An electrochemical cell device for in-situ infrared spectroscopy testing

Abstract

This invention discloses an electrochemical cell device for in-situ infrared spectroscopy testing, relating to the field of electrochemical technology. The main body has an opening on one side connected to a side cover, forming a receiving groove between the main body and the side cover. The upper end of the receiving groove is open and closed by a top cover. Sealing rings seal the main body and the side cover, the main body and the top cover, and the side cover and the top cover. The top cover has mounting holes and vent holes, both connecting the receiving groove to the outside. A window channel is provided on the side of the main body near the side cover, and on the side cover near the main body, connecting the receiving groove to the outside. The two window channels are coaxially arranged, and the space between them is used to place the sample to be tested. A gasket is located between the window channel and the sample to be tested. A substrate is located between the two window channels and is used to connect to the working electrode rod. This invention is simple to install, flexible, easy to clean, and has good sealing performance.

Description

Technical Field

[0001] This invention relates to the field of electrochemical technology, specifically to an electrochemical cell device for in-situ infrared spectroscopy testing. Background Technology

[0002] Catalysts are one of the key materials in fuel cells. The catalytic performance of a catalyst directly affects the energy conversion efficiency of the fuel cell. Scientists worldwide are continuously developing and researching catalyst materials that combine low cost, high activity, and high stability. In studying the catalytic performance of catalysts, it is usually necessary to delve into key information such as changes in electronic structure and catalytic kinetics during the catalytic process. Adsorption / desorption products and electron transfer processes on the catalyst surface can occur on a timescale ranging from femtoseconds to picoseconds, which can be obtained using two-dimensional infrared spectroscopy (2D-IR). 2D-IR spectroscopy uses a series of femtosecond infrared laser pulses to detect changes in the molecular structure of the catalyst surface from fs to ps, thereby allowing the study of reaction kinetics occurring on this timescale. This is of great significance for exploring catalytic mechanisms and optimizing catalyst structures.

[0003] Because infrared light attenuates significantly in water, in-situ infrared spectroscopy testing of electrochemical reactions (such as the oxygen reduction reaction (ORR) at the cathode of a hydrogen fuel cell) in aqueous solutions of certain concentrations of perchloric acid, sulfuric acid, or sodium hydroxide requires a very compact infrared window design. Infrared spectroscopy testing modes can be broadly categorized into transmission and reflection modes, but regardless of the mode, the total thickness of the aqueous solution through which the infrared light passes should ideally be less than 200 μm. Summary of the Invention

[0004] The purpose of this invention is to provide an electrochemical cell device for in-situ infrared spectroscopy testing, which solves the problems existing in the prior art, and is simple to install, flexible, easy to clean, and has good sealing performance.

[0005] To achieve the above objectives, the present invention provides the following solution:

[0006] This invention provides an electrochemical cell device for in-situ infrared spectroscopy testing, comprising a body, a top cover, a side cover, a gasket, and a substrate. One side of the body is open and connected to the side cover, forming a receiving groove between the body and the side cover. The upper end of the receiving groove is open and closed by the top cover. Sealing rings are used to seal the body and the side cover, the body and the top cover, and the side cover and the top cover. The top cover has a mounting hole and a vent hole, both of which connect the receiving groove to the outside. A window channel is provided on the side of the body near the side cover, and on the side cover near the body, both connecting the receiving groove to the outside. Two window channels are coaxially arranged, and a sample to be tested is placed between the two window channels. The gasket is located between the window channel and the sample to be tested. The substrate is located between the two window channels and is used to connect to the working electrode rod.

[0007] Preferably, the body and the side cover are connected by bolts.

[0008] Preferably, the top cover and the body, as well as the top cover and the side cover, are connected by bolts.

[0009] Preferably, there are three mounting holes, and the mounting holes are respectively used to install the working electrode rod, the reference electrode rod, and the counter electrode rod. The vent hole includes an air inlet and an air outlet, and the air inlet is used to install an air inlet pipe, and the air outlet is used to install an air outlet pipe.

[0010] Preferably, each of the two window channels has a window on one side that is close to each other, and the window is made of calcium fluoride single crystal material.

[0011] Preferably, the gasket is an annular shape with a notch, and the gasket is made of Teflon material.

[0012] Preferably, the accommodating tank contains an electrolyte, and a conductive layer is provided on the area of ​​the substrate that is not in contact with the electrolyte.

[0013] Preferably, the conductive layer is a metal layer.

[0014] Preferably, the substrate is made of calcium fluoride material.

[0015] Preferably, the body, the top cover, and the side cover are all made of polytetrafluoroethylene or PEEK material.

