Flow field control coupled surface enhanced infrared spectroscopy electrochemical equipment
By using a surface-enhanced infrared spectroscopy electrochemical device coupled with flow field control, the problem of existing devices being unable to simulate real electrochemical cell reactions has been solved. This enables in-depth research and data support on electrochemical cell reaction factors, improving the accuracy and reliability of the analysis.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- CHANGCHUN INSTITUTE OF APPLIED CHEMISTRY CHINESE ACADEMY OF SCIENCES
- Filing Date
- 2026-02-26
- Publication Date
- 2026-05-12
AI Technical Summary
Existing electrochemical reaction analysis devices are unable to simulate various reaction scenarios in real electrochemical cells, which limits the analysis and research of reactions inside electrochemical cells.
A flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device was designed, including an electrochemical cell assembly and an infrared spectroscopy detection assembly. By setting up a multi-channel thin-layer flow channel, an ion exchange membrane and a peristaltic pump, independent fluid control of the electrode and the working electrode is achieved, and infrared detection is performed through an infrared-transmitting crystal and an optical path structure.
It enables more effective research into factors affecting electrochemical cell reactions, provides reliable data for the regulation of electrochemical cells, simulates various reaction scenarios in real electrochemical cells, and improves the accuracy and reliability of electrochemical reaction analysis.
Smart Images

Figure CN122016960A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of electrochemical technology, and in particular to a flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device. Background Technology
[0002] Attenuated total reflectance-surface-enhanced infrared spectroscopy (ADIR-SIR) electrochemical technology is a core characterization technique that integrates spectroscopy and electrochemistry. This technology can capture in real time the molecular structure evolution, charge transfer processes, and reaction intermediates at the electrode interface in an electrochemical cell. It is a key means to reveal electrocatalytic mechanisms and optimize electrode materials, and has wide applications in energy storage and conversion, electrochemical synthesis, and environmental remediation.
[0003] The device for realizing surface-enhanced infrared spectroscopy electrochemistry mainly consists of two core modules: a reflective optical path device and an electrochemical cell. The reflective optical path device is responsible for the transmission, reflection, and signal acquisition of infrared light. The electrochemical cell is responsible for providing a stable electrochemical reaction environment and supporting the electrode system. The electrode system is mainly a three-electrode structure composed of a counter electrode, a reference electrode, and a working electrode. This electrode system is equivalent to a simplified version of the electrochemical cell. Although it can reduce the structural composition of the electrochemical cell module to a certain extent, the ability of the electrochemical cell to simulate the internal reaction of a real electrochemical cell is very limited, which restricts the working performance of the device and restricts the analysis and research of the internal reaction of the electrochemical cell using surface-enhanced infrared spectroscopy electrochemistry. Summary of the Invention
[0004] The purpose of this invention is to provide a flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device, which solves the problem of limited electrochemical reaction analysis and research. It can simulate various reaction scenarios in a real electrochemical cell, thereby more effectively studying the factors affecting the electrochemical cell reaction and providing more reliable data for the real regulation of the electrochemical cell.
[0005] To address the aforementioned technical problems, this invention provides a flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device, comprising an electrochemical cell assembly and an infrared spectroscopy detection assembly;
[0006] The electrochemical cell assembly includes, in sequence, a working electrode side end plate, a working electrode, a reference electrode, a first multi-channel thin-layer flow channel, an ion exchange membrane, a second multi-channel thin-layer flow channel, a counter electrode, and a counter electrode side end plate; an infrared detection window is provided on the working electrode side end plate; the working electrode is fitted to the infrared detection window; a working electrode side fluid inlet is provided on the working electrode side end plate, and a peristaltic pump is connected to the working electrode side fluid inlet; a counter electrode side fluid inlet is provided on the counter electrode side end plate.
[0007] The infrared spectral detection component includes an incident optical path structure for transmitting a first infrared detection light into the infrared detection window and a detection optical path structure for detecting a second infrared detection light output from the infrared detection window.
[0008] In one optional embodiment of this application, both the first multi-channel thin-film flow channel and the second multi-channel thin-film flow channel are polytetrafluoroethylene (PTFE) flow channels;
[0009] The ion exchange membrane is a perfluorosulfonic acid type proton exchange membrane;
[0010] The counter electrode is a platinum sheet electrode, gold sheet electrode, nickel sheet electrode, or copper sheet electrode with mesh or foam holes; the edge of the counter electrode is provided with a sealing gasket, which is a polytetrafluoroethylene sheet or a polysiloxane sheet with a thickness of 0.1mm-1mm.
[0011] In one optional embodiment of this application, the infrared detection window includes an infrared detection through hole opened on the working electrode side end plate, and an infrared transparent crystal embedded in the infrared detection through hole;
[0012] The working electrode is a gold nanofilm or silver nanofilm deposited on the first end face of the infrared transparent crystal, with a thickness of 50nm-200nm.
