Electrochemical reaction tank for in-situ Raman test and use method of electrochemical reaction tank

Abstract

The invention belongs to the technical field of in-situ Raman testing, and particularly discloses an electrochemical reaction tank for in-situ Raman testing and a use method thereof.The electrochemical reaction tank comprises a cathode chamber, a sealing ring is mounted in the cathode chamber, a cover plate is mounted on the cathode chamber, a first sealing gasket is embedded in the cover plate, and a second sealing gasket is mounted on the first sealing gasket. The window sealing cover, the quartz window and the annular sealing ring are tightly mounted on the cell cover to form an efficient sealing structure for an optical path, so that electrolyte leakage can be effectively avoided, the problems of equipment corrosion, experimental pollution and the like caused by electrolyte overflow are prevented, the safety of experimental operation is guaranteed, and meanwhile, the service life of the experimental device is prolonged. External impurities can be prevented from entering the device, the interference of the impurities on electrochemical reaction and Raman spectrum test is avoided, a pure and stable reaction environment is provided for experiments, and the accuracy and reliability of subsequent electrochemical reaction and spectrum monitoring are fundamentally ensured.

Description

Technical Field

[0001] The present invention belongs to the technical field of in-situ Raman testing, and in particular relates to an electrochemical reaction cell for in-situ Raman testing and a method for using the same. Background Art

[0002] The combination of in-situ Raman spectroscopy and an electrochemical reaction cell is an important experimental device for real-time monitoring of molecular structural changes during electrochemical reactions. By coupling the electrochemical system with Raman spectroscopy, it enables in-situ characterization of reaction intermediates, products, and interfacial processes on the electrode surface.

[0003] Existing reaction cells have shortcomings in meeting various experimental conditions and adapting to Raman testing. For example, they are unable to simultaneously achieve atmosphere introduction and solution circulation at room temperature and pressure. In addition, the window design and electrode configuration cannot well meet the in-situ Raman testing requirements of supported catalyst research, limiting the application and development of this technology in related fields. Summary of the Invention

[0004] The object of the present invention is to provide an electrochemical reaction cell for in-situ Raman testing and a method of using the same, so as to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] An electrochemical reaction cell for in-situ Raman testing includes a cathode chamber, a sealing ring is installed inside the cathode chamber, a cover plate is installed on the cathode chamber, a first sealing gasket is embedded on the cover plate, a second sealing gasket is provided on the first sealing gasket, a first proton exchange membrane, carbon paper and copper foil tape are provided between the first sealing gasket and the second sealing gasket, a cell cover is installed on the cover plate, a ventilation mechanism is provided inside the cell cover, the ventilation mechanism includes an air chamber arranged inside the cell cover, an annular sealing ring is provided inside the air chamber, an air outlet and an air inlet are opened inside the air chamber, a quartz window is installed inside the air chamber, a window sealing cover is fixedly connected to the cell cover, and the window sealing cover presses and fixes the quartz window.

[0007] Preferably, the side wall of the cathode chamber is connected to the anode chamber, the anode chamber is provided with a liquid inlet, the anode chamber is provided with two anode and cathode sealing gaskets, and a proton exchange membrane is sandwiched between the two anode and cathode sealing gaskets.

[0008] Preferably, a large plug is installed on the cathode chamber, and a large plug annular ring is sleeved on the large plug.

[0009] Preferably, a platinum wire electrode is inserted into the interior of the anode chamber, a small plug is provided on the platinum wire electrode, and an annular ring is provided on the small plug.

[0010] Preferably, a silver chloride electrode is inserted into the cathode chamber, a second annular ring and an electrode sleeve are sleeved on the silver chloride electrode, and the second annular ring is located inside the electrode sleeve.

[0011] Preferably, the quartz window is made of high-purity quartz glass in one piece, and the diameter of the quartz window is 37 mm.

[0012] Preferably, an observation port is provided inside the air chamber, the observation port is square, and the size of the observation port is 15 mm×15 mm.