[0016] The present invention achieves the following technical effects compared to the prior art:

[0017] The electrochemical cell device for in-situ infrared spectroscopy testing provided by this invention has an opening on one side of the main body connected to a side cover, forming a receiving groove between the main body and the side cover. The upper end of the receiving groove is open and closed by a top cover. Sealing rings are used to seal the main body and the side cover, the main body and the top cover, and the side cover and the top cover, ensuring good sealing. The top cover has mounting holes and vent holes, both of which connect the receiving groove to the outside. A window channel is provided on the side of the main body near the side cover, and on the side cover near the main body, both connecting the receiving groove to the outside. The two window channels are coaxially arranged, and the space between the two window channels is used to place the sample to be tested. The areas on both sides of the window channels... The region is used to place the reference electrode and the counter electrode. The cross-section of the receiving groove is H-shaped, and the space on both sides of the window channel is larger than the space inside the window channel to accommodate reference electrodes and counter electrodes of conventional size and to accommodate a larger volume of electrolyte. The structure is simple, easy to install and clean. The gasket is located between the window channel and the sample to be tested. By adjusting the thickness of the gasket, the distance between the sample to be tested and the window can be adjusted so that the total thickness of the liquid layer through which infrared light passes does not exceed 100μm, which is flexible. The substrate is located between the two window channels and is used to connect to the working electrode rod to realize current transmission. By changing different substrates, the transmission mode and the reflection mode can be switched. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the electrochemical cell device for in-situ infrared spectroscopy testing provided by the present invention.

[0020] Figure 2 This is an exploded view of the electrochemical cell device for in-situ infrared spectroscopy testing provided by the present invention from one angle. Figure 3 This is an exploded view of the electrochemical cell device for in-situ infrared spectroscopy testing provided by the present invention from another angle. Figure 4 This is an exploded view of the electrochemical cell device for in-situ infrared spectroscopy testing provided by the present invention; Figure 5 This is a cross-sectional view of the electrochemical cell device for in-situ infrared spectroscopy testing provided by the present invention;

[0021] In the figure: 1-body, 2-top cover, 3-side cover, 4-gasket, 5-base, 6-sealing ring, 7-mounting hole, 8-window channel, 9-sample to be tested, 10-working electrode rod, 11-air inlet, 12-exhaust outlet, 13-window, 14-electrolyte. Detailed Implementation

[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] The purpose of this invention is to provide an electrochemical cell device for in-situ infrared spectroscopy testing, so as to solve the technical problems of existing infrared spectroscopy testing devices being complex in structure, inconvenient to install, and inconvenient to clean.

[0024] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0025] like Figures 1-5 As shown, this embodiment provides an electrochemical cell device for in-situ infrared spectroscopy testing, including a body 1, a top cover 2, a side cover 3, a gasket 4, and a substrate 5. One side of the body 1 is open and connected to the side cover 3, and a receiving groove is formed between the body 1 and the side cover 3. The upper end of the receiving groove is open and closed by the top cover 2. The body 1 and the side cover 3, the body 1 and the top cover 2, and the side cover 3 and the top cover 2 are all sealed by sealing rings 6, providing good sealing performance. The top cover 2 is provided with mounting holes 7 and vent holes, both of which can connect the receiving groove to the outside. A window channel 8 is provided on the side of the body 1 near the side cover 3 and on the side cover 3 near the body 1, respectively. The window channel 8 can connect the receiving groove to the outside. The two window channels 8 are coaxially arranged and connected by a gasket. The sample 9 is placed in the window channel 8. The areas on both sides of the window channel 8 are used to place the reference electrode and the counter electrode. The cross-section of the receiving groove is H-shaped, and the space on both sides of the window channel 8 is larger than the space inside the window channel 8 to accommodate reference electrodes and counter electrodes of conventional size and to accommodate a larger volume of electrolyte. The structure is simple, easy to install and clean. The gasket 4 is located between the window channel 8 and the sample 9. By adjusting the thickness of the gasket 4, the distance between the sample 9 and the window 13 can be adjusted so that the total thickness of the liquid layer through which infrared light passes does not exceed 100μm. It has good flexibility. The substrate 5 is located between the two window channels 8 and is used to connect with the working electrode rod 10 to realize current transmission. By changing different substrates 5, the transmission mode and the reflection mode can be switched.

[0026] Specifically, the main body 1 and the side cover 3 are connected by bolts. The top cover 2 is also connected to the main body 1, and the top cover 2 is connected to the side cover 3 by bolts, which facilitates installation and disassembly and ensures stable connection.

[0027] There are three mounting holes 7, which are used to install the working electrode rod 10, the reference electrode rod, and the counter electrode rod, respectively. The three mounting holes 7 are arranged in a straight line, so that after installation, the working electrode is located between the two window channels 8, and the reference electrode and the counter electrode are located on both sides of the window channel 8. The venting holes include an inlet hole 11 and an outlet hole 12. The inlet hole 11 is used to install an inlet pipe, and the outlet hole 12 is used to install an outlet pipe, which can realize the introduction and discharge of gases such as oxygen and nitrogen. In actual use, electrolyte input and output pipelines can also be designed on the device according to experimental needs.

[0028] Each of the two window channels 8 has a window 13 on one side that is close to each other. The window 13 is made of calcium fluoride single crystal material. The diameter of the window channel 8 and the window 13 can be designed as needed.