[0013] In one optional embodiment of this application, the infrared detection through-hole is a circular through-hole; the infrared transparent crystal is a silicon crystal, a zinc selenide crystal, or a germanium crystal;
[0014] The infrared transparent crystal is a cylindrical crystal with its second end protruding from the outside of the working electrode side plate; the second end of the infrared transparent crystal includes a middle end face perpendicular to the central axis of the infrared transparent crystal, and an incident end face and an exit end face symmetrically located on both sides of the middle end face and inclined relative to the middle end face; and the incident end face and the exit end face are both planar.
[0015] Alternatively, the infrared-transmitting crystal may be a hemispherical crystal.
[0016] In one optional embodiment of this application, the infrared spectroscopy detection component includes a package housing, and a through hole is formed on one side wall of the package housing; the second end of the infrared transparent crystal is embedded in the through hole.
[0017] In one optional embodiment of this application, the incident angle of the first infrared detection light input into the infrared detection window by the incident light path structure is adjustable.
[0018] In one optional embodiment of this application, the infrared spectroscopy detection component includes a slide rail; the incident light path structure includes an infrared light source and a first transmission light path structure; and the detection light path structure includes a second transmission light path structure and an infrared spectrometer.
[0019] The optical elements of the first transmission optical path structure and the second transmission optical path structure are the same and are opposite to each other; at least a portion of the optical path structure in both the first transmission optical path structure and the second transmission optical path structure is disposed on the slide rail.
[0020] In one optional embodiment of this application, the first transmission optical path assembly includes a first collimating optical element, a first sliding reflective element, and a first focusing element arranged sequentially along the optical path; the second transmission optical path assembly includes a second focusing element, a second sliding reflective element, and a second collimating optical element arranged sequentially along the optical path.
[0021] The infrared detection window is located at the focal point of the first focusing element and the second focusing element;
[0022] The slide rail is a straight track extending in a set direction; the first sliding reflective element and the second sliding reflective element can slide synchronously on the slide rail in the set direction;
[0023] The first infrared detection light output by the infrared light source is sequentially modulated into parallel light by the first collimating optical element and incident on the first sliding reflective element along the set direction. After being reflected by the first sliding reflective element, it is incident on the first focusing element and then converged by the first focusing element to be incident on the infrared detection window.
[0024] The second infrared detection light output from the infrared detection window is modulated into parallel light by the second focusing element and incident on the second sliding reflective element. After being reflected by the second sliding reflective element, it is incident on the second collimating optical element along the set direction. After being modulated into a diverging beam by the second collimating optical element, it is incident on the infrared spectrometer.
[0025] In an optional embodiment of this application, the first sliding reflective element and the second sliding reflective element are planar reflective mirrors formed by two adjacent facets on the same prism; and the included angle between the two planar reflective mirrors and the set direction is the same.
[0026] The slide rail is equipped with an adjustment knob connected to the prism, which is used to adjust the position of the prism on the slide rail.
[0027] In one optional embodiment of this application, the first collimating optical element and the second collimating optical element are concave reflectors formed by two parabolic surfaces.
[0028] The present invention provides a flow field controlled coupled surface-enhanced infrared spectroscopy electrochemical device, comprising an electrochemical cell assembly and an infrared spectroscopy detection assembly; wherein, the electrochemical cell assembly includes a working electrode side end plate, a working electrode, a reference electrode, a first multi-channel thin-layer flow channel, an ion exchange membrane, a second multi-channel thin-layer flow channel, a counter electrode, a sealing gasket, and a counter electrode side end plate arranged sequentially; an infrared detection window is provided on the working electrode side end plate; the working electrode is fitted to the infrared detection window; a working electrode side fluid inlet is provided on the working electrode side end plate, and a peristaltic pump is connected to the working electrode side fluid inlet; a counter electrode side fluid inlet is provided on the counter electrode side end plate; the infrared spectroscopy detection assembly includes an incident optical path structure for transmitting first infrared detection light into the infrared detection window and a detection optical path structure for detecting second infrared detection light output from the infrared detection window.
[0029] In this application, a first multi-channel thin-layer flow path, an ion exchange membrane, and a second multi-channel thin-layer flow path are further provided between the reference electrode and the counter electrode in the electrochemical cell assembly. Therefore, during the actual analysis and research of the reaction process within the electrochemical cell using infrared light, the isolation effect of the ion exchange membrane allows for differentiated control of the fluid environment where the reference electrode and working electrode are located compared to the fluid environment where the counter electrode is located. Furthermore, the first and second multi-channel thin-layer flow paths can separately control different fluid flow and diffusion processes on both sides of the ion exchange membrane. Moreover, through the synergistic cooperation of the peristaltic pump, the first and second multi-channel thin-layer flow paths, the flow field distribution within the electrochemical cell can be altered, providing support for studying the influence of different reaction conditions on the reaction process. Thus, the electrochemical cell assembly in this application can more richly simulate various reaction scenarios in a real electrochemical cell, thereby more effectively studying the factors affecting the electrochemical cell reaction and providing more reliable data for the actual control of the electrochemical cell. Attached Figure Description
[0030] To more clearly illustrate the technical solutions of the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art 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.
