outlet 51 and 52 are screwed into the joints and connected to the pipeline to achieve electrolyte circulation.

[0057] The cathode gas chamber 8 defines a working electrode mounting hole 82. Cathode reactant gas inlet and outlet ports 83 and 84 are screwed into connectors and connected to pipelines to allow the introduction of reactant gas. The gas flow channel 81 is arranged in a serpentine shape and communicates with the cathode reactant gas inlet and outlet ports 83 and 84. A cathode conductive copper post 15 is inserted into the working electrode mounting hole 82 and electrically connected to the working electrode 7, ensuring conductivity of the cathode working electrode 7 and sealing of the working electrode mounting hole 82.

[0058] Example 2

[0059] In situ XRD Detection of Electrocatalytic CO2 Reduction on Gas Diffusion Electrodes

[0060] The reference electrode is an Ag / AgCl electrode, the counter electrode is iridium oxide with a sintered coating, the working electrode is a catalyst layer / glassy carbon electrode, and the ion exchange membrane is an anion exchange membrane.

[0061] The assembled in-situ flow reaction cell was placed in the in-situ X-ray diffractometer sampling area. The second cathode cavity was rotated to control the distance between the working electrode and the light-transmitting sealing window (polyimide film) to be 1 mm. The temperature of the electrolytic cell was controlled at 20-80 °C using a heating plate. CO2 gas was introduced into the cathode gas chamber at a gas flow rate of 10-50 mL min -1 The electrolytes in the anode and cathode chambers are both 0.1 to 2 mol L -1 KOH or 0.1-1 mol L -1KHCO3, with a volume of 5-50 mL, was circulated in the two electrodes using a peristaltic pump at a liquid flow rate of 5-20 mL min -1 The anode conductive copper cylinder, cathode conductive copper cylinder, and Ag / AgCl reference electrode were connected to the electrochemical workstation using banana clips for the counter electrode, working electrode, and reference electrode, respectively. The applied potential for electrocatalytic testing was 0 to -5.0 V (vs. Ag / AgCl). The electrode surface was observed through a polyimide membrane, and X-ray diffraction spectra were collected during the electrocatalytic process. X-ray diffractometer parameters were: target: copper palladium, voltage: 40 kV, current: 40 A.

[0062] Example 3

[0063] In situ synchrotron radiation detection of electrocatalytic carbon dioxide reduction at gas diffusion electrodes

[0064] The detection method is the same as that in Example 2. The instrument used is a synchrotron radiation spectroscopy line station, and the relevant parameters are: the excitation energy range is 4k to 20keV.

[0065] Example 4

[0066] In situ Raman Detection of Electrocatalytic CO2 Reduction on Glassy Carbon Electrodes

[0067] The reference electrode is an Ag / AgCl electrode, the counter electrode is iridium oxide with a sintered coating, the working electrode is a catalyst layer / carbon-based gas diffusion electrode, and the ion exchange membrane is an anion exchange membrane.

[0068] The assembled in-situ flow reaction cell was placed in the sample measurement area of ​​the in-situ Raman spectrometer. The reaction temperature was controlled at 0-90°C. The second cathode cavity was rotated to control the distance between the working electrode and the light-transmitting sealing window (quartz window) to be 0.3 mm. The first cathode cavity was filled with 0.1-3 mol L CO gas. -1 KOH electrolyte, the electrolyte in the anode chamber is 0.1~3 mol L - 1 KOH, with a volume of 20 mL, was circulated in the two electrodes using a peristaltic pump at a liquid flow rate of 5 to 20 mL min -1 The anode conductive copper cylinder, cathode conductive copper cylinder, and Ag / AgCl reference electrode were connected to the electrochemical workstation using banana clips for the counter electrode, working electrode, and reference electrode, respectively. The applied potential for electrocatalytic testing was 0 to -5.0 V (vs. Ag / AgCl). The electrode surfaces were observed through quartz windows, and X-ray diffraction spectra were collected during the electrocatalytic process. Relevant parameters included Raman laser wavelengths of 266 nm, 532 nm, 633 nm, 785 nm, 830 nm, and 1064 nm.

[0069] The present invention realizes the integration of multiple in-situ characterization devices with different functions, and the distance between the working electrode and the light-transmitting sealing window can be adjusted within a wide range.