[0029] The gasket 4 is a ring with a notch and is made of Teflon material. The notch design ensures that the sample surface is immersed in the electrolyte 14 solution.

[0030] The container contains electrolyte 14. In order to ensure that the sample 9 to be tested can achieve good conductivity with the working electrode rod 10, the working electrode rod 10 and the sample 9 to be tested can be connected by a clamping method. Alternatively, a conductive layer can be provided on the substrate 5 in the area that does not contact the electrolyte 14. The conductive layer can be a metal layer to enhance the conductivity between the sample 9 to be tested and the working electrode rod 10.

[0031] Substrate 5 is made of calcium fluoride. Calcium fluoride is used as substrate 5 for ion beam deposition, which will not affect the catalytic reaction.

[0032] The sealing ring 6 is a fluorine O ring.

[0033] The main body 1, top cover 2, and side cover 3 are all made of polytetrafluoroethylene or PEEK material.

[0034] As a specific example, ORR catalysis is carried out using FeCoNiCuTi high-entropy alloy nanofilms.

[0035] (1) Using a calcium fluoride single crystal with a size of 20mm×40mm×0.5mm as the substrate 5, FeCu target, CoCu target and NiTi target were selected as ion source targets, and FeCoNiCuTi alloy nanofilm was prepared by using 3-channel magnetic filter cathode vacuum arc deposition technology. The film thickness was about 50nm.

[0036] (2) Calcium fluoride with a FeCoNiCuTi alloy nanofilm deposited on it is used as the working electrode and connected to the working electrode rod 10 using a clamping method. Teflon gaskets with a thickness of 40 μm are selected to install the sample 9 in the corresponding position (connecting the body 1 and side cover 3). This ensures that the thickness of the liquid layer through which infrared light passes is 80 μm, which meets the testing requirements. Then, electrolyte 14 (0.1 M perchloric acid solution) is injected into the container to a suitable height. Finally, the top cover 2 is connected to the side cover 3 and the body 1, and the Ag / AgCl reference electrode, graphite counter electrode, inlet pipe, and exhaust pipe are installed sequentially. The installed electrochemical cell device for in-situ infrared spectroscopy testing is then connected to the electrochemical workstation.

[0037] (3) The electrochemical cell device used for in-situ infrared spectroscopy testing is adjusted in the test optical path to obtain a clear infrared spectral reflection signal. Then, an electrochemical experiment is carried out under certain conditions: LSV scanning is performed in the potential range of 0.01-1.2V vs RHE at a scanning speed of 10mV / s. The catalytic reaction process on the sample surface is tested in-situ using infrared spectroscopy to obtain infrared spectral signals.

[0038] This specification uses specific examples to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of the present invention. At the same time, those skilled in the art will recognize that, based on the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. An electrochemical cell device for in-situ infrared spectroscopy testing, characterized in that: The device includes a body, a top cover, side covers, a gasket, and a base. One side of the body is open and connected to the side cover, forming a receiving groove between the body and the side cover. The upper end of the receiving groove is open and closed by the top cover. Sealing rings seal the body and the side cover, the body and the top cover, and the side cover and the top cover. The top cover has mounting holes and vent holes, both of which connect the receiving groove to the outside. A window channel is provided on the side of the body near the side cover, and on the side cover near the body, both connecting the receiving groove to the outside. The two window channels are coaxially arranged, with a window on each of the two window channels located close to each other. The sample to be tested is placed between the two windows. One of the gaskets is located between one of the windows and the sample to be tested, and the other gasket is located between the substrate and the other window. The distance between the sample to be tested and the window can be adjusted by changing the gaskets of different thicknesses. The substrate is located between the two windows and is used to connect to the working electrode rod. The sample to be tested is in contact with the substrate, and the sample to be tested and the working electrode rod are electrically conductive. The accommodating groove contains electrolyte. The gasket is an annular shape with a notch. The notch design ensures that the surface of the sample to be tested is immersed in the electrolyte solution. By changing different substrates, the transmission mode and the reflection mode can be switched.

2. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: The main body and the side cover are connected by bolts.

3. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: The top cover and the main body, as well as the top cover and the side cover, are all connected by bolts.

4. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: There are three mounting holes, and the mounting holes are respectively used to install the working electrode rod, the reference electrode rod, and the counter electrode rod. The vent hole includes an air inlet hole and an air outlet hole, and the air inlet hole is used to install an air inlet pipe, and the air outlet hole is used to install an air outlet pipe.

5. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: The window is made of calcium fluoride single crystal material.

6. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: The gasket is made of Teflon material.

7. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: A conductive layer is provided on the area of ​​the substrate that is not in contact with the electrolyte.

8. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 7, characterized in that: The conductive layer is a metal layer.

9. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: The substrate is made of calcium fluoride material.

10. The electrochemical cell device for in-situ infrared spectroscopy testing according to claim 1, characterized in that: The body, the top cover, and the side cover are all made of polytetrafluoroethylene or PEEK material.

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