[0013] A method for using an electrochemical reaction cell for in-situ Raman testing, the method comprising the following steps:

[0014] S1: When using, first install the window sealing cover, quartz window and annular sealing ring tightly to the cell cover to prevent electrolyte leakage or interference from external impurities and ensure the sealing of the optical path. Then install the external liquid inlet connector at the liquid inlet hole, and install the air inlet component and air outlet component at the air inlet hole and air outlet hole respectively to ensure that the pipeline is unobstructed and leak-free, laying the foundation for subsequent solution circulation and atmosphere introduction.

[0015] S2: After all installation work is completed, you can insert the silver chloride electrode and the large plug into the cathode chamber, insert the platinum wire electrode into the anode chamber, and then connect the external working electrode at the copper foil tape. After the three electrodes are installed, adjust the distance between the external working electrode and the platinum wire electrode to be greater than or equal to six millimeters to optimize the electric field distribution between the electrodes and improve the test accuracy.

[0016] S3: After all preparations are completed, the appropriate electrolyte can be prepared according to the experimental requirements and injected into the anode chamber through the liquid inlet connector. The static no-circulation mode or dynamic start-up circulation mode can be selected according to the needs. In the dynamic mode, the circulation system needs to be started to ensure the stability of the reaction system.

[0017] S4: After the above work is completed, the Raman testing instrument works synchronously, the laser irradiates the sample surface, collects the Raman scattered light generated during the reaction, and obtains Raman spectrum data through spectrometer analysis to monitor the changes in the molecular structure in the reaction system in real time. During the test, the atmosphere type, flow rate, electrolyte circulation rate or electrochemical parameters can be dynamically adjusted according to the experimental design, and the Raman spectra under different conditions can be recorded synchronously to achieve multi-dimensional analysis of the electrochemical reaction mechanism.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1. By tightly installing the window sealing cover, quartz window and annular sealing ring on the cell cover, an efficient sealing structure for the optical path is formed. This design can effectively prevent electrolyte leakage, prevent equipment corrosion and experimental contamination caused by electrolyte overflow, and ensure the safety of experimental operation. At the same time, it can isolate external impurities from entering the device, avoiding impurities from interfering with electrochemical reactions and Raman spectroscopy testing, providing a pure and stable reaction environment for the experiment, and fundamentally ensuring the accuracy and reliability of subsequent electrochemical reactions and spectral monitoring.

[0020] 2. By inserting a silver chloride electrode into the cathode chamber and a platinum wire electrode into the anode chamber, and connecting an external working electrode at the copper foil tape, and adjusting the distance between the external working electrode and the platinum wire electrode to be greater than or equal to six millimeters, this electrode installation method effectively optimizes the electric field distribution between the electrodes. The uniform electric field distribution can reduce interference between the electrodes, making the electrochemical reaction more uniform and stable, thereby improving the accuracy of the test and providing strong support for the precise study of the electrochemical reaction mechanism.

[0021] 3. The entire device can be operated in either static (no circulation) or dynamic (circulation) electrolyte modes depending on experimental requirements. In dynamic mode, the circulation system is activated to promptly replenish the electrolyte consumed by the reaction and remove the reaction products, ensuring the stability of the reaction system. This avoids problems such as reaction rate fluctuations caused by changes in electrolyte composition, making it suitable for experiments with demanding reaction conditions and broadening the device's application range. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a disassembled structural diagram of the present invention;

[0023] Figure 2 This is a partial disassembled structural diagram of the present invention;

[0024] Figure 3 This is a structural diagram of the installation state of the present invention;

[0025] Figure 4 This is a structural diagram of the large plug of the present invention;

[0026] Figure 5 This is a structural diagram of the silver chloride electrode and the small plug of the present invention;

[0027] Figure 6 It is a structural diagram of the silver chloride electrode of the present invention.