[0031] Figure 1 A schematic diagram of the electrochemical cell assembly in the flow field control coupled surface-enhanced infrared spectroscopy electrochemical device provided in the embodiments of this application;
[0032] Figure 2 A schematic diagram of the fluid flow path in an electrochemical cell provided in an embodiment of this application;
[0033] Figure 3 A schematic diagram of the infrared spectroscopy detection component in the flow field control coupled surface-enhanced infrared spectroscopy electrochemical device provided in the embodiments of this application;
[0034] Figure 4 This is a schematic diagram of the structure of an infrared-transparent wafer provided in an embodiment of this application;
[0035] Figure 5 This is a schematic diagram of the optical path of a parabolic concave reflector provided in an embodiment of this application;
[0036] Figure 6 This is a schematic diagram of the connection structure between the prism and the slide rail provided in an embodiment of this application;
[0037] In the attached diagram: 1 is the electrochemical cell assembly, 10 is the infrared transparent crystal, 100 is the intermediate end face, 101 is the incident end face, 102 is the exit end face, 11 is the working electrode side end plate, 110 is the infrared detection through hole, 111 is the working electrode side fluid inlet, 12 is the working electrode, 13 is the reference electrode, 14 is the first multi-channel thin-layer flow channel, 15 is the ion exchange membrane, 16 is the second multi-channel thin-layer flow channel, 17 is the counter electrode, 18 is the counter electrode side end plate, and 181 is the counter electrode side fluid inlet. 19 is a sealing gasket, 20 is a package housing, 200 is a plane mirror, 210 is an infrared light source, 21 is a prism element, 211 is a first collimating optical element, 212 is a first sliding reflective element, 213 is a first focusing element, 220 is an infrared spectrometer, 22 is a triangular prism, 221 is a second collimating optical element, 222 is a second sliding reflective element, 223 is a second focusing element, 23 is a slide rail, 24 is a threaded ring, 25 is a threaded rod, 26 is an adjusting knob, and 27 is a limiting ring. Detailed Implementation
[0038] The core of this invention is to provide a flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device, which can better simulate various reaction scenarios in real electrochemical cells, thereby effectively studying the influencing factors affecting the reaction process of electrochemical cells and providing reliable data for the practical application of electrochemical cells.
[0039] To enable those skilled in the art to better understand the present invention, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. Obviously, the described embodiments are merely 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.
[0040] like Figures 1 to 3 As shown, Figure 1A schematic diagram of the electrochemical cell assembly in the flow field control coupled surface-enhanced infrared spectroscopy electrochemical device provided in the embodiments of this application; Figure 2 A schematic diagram of the fluid flow path in an electrochemical cell provided in an embodiment of this application; Figure 3 The infrared spectroscopy detection component in the surface-enhanced infrared spectroscopy electrochemical device with flow field control coupling provided in the embodiments of this application.
[0041] In one specific embodiment of this application, the flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device may include:
[0042] Electrochemical cell assembly 1 and infrared spectroscopy detection assembly;
[0043] The electrochemical cell assembly 1 includes a working electrode side end plate 11, a working electrode 12, a reference electrode 13, a first multi-channel thin-layer channel 14, an ion exchange membrane 15, a second multi-channel thin-layer channel 16, a counter electrode 17, and a counter electrode side end plate 18 arranged sequentially. An infrared detection window is provided on the working electrode side end plate 11. The working electrode 12 is attached to the infrared detection window. A working electrode side fluid inlet 111 is provided on the working electrode side end plate 11, and a peristaltic pump is connected to the working electrode side fluid inlet 111. A counter electrode side fluid inlet 181 is provided on the counter electrode side end plate 18.
[0044] The infrared spectroscopy detection component includes an incident optical path structure for transmitting a first infrared detection light into an infrared detection window and a detection optical path structure for detecting a second infrared detection light output from the infrared detection window.
[0045] like Figure 1 As shown, the electrochemical cell assembly 1 of this embodiment includes a complete structure for electrochemical reactions, comprising a working electrode 12, a reference electrode 13, a first multi-channel thin-layer channel 14, an ion exchange membrane 15, a second multi-channel thin-layer channel 16, and a counter electrode 17 disposed between the working electrode side end plate 11 and the counter electrode side end plate 18. That is to say, in addition to the conventional three-electrode structure consisting of a working electrode 12, a reference electrode 13, and a counter electrode 17, the electrochemical cell assembly 1 of this embodiment further provides a first multi-channel thin-layer channel 14, an ion exchange membrane 15, and a second multi-channel thin-layer channel 16 between the reference electrode 13 and the counter electrode 17. Therefore, the structure of the electrochemical cell assembly 1 in this embodiment is closer to the structure of a real-world electrochemical reaction cell, and can more realistically simulate the electrochemical reaction process in actual applications.