[0070] The device of the present invention has excellent gas-liquid sealing. The anode cavity and the first cathode cavity are sealed by a threaded fit and a sealing gasket structure. The working electrode is secured and sealed by a spiral structure that fits between the two cathode cavities. Different window materials can be selected for different in-situ characterizations. The combination of the anode cavity and the sealing rubber ring ensures a gas-liquid seal for the light-transmitting sealing window.

Claims

1. A multifunctional flow-type in-situ spectral detection device for electrocatalytic reactions, characterized by: It includes an in-situ reaction cell and an electrochemical workstation; the in-situ reaction cell includes a first heating plate, a light-transmitting sealing window, a first cathode cavity, a second cathode cavity, a cathode gas chamber and a second heating plate, which are arranged in sequence from top to bottom; An anode cavity is provided on the side of the first cathode cavity. The interior of the first cathode cavity is a cylindrical hollow structure with a threaded inner wall. An opening is provided on the side of the first cathode cavity to connect the hollow structure with the anode cavity. The light-transmitting sealing window cover is provided on the hollow structure of the first cathode cavity. The second cathode cavity is a columnar structure, with threads on both the outer and inner walls. The second cathode cavity is placed in the lower part of the first cathode cavity and is screwed to the first cathode cavity. The cathode gas chamber is a columnar structure with a threaded outer wall. The cathode gas chamber is placed inside the second cathode cavity and is screwed to the second cathode cavity. The anode cavity is provided with an anode electrolyte circulation inlet and outlet; the first cathode cavity is provided with a cathode electrolyte circulation inlet and outlet; the cathode gas chamber is provided with a cathode reaction gas inlet and outlet, and a gas flow channel connected to the second cathode cavity; the top of the second cathode cavity is provided with a connecting hole; The first heating plate is arranged at the upper part of the first cathode cavity, and the second heating plate is arranged at the lower part of the second cathode cavity; It also includes a reference electrode, a counter electrode, a working electrode, and an ion exchange membrane; One end of the reference electrode is connected to the electrochemical workstation, and the other end is inserted into the hollow structure from the side of the first cathode cavity; the counter electrode and the ion exchange membrane are arranged between the anode cavity and the first cathode cavity, and the ion exchange membrane is close to the first cathode cavity, and the counter electrode is connected to the electrochemical workstation through a conductive part inserted into the anode cavity; the working electrode is arranged between the second cathode cavity and the cathode gas chamber, and the cathode gas chamber is made of conductive material, and the working electrode is connected to the chemical workstation through a conductive part inserted into the cathode gas chamber.

2. The multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction according to claim 1, characterized in that: It also includes a window cover and a sealing rubber ring, wherein the sealing rubber ring is arranged between the light-transmitting sealing window and the window cover.

3. The multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction according to claim 1, characterized in that: The invention also includes a sealing gasket, which is arranged between the first cathode cavity and the anode cavity.

4. The multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction according to claim 1, characterized in that: The anode cavity and the first cathode cavity are connected by bolts.

5. The multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction according to claim 1, characterized in that: A serpentine flow channel communicating with the anode electrolyte circulation inlet and outlet is provided on the inner side of the anode cavity, and the counter electrode is located at the serpentine flow channel.

6. The multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction according to claim 1, characterized in that: The cathode gas chamber is made of titanium or stainless steel.

7. The multifunctional flow-type in-situ spectral detection device for electrocatalytic reaction according to claim 1, characterized in that: The working electrode includes a gas diffusion electrode, a glassy carbon electrode and a metal foil.

8. The use of the multifunctional flow-type in-situ spectral detection device for electrocatalytic reactions according to claim 1, characterized in that: The in-situ reaction cell is connected to the in-situ spectrometer. The distance between the working electrode and the light-transmitting sealing window is adjusted by rotating the second cathode cavity. Voltage and current are applied through the electrochemical workstation, and the in-situ spectrometer is used to collect spectral signals during the electrocatalytic reaction.

9. The use according to claim 8, characterized in that: The spectral signals include X-ray diffraction spectral signals, synchrotron radiation spectral signals or Raman spectral signals to meet different in-situ characterization requirements.

Images