[0028] In the figure; 1, cathode chamber; 2, sealing ring; 3, cover plate; 4, first sealing gasket; 5, second sealing gasket; 6, copper foil tape; 7, cell cover; 8, window sealing cover; 9, quartz window; 10, anode chamber; 11, cathode and anode sealing gaskets; 12, annular sealing ring; 13, proton exchange membrane; 14, platinum wire electrode; 15, annular ring; 16, silver chloride electrode; 17, second annular ring; 18, electrode sleeve; 19, large plug annular ring; 20, small plug; 21, large plug; 22, carbon paper; 23, first proton exchange membrane; 24, air outlet; 25, air inlet; 26, liquid inlet; 27, gas chamber; 28, observation port. DETAILED DESCRIPTION

[0029] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0030] Example 1, refer to Figure 1-6 , an electrochemical reaction cell for in-situ Raman testing, comprising a cathode chamber 1, a sealing ring 2 is installed inside the cathode chamber 1, a cover plate 3 is installed on the cathode chamber 1, a first sealing gasket 4 is embedded on the cover plate 3, a second sealing gasket 5 is provided on the first sealing gasket 4, a first proton exchange membrane 23, carbon paper 22 and copper foil tape 6 are provided between the first sealing gasket 4 and the second sealing gasket 5, a cell cover 7 is installed on the cover plate 3, a ventilation mechanism is provided inside the cell cover 7, the ventilation mechanism includes an air chamber 27 arranged inside the cell cover 7, an annular sealing ring 12 is provided inside the air chamber 27, an air outlet 24 and an air inlet 25 are opened inside the air chamber 27, a quartz window 9 is installed inside the air chamber 27, a window sealing cover 8 is fixedly connected to the cell cover 7, and the window sealing cover 8 presses and fixes the quartz window 9.

[0031] The side wall of the cathode chamber 1 is connected to the anode chamber 10 . The anode chamber 10 is provided with a liquid inlet 26 . The anode chamber 10 is provided with two anode and cathode sealing gaskets 11 . A proton exchange membrane 13 is sandwiched between the two anode and cathode sealing gaskets 11 .

[0032] In this embodiment, when in use, first install the window sealing cover 8, the quartz window 9 and the annular sealing ring 12 tightly on the pool cover 7 to avoid leakage of electrolyte or interference from external impurities and ensure the sealing of the optical path. Then install the external liquid inlet joint at the liquid inlet hole 26, and install the air inlet component and the air outlet component at the air inlet hole 25 and the air outlet hole 24 respectively to ensure that the pipeline is unobstructed and leak-free, laying the foundation for subsequent solution circulation and atmosphere introduction. When all the installation work is completed, the silver chloride electrode 16 can be inserted into the cathode chamber 1 and the silver chloride electrode 16 can be inserted into the anode chamber. 10, and then connect the external working electrode at the copper foil tape 6. After the three electrodes are installed, adjust the distance between the external working electrode and the platinum wire electrode 14 to be greater than or equal to six millimeters to optimize the electric field distribution between the electrodes and improve the test accuracy. When all preparations are completed, the appropriate electrolyte can be configured according to the experimental requirements, and the electrolyte can be injected into the anode chamber 10 through the liquid inlet connector. The static (no circulation) or dynamic (circulation) mode can be selected according to the needs. In the dynamic mode, the circulation system needs to be started to ensure the stability of the reaction system.

[0033] Example 2, refer to Figure 1-6 A large plug 21 is installed on the cathode chamber 1, and a large plug annular ring 19 is sleeved on the large plug 21.

[0034] A platinum wire electrode 14 is inserted into the anode chamber 10 . A small plug 20 is provided on the platinum wire electrode 14 . An annular ring 15 is provided on the small plug 20 .

[0035] A silver chloride electrode 16 is inserted into the cathode chamber 1 . A second annular ring 17 and an electrode sleeve 18 are sleeved on the silver chloride electrode 16 . The second annular ring 17 is located inside the electrode sleeve 18 .

[0036] The quartz window 9 is made of high-purity quartz glass in one piece, and the diameter of the quartz window 9 is 37 mm.

[0037] An observation port 28 is provided inside the air chamber 27 . The observation port 28 is square in shape and has a size of 15 mm×15 mm.