[0046] In this embodiment, the ion exchange membrane 15 can be a perfluorosulfuric acid type proton exchange membrane. The ion exchange membrane 15 is a semi-permeable membrane layer that allows specific ions to pass through while other ions cannot. This can provide different fluid material environments for the working electrode 12 and the counter electrode 17, respectively.
[0047] The first multi-channel thin-film flow channel 14 and the second multi-channel thin-film flow channel 16 are film structures used to restrict the flow and diffusion path of fluid substances on the working electrode 12 side and the counter electrode 17 side. Both the first multi-channel thin-film channel 14 and the second multi-channel thin-film channel 16 can be polytetrafluoroethylene (PTFE) channels, and both can be flat plate structures containing several fluid channels. Figure 1 As shown, in Figure 1 Both the first multi-channel thin-film channel 14 and the second multi-channel thin-film channel 16 include several spaced-apart spacers, with at least one end of each adjacent spacer connected to the other, and the gap between adjacent spacers forming a flow channel. Taking the first multi-channel thin-film channel 14 as an example, when the two sides of the first multi-channel thin-film channel 14 are respectively attached and connected to the ion exchange membrane 15 and the working electrode 12, the gap between two adjacent spacers also forms a flow channel through which the fluid flows.
[0048] Furthermore, the spacing between adjacent flow channels in the first multi-channel thin-layer channel 14 and the second multi-channel thin-layer channel 16 can be 0.6 mm to 1 mm, that is, the width of the spacer is 0.6 mm to 1 mm, for example, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1.0 mm, etc., and the thickness of the thin layer in the first multi-channel thin-layer channel 14 and the second multi-channel thin-layer channel 16 can be 2 mm to 4 mm, for example, 2 mm, 3 mm, 4 mm, etc.
[0049] In this embodiment, the synergistic operation of the first multi-channel thin-layer channel 14, the second multi-channel thin-layer channel 16, and the ion exchange membrane 15 can effectively disperse the bubbles generated by the electrochemical reaction, prevent the bubbles from accumulating on the surface of the working electrode 12 to form a phase separation region, and at the same time prevent cross-interference of reactants between the anode and cathode (working electrode 12 and counter electrode 17), thus ensuring the uniformity of the material on the surface of the working electrode 12 and the stability of the reaction.
[0050] In addition, a working electrode side fluid inlet 111 and a working electrode side fluid outlet may be provided on the working electrode side end plate 11, and a peristaltic pump is connected to the working electrode side fluid inlet 111; a counter electrode side fluid inlet 181 and a counter electrode side fluid outlet are provided on the counter electrode side end plate 18.
[0051] Understandably, the fluid outlet on the working electrode side is... Figure 1Although not shown in the figure, it can be symmetrically arranged on both sides of the working electrode side end plate 11 with the working electrode side inlet 111; similarly, the counter electrode side fluid outlet can also be arranged on both sides of the counter electrode side end plate with the counter electrode side fluid inlet 181.
[0052] Therefore, in practical applications, based on the division of the electrochemical cell into two chambers by the ion exchange membrane 15, the fluid flow in the two chambers is controlled by a peristaltic pump, the working electrode side fluid inlet 111, the working electrode side fluid outlet, the counter electrode side fluid inlet 181, and the counter electrode side fluid outlet, respectively. This allows substances that can permeate the ion exchange membrane 15 to flow and exchange between the two chambers. Simultaneously, some reactants and products flow in and out through the working electrode side fluid inlet 111, while other reactants and products flow out through the counter electrode side fluid inlet 181, keeping the fluid in the electrochemical cell in a flowing state. Figure 2 As shown, Figure 2 The diagram illustrates four different flow paths that fluid substances can flow through in an electrochemical cell.
[0053] Taking the carbon dioxide reduction reaction occurring in the electrochemical cell as an example, a saturated carbon dioxide solution can be introduced into the working electrode 12 side through the working electrode side fluid inlet 111, and water or water vapor can be introduced into the counter electrode 17 side through the counter electrode side fluid inlet 181. The water or water vapor is oxidized in the chamber on the counter electrode 17 side to produce oxygen and hydrogen ions. The produced oxygen is discharged through the counter electrode side fluid outlet, while the hydrogen ions enter the chamber on the working electrode 12 side through the ion exchange membrane and undergo a reduction reaction with carbon dioxide to form reduction products that flow out with the fluid from the working electrode side fluid outlet.
[0054] On the counter electrode side, a water oxidation reaction occurs. Water or water vapor is introduced and oxidized on the counter electrode to produce oxygen. The generated oxygen flows out with the fluid on the counter electrode side, while the generated H+ ions pass through the ion exchange membrane into the chamber on the working electrode side. On the working electrode side, a carbon dioxide reduction reaction occurs. A carbon dioxide-saturated solution is introduced, and the carbon dioxide and H+ ions from the counter electrode side chamber are reduced by the working electrode to form reduction products. These products flow out of the working electrode reaction chamber with the fluid. In summary, the reaction chambers of the working electrode and counter electrode are independently controlled; only H+ ions pass through the ion exchange membrane from the counter electrode side chamber into the working electrode side chamber.
[0055] In addition, the fluid inlet 111 on the working electrode side is also connected to a peristaltic pump, which can realize the active transport of fluid substances and the control of flow rate in the electrochemical cell. This significantly accelerates the renewal rate of reactants / products at the electrode interface, reduces concentration polarization, and effectively disperses the bubbles generated by the reaction, preventing them from accumulating on the electrode surface to form a phase separation region, thus ensuring the uniformity of the fluid on the electrode surface and the stability of the reaction. Furthermore, through the synergistic cooperation of the peristaltic pump and the first multi-channel thin-layer channel 14 and the second multi-channel thin-layer channel 16, the flow field distribution in the electrochemical cell can be changed, providing support for studying the influence of different reaction conditions on the reaction process in the electrochemical cell.
[0056] Optionally, in this embodiment, the working electrode side end plate 11 and the counter electrode side end plate 18 can be any one of polyetheretherketone end plates, polytetrafluoroethylene end plates, or polymethyl methacrylate end plates. End plates made of this type of material have excellent insulation, corrosion resistance, and mechanical strength.
[0057] Furthermore, in this embodiment, the reference electrode 13 can be any one of a silver electrode, silver chloride electrode, mercury electrode, mercuric oxide electrode, or saturated calomel electrode. The counter electrode 17 can be a platinum sheet electrode, gold sheet electrode, nickel sheet electrode, or copper sheet electrode with mesh or pores. A sealing gasket 19 is provided at the edge of the counter electrode 17. This sealing gasket 19 can be a polytetrafluoroethylene (PTFE) sheet or a polysiloxane sheet, with a thickness of 0.1 mm to 1 mm. PTFE gaskets are suitable for highly corrosive electrolyte systems, while polysiloxane gaskets have superior elastic sealing performance. Figure 1 As shown, the sealing gasket 19 is sealed to the edge of the counter electrode side plate 18 and the second multi-channel thin-layer channel 16, forming a closed space for the counter electrode 17.
[0058] Based on the above discussion, in order to further detect the electrochemical reaction process in the electrochemical cell using infrared light, an infrared detection window is further provided on the working electrode side end plate 11. For example... Figure 1 As shown, the infrared detection window may include an infrared detection through-hole 110 formed on the working electrode side end plate 11, and an infrared transparent crystal 10 sealed in the infrared detection through-hole 110. Furthermore, the working electrode 12 in the electrochemical cell assembly 1 may be attached to the end face of the infrared transparent crystal 10 near the interior of the electrochemical cell; specifically, the working electrode 12 may be a gold nanofilm or silver nanofilm deposited on the first end face of the infrared transparent crystal 10 (i.e., the end face near the interior of the electrochemical cell assembly 1), with a thickness of 50 nm-200 nm.
[0059] Therefore, during the infrared detection of the electrochemical reaction inside the electrochemical cell assembly 1, infrared light can be incident into the electrochemical cell through the infrared-transmitting crystal 10. The infrared light is reflected from the first end face of the infrared-transmitting crystal 10 and then output. It should be noted that as the electrochemical reaction within the electrochemical cell changes, the reflection of infrared light at the first end face of the infrared-transmitting crystal 10 will change accordingly. Therefore, the infrared light reflected by the infrared-transmitting crystal 10 can be detected, and based on the changes in the infrared light, relevant data on the changes in the electrochemical reaction can be obtained, providing data support for the analysis and research of these changes.
[0060] Further, optionally, the infrared detection through-hole 110 in this application can be a circular through-hole; the infrared transparent crystal 10 is a silicon crystal, a zinc selenide crystal, or a germanium crystal.
[0061] In addition, such as Figure 4 As shown, the infrared transparent crystal 10 can be a cylindrical crystal, and the second end of the infrared transparent crystal 10 protrudes outward from the outer side of the working electrode side plate 11; the second end of the infrared transparent crystal 10 includes a middle end face 100 perpendicular to the central axis of the infrared transparent crystal 10, and an incident end face 101 and an exit end face 102 symmetrically located on both sides of the middle end face 100 and inclined relative to the middle end face 100; and the incident end face 101 and the exit end face 102 are both planar. Figure 4 As shown, since the incident end face 101 and the exit end face 102 are symmetrically arranged, the light path of the infrared light entering the infrared transparent crystal 10 from the incident end face 101 and being reflected from the first end face to the exit end face 102 can always remain symmetrical.