[0038] In this embodiment, if atmosphere is required during the experiment, the operator can introduce a fixed amount of atmosphere into the cathode chamber 1 and the anode chamber 10 through the air inlet 25. Finally, a sample to be tested (20 mm × 20 mm or larger) is placed at the observation port 28. The laser focus position of the Raman test instrument is adjusted so that the laser accurately irradiates the sample surface through the quartz window 9. Instrument parameters such as laser wavelength, power, and integration time are calibrated to ensure the stability of the test signal. Then, a three-electrode electrochemical workstation is connected, and parameters such as the working electrode potential and current density are set. The electrochemical reaction is initiated. At this time, an electric field is formed in the cathode chamber 1 and the anode chamber 10, promoting ion migration and electrochemical reaction in the electrolyte. At this time, the Raman test instrument operates synchronously, irradiating the sample surface with laser light, collecting Raman scattered light generated during the reaction, and analyzing it with a spectrometer to obtain Raman spectral data, thereby monitoring changes in the molecular structure of the reaction system in real time. During the test, the atmosphere type, flow rate, electrolyte circulation rate, or electrochemical parameters can be dynamically adjusted according to the experimental design, and Raman spectra under different conditions can be simultaneously recorded to achieve multi-dimensional analysis of the electrochemical reaction mechanism.

[0039] A method for using an electrochemical reaction cell for in-situ Raman testing, the method comprising the following steps:

[0040] S1: When using, first install the window sealing cover 8, quartz window 9 and annular sealing ring 12 tightly on the cell cover 7 to prevent electrolyte leakage or interference from external impurities and ensure the sealing of the optical path. Then install the external liquid inlet connector at the liquid inlet hole 26, and install the air inlet component and the air outlet component at the air inlet hole 25 and the air outlet hole 24 respectively to ensure that the pipeline is unobstructed and leak-free, laying the foundation for subsequent solution circulation and atmosphere introduction.

[0041] S2: After all installation work is completed, the silver chloride electrode 16 and the large plug 21 can be inserted into the cathode chamber 1, and the platinum wire electrode 14 can be inserted into the anode chamber 10. Then, the external working electrode can be connected at the copper foil tape 6. After the three electrodes are installed, the distance between the external working electrode and the platinum wire electrode 14 is adjusted to be greater than or equal to 6 mm to optimize the electric field distribution between the electrodes and improve the test accuracy.

[0042] S3: After all preparations are completed, appropriate electrolyte can be prepared according to experimental requirements and injected into the anode chamber 10 through the liquid inlet connector. Static no-circulation mode or dynamic start-up circulation mode can be selected according to needs. In the dynamic mode, the circulation system needs to be started to ensure the stability of the reaction system.

[0043] S4: After the above work is completed, the Raman testing instrument works synchronously, the laser irradiates the sample surface, collects the Raman scattered light generated during the reaction, and obtains Raman spectrum data through spectrometer analysis to monitor the changes in the molecular structure in the reaction system in real time. During the test, the atmosphere type, flow rate, electrolyte circulation rate or electrochemical parameters can be dynamically adjusted according to the experimental design, and the Raman spectra under different conditions can be recorded synchronously to achieve multi-dimensional analysis of the electrochemical reaction mechanism.

[0044] It should be noted that the external liquid inlet head is a 1 / 8in quick-connect.

[0045] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. An electrochemical reaction cell for in-situ Raman testing, comprising a cathode chamber (1), characterized in that: A sealing ring (2) is installed inside the cathode chamber (1), a cover plate (3) is installed on the cathode chamber (1), a first sealing gasket (4) is embedded on the cover plate (3), a second sealing gasket (5) is provided on the first sealing gasket (4), a first proton exchange membrane (23), carbon paper (22) and copper foil tape (6) are provided between the first sealing gasket (4) and the second sealing gasket (5), a pool cover (7) is installed on the cover plate (3), and the pool cover (7) A ventilation mechanism is provided inside the pool cover (7), the ventilation mechanism includes an air chamber (27) provided inside the pool cover (7), an annular sealing ring (12) is provided inside the air chamber (27), an air outlet (24) and an air inlet (25) are provided inside the air chamber (27), a quartz window (9) is installed inside the air chamber (27), a window sealing cover (8) is fixedly connected to the pool cover (7), and the window sealing cover (8) presses and fixes the quartz window (9).