[0062] Of course, in another optional embodiment of this application, the infrared transparent crystal 10 can also be a hemispherical crystal. By reasonably configuring the relative positional relationship between the infrared transparent crystal 10 and the incident light path structure and the detection light path structure in the infrared spectral detection component, the infrared light can always be incident along the radial direction of the hemispherical crystal even if the incident angle of the infrared light on the infrared transparent crystal 10 changes. Correspondingly, the infrared light output from the infrared transparent crystal 10 should also be output along the radial direction of the hemispherical crystal.
[0063] Alternatively, in this embodiment, the infrared spectral detection components can be encapsulated together in the same encapsulation housing 20, and a through hole is provided on one side wall of the encapsulation housing 20. The through hole is located on the output optical path of the incident optical path structure and on the incident optical path of the detection optical path structure. Thus, the second end of the infrared transparent crystal 10 can be embedded in the through hole, thereby realizing the coupling between the optical path structure of the infrared detection component and the electrochemical cell component 1.
[0064] Based on this, in an optional embodiment of this application, the incident angle of the incident light path structure in the infrared spectral detection component into the infrared detection window is adjustable.
[0065] In this embodiment, the first infrared detection light input to the infrared detection window by the incident light path structure is the infrared light incident on the infrared transparent crystal 10; while the infrared light reflected and output from the infrared transparent crystal 10 is the second infrared detection light. Based on this, the incident angle of the incident light path structure onto the infrared transparent crystal 10 in this embodiment is adjustable. Therefore, when actually using infrared spectroscopy to analyze and study the electrochemical reactions inside the electrochemical cell, as the reaction factors (such as fluid velocity, substance concentration, and substance type) within the electrochemical cell change, the incident angle of the first infrared detection light incident on the infrared transparent crystal 10 can be adjusted accordingly. This maximizes the luminous flux and infrared light collection efficiency of the incident light on the surface of the working electrode 12, enhancing the intensity and signal-to-noise ratio of the surface-enhanced infrared light.
[0066] Furthermore, it is understood that the incident angle of the first infrared detection light incident on the infrared transparent crystal 10 changes, and thus the output angle of the second infrared detection light output from the infrared transparent crystal 10 should also change accordingly. As described above, the second end of the infrared transparent crystal 10 in this application may have a mutually symmetrical incident end face 101 and an exit end face 102, or the infrared transparent crystal 10 may be a hemispherical crystal, so that the first infrared detection light and the second infrared detection light always remain mutually symmetrical. Thus, when the first infrared detection light is incident on the infrared transparent crystal 10, the output angle of the second infrared detection light changes by the same amount. A slight change in the angle of the first infrared detection light incident on the incident end face 101 will not cause a large angle change in the second infrared detection light output from the exit end face 102, thus preventing the problem of difficulty in detecting infrared light output from the exit end face 102.
[0067] Based on the above discussion, in another optional embodiment of this application, the infrared spectroscopy detection component may further include a slide rail 23; and the incident light path structure includes an infrared light source 210 and a first transmission light path structure, and the detection light path structure includes a second transmission light path structure and an infrared spectrometer 220.
[0068] The optical elements of the first and second transmission optical path structures are the same and are opposite to each other; at least a portion of the optical path structure in both the first and second transmission optical path structures is set on the slide rail 23.
[0069] As described above, the first infrared detection light incident on the incident end face 101 of the infrared transparent crystal 10 and the second infrared detection light output from the exit end face 102 of the infrared transparent crystal 10 are symmetrical to each other. Therefore, in this embodiment, the first transmission optical path structure in the incident optical path structure and the second transmission optical path structure in the detection optical path structure are further set as optical path structures that are opposite to each other. Thus, during the adjustment and output process of the first infrared detection light output from the infrared light source 210 through the first transmission optical path structure, by adjusting some optical elements in the first transmission optical path structure, during the change of the incident angle of the first infrared detection light incident on the infrared transparent crystal 10, it is only necessary to adjust the corresponding optical elements in the second transmission optical path structure and the first transmission optical path structure to ensure that the second transmission optical path structure can effectively transmit the second infrared detection light to the infrared spectrometer 220, thereby reducing the difficulty of setting up the incident optical path structure and the detection optical path structure to a certain extent.
[0070] Furthermore, in both the first and second transmission optical path structures, at least some optical elements are located on the slide rail 23. That is, the incident angle of the first infrared detection light incident on the infrared transparent crystal 10 is changed by the sliding movement of the optical elements on the slide rail 23. Of course, the optical elements in the first and second transmission optical path structures located on the slide rail 23 should be corresponding to each other, and they can be synchronously adjusted to ensure that as the incident angle of the first infrared detection light incident on the infrared transparent crystal 1 changes, the second transmission optical path structure can always receive the second infrared detection light with a correspondingly changing output angle.
[0071] Further optional, such as Figure 3 As shown, the first transmission optical path assembly in this embodiment may specifically include a first collimating optical element 211, a first sliding reflective element 212 and a first focusing element 213 arranged sequentially along the optical path; the second transmission optical path assembly may include a second focusing element 223, a second sliding reflective element 222 and a second collimating optical element 221 arranged sequentially along the optical path.
[0072] The infrared detection window is located at the focal point of the first focusing element 213 and the second focusing element 223;
[0073] The slide rail 23 is a straight track extending in a set direction; the first sliding reflective element 212 and the second sliding reflective element 222 can slide synchronously in the set direction on the slide rail 23;
[0074] The first infrared detection light output by the infrared light source 210 is sequentially modulated into parallel light by the first collimating optical element 211 and incident on the first sliding reflective element 212 along the set direction. After being reflected by the first sliding reflective element 212, it is incident on the first focusing element 213 and then focused on the infrared detection window by the first focusing element 213.
[0075] The second infrared detection light output from the infrared detection window is modulated into parallel light by the second focusing element 223 and incident on the second sliding reflective element 222. After being reflected by the second sliding reflective element 222, it is incident on the second collimating optical element 221 along a set direction. After being modulated into a diverging beam by the second collimating optical element 221, it is incident on the infrared spectrometer 220.
[0076] As described above, the first transmission optical path structure and the second transmission optical path structure in this embodiment are opposite optical path structures to each other. Therefore, the first collimating optical element 211 and the second collimating optical element 221, the first sliding reflective element 212 and the second sliding reflective element 222, and the first focusing element 213 and the second focusing element 223 are all corresponding elements and the same optical elements. The optical path structures formed in space are also symmetrical to each other.
[0077] Thus, in the incident light path structure, the first infrared detection light output by the infrared light source 210 passes sequentially through the first collimating optical element 211, the first sliding reflective element 212, and the first focusing element 213 before being transmitted to the infrared transparent crystal 10; while the second infrared detection light output by the infrared transparent crystal 10 passes sequentially through the second focusing element 223, the second sliding reflective element 222, and the first collimating optical element 211 before finally being transmitted to the infrared spectrometer 220.
[0078] Reference Figure 3 In this embodiment, both the first collimating optical element 211 and the second collimating optical element 221 can be either reflective or transmissive optical elements. Figure 3 In the embodiment shown, the first collimating optical element 211 and the second collimating optical element 222 are concave reflectors formed by two parabolic surfaces on the same prism element 21. In addition, in order to accommodate the installation space inside the package housing 20, a number of planar reflectors 200 are provided between the infrared light source 210 and the first collimating optical element to achieve optical path deflection between the infrared light source 210 and the first collimating optical element.
[0079] Both the first collimating optical element 211 and the second collimating optical element 221 can be parabolic concave mirrors, and the infrared light source 210 should be located at the equivalent focal point of the first collimating optical element. That is to say, the mirror image positions of each plane mirror 200 between the first collimating optical element and the infrared light source 210 with respect to the focal point of the first collimating optical element coincide with the position of the infrared light source 210. Thus, the first infrared detection light with a divergence angle output by the infrared light source 210 can be modulated into infrared parallel light by the first collimating optical element. The first infrared detection light is incident on the first sliding reflective element 212 in the form of parallel light, and then incident on the first focusing element 213 after passing through the first sliding reflective element 212.
[0080] like Figure 3 As shown, in this embodiment, the first focusing element 213 can be a concave reflector, and the reflection direction of the first infrared detection light reflected by the first sliding reflector 212 should be parallel to the optical axis of the first focusing element 213. This means that the second infrared detection light is incident on the first focusing element 213 as parallel light parallel to the optical axis of the first focusing element 213. The first infrared detection light output by the second focusing element 223 can obviously converge on the focal point of the first focusing element 213. As mentioned above, the position point on the first end face of the infrared transparent crystal 10 that reflects the first infrared detection light should be located at the equivalent focal point of the first focusing element 213 (i.e., the focal position of the first focusing element 213 in the infrared transparent crystal 10 after considering the light deflection caused by the infrared transparent crystal 10).
[0081] Based on this, in this embodiment, the sliding direction of the first sliding reflective element 212 along the slide rail 23 is parallel to the set direction of the first collimating optical element 211 outputting the first infrared detection light to the first sliding reflective element 212. Therefore, as the first sliding reflective element 212 slides along the slide rail 23, the incident angle of the first infrared detection light onto the first sliding reflective element 212 does not change. Consequently, the angle at which the first sliding reflective element 212 reflects the first infrared detection light also does not change. That is, the first infrared detection light is still incident on the first focusing element 213 in a direction parallel to the optical axis of the first focusing element 213. In other words, even when the first sliding reflective element 212 slides on the slide rail 23, the first infrared detection light can still pass through the first focusing element 213 and be incident on the equivalent focal point within the infrared transparent crystal 10.