2. The electrochemical reaction cell for in-situ Raman testing according to claim 1, characterized in that: The side wall of the cathode chamber (1) is connected to an anode chamber (10), a liquid inlet hole (26) is provided on the anode chamber (10), two anode and cathode sealing gaskets (11) are provided on the anode chamber (10), and a proton exchange membrane (13) is sandwiched between the two anode and cathode sealing gaskets (11).

3. The electrochemical reaction cell for in-situ Raman testing according to claim 1, characterized in that: A large plug (21) is installed on the cathode chamber (1), and a large plug annular ring (19) is sleeved on the large plug (21).

4. The electrochemical reaction cell for in-situ Raman testing according to claim 2, characterized in that: A platinum wire electrode (14) is inserted into the interior of the anode chamber (10), a small plug (20) is provided on the platinum wire electrode (14), and an annular ring (15) is provided on the small plug (20).

5. The electrochemical reaction cell for in-situ Raman testing according to claim 1, characterized in that: A silver chloride electrode (16) is inserted into the cathode chamber (1), a second annular ring (17) and an electrode sleeve (18) are sleeved on the silver chloride electrode (16), and the second annular ring (17) is located inside the electrode sleeve (18).

6. The electrochemical reaction cell for in-situ Raman testing according to claim 1, characterized in that: The quartz window (9) is made of high-purity quartz glass in an integrated manner, and the diameter of the quartz window (9) is 37 mm.

7. The electrochemical reaction cell for in-situ Raman testing according to claim 1, characterized in that: An observation port (28) is provided inside the air chamber (27). The observation port (28) is square in shape and has a size of 15 mm×15 mm.

8. The method for using the electrochemical reaction cell for in-situ Raman testing according to any one of claims 1 to 7, characterized in that: The method includes the following steps: S1: When using, first tightly install the window sealing cover (8), quartz window (9) and annular sealing ring (12) on the pool cover (7) to avoid electrolyte leakage or interference from external impurities and ensure the sealing of the optical path. Then install the external liquid inlet connector at the liquid inlet hole (26), and install the air inlet component and the air outlet component at the air inlet hole (25) and the air outlet hole (24) respectively to ensure that the pipeline is unobstructed and leak-free, laying the foundation for subsequent solution circulation and atmosphere introduction; S2: After all installation work is completed, the silver chloride electrode (16) and the large plug (21) can be inserted into the cathode chamber (1), and the platinum wire electrode (14) can be inserted into the anode chamber (10). Then, the external working electrode is connected at the copper foil tape (6). After the three electrodes are installed, the distance between the external working electrode and the platinum wire electrode (14) is adjusted to be greater than or equal to six millimeters to optimize the electric field distribution between the electrodes and improve the test accuracy. S3: After all preparations are completed, appropriate electrolyte can be prepared according to the experimental requirements, and the electrolyte can be injected into the anode chamber (10) through the liquid inlet connector. The static no-circulation mode or the dynamic open circulation mode can be selected according to the needs. In the dynamic mode, the circulation system needs to be started to ensure the stability of the reaction system; S4: After the above work is completed, the Raman testing instrument works synchronously, the laser irradiates the sample surface, collects the Raman scattered light generated during the reaction, and obtains Raman spectrum data through spectrometer analysis to monitor the changes in the molecular structure in the reaction system in real time. During the test, the atmosphere type, flow rate, electrolyte circulation rate or electrochemical parameters can be dynamically adjusted according to the experimental design, and the Raman spectra under different conditions can be recorded synchronously to achieve multi-dimensional analysis of the electrochemical reaction mechanism.

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