[0082] like Figure 5 As shown, Figure 5The output shows a schematic diagram of the optical path of two parallel beams at different positions reflected by a concave surface mirror. The dashed and solid lines with arrows represent two parallel beams that are parallel to the optical axis of the concave surface mirror but at different distances from the optical axis. Obviously, both parallel beams can converge at the focal point of the concave surface mirror, but the angle between the principal ray of the converging beam and the optical axis is different.
[0083] However, as the first sliding reflective element 212 slides and moves, when the first infrared detection light is incident on the first focusing element 213, the distance between the main ray of the first infrared detection light and the optical axis of the first focusing element 213 will change, thereby changing the incident angle of the light incident on the infrared transparent crystal 10 after passing through the first focusing element 213.
[0084] Based on the transmission process of the first infrared detection light by the first transmission optical path structure described above, and considering that the second transmission optical path structure and the first transmission optical path structure are opposite optical path structures, it can be seen that the second infrared detection light output from the infrared transparent crystal 10 should obviously be equivalent to the divergent beam output from the equivalent focal point of the second focusing element 223. Therefore, the second focusing element 223 converges the second infrared detection light to form parallel light parallel to its optical axis, which is then incident on the second sliding reflective element 222. The second sliding reflective element 222 is parallel to the set direction. The second infrared detection light is reflected so that it is incident on the second collimating optical element 221 in the form of parallel light. Obviously, the modulation process of the second infrared detection light by the second collimating optical element 221 is the reverse of the modulation process of the first infrared detection light by the first collimating optical element 211. Therefore, the second infrared detection light output by the second collimating optical element 221 can become divergent light. This divergent second infrared detection light can also be transmitted through multiple plane mirrors 200 in sequence before being incident on the infrared spectrometer 220.
[0085] It is understood that the input end of the infrared spectrometer 220 in this embodiment should also be located on the equivalent focal point of the second collimating optical element 221, and the sliding of the second sliding reflective element 222 and the first sliding reflective element 212 along the slide rail 23 should be synchronized, so as to ensure that as the first sliding reflective element 212 slides, the second infrared detection light output from the infrared transparent crystal 10 can always be received and reflected by the second sliding reflective element 222.
[0086] Based on this, in order to simplify the difficulty of synchronously adjusting the first sliding reflective element 212 and the second sliding reflective element 222 on the slide rail 23, the slide rail 23 can be a straight track, and the first sliding reflective element 212 and the second sliding reflective element 222 are two adjacent facets on the same prism 22 forming a plane reflecting mirror; and the angle between the two plane reflecting mirrors and the set direction is the same.
[0087] In addition, such as Figure 6 As shown, a threaded ring 24 with a threaded inner wall, connected to the bottom end of the prism 22, can be provided on the slide rail 23. A threaded rod 25 passes through the threaded ring 24, and an adjusting knob 26 is fixedly connected to one end of the threaded rod 25. Therefore, by simply turning the adjusting knob 26 to rotate the threaded rod 25, the threaded structure on the threaded rod 25 and the threaded ring 24 can be made to engage, driving the threaded ring 24 to move the prism 22 along the slide rail 23. Furthermore, as... Figure 6 As shown, two limiting rings 27 can be connected to both ends of the threaded rod 25. These limiting rings 21 are fixedly connected to the slide rail 23 and to the threaded rod 25. Thus, the limiting rings 21 can restrict the position of the threaded rod 25 while ensuring that the threaded rod 25 can rotate around its own central axis. Furthermore, the limiting rings 27 can prevent the threaded ring 24 from falling off the threaded rod 25. Based on this, the maximum sliding distance of the threaded rod 25 driving the threaded ring 24 can be approximately 3 cm, and the thread pitch on the threaded ring 24 can be 1 mm, thereby enabling high-precision adjustment of the prism 22.
[0088] Furthermore, such as Figure 3 As shown, the prism element 21, where the first collimating optical element 211 and the second collimating optical element 221 are located, can be located at different ends of the slide rail 23, respectively, along with the triangular prism 22.
[0089] In summary, this application further incorporates a first-channel thin-layer flow path, an ion-exchange membrane, and a second-channel thin-layer flow path between the reference electrode and the counter electrode in the electrochemical cell assembly. This allows for differentiated control of the fluid environments of the reference and working electrodes from those of the counter electrode during infrared light analysis of the reaction process within the electrochemical cell, thanks to the isolation effect of the ion-exchange membrane. Furthermore, the first and second multi-channel thin layers can control different fluid flow and diffusion processes on either side of the ion-exchange membrane. The synergistic operation of the peristaltic pump, the first multi-channel thin-layer flow path, and the second multi-channel thin-layer flow path can alter the flow field distribution within the electrochemical cell, providing support for studying the influence of different reaction conditions on the reaction process. Therefore, the electrochemical cell assembly in this application can more comprehensively simulate various reaction scenarios in a real electrochemical cell, enabling more effective research into factors affecting the electrochemical cell reaction and providing more reliable data for the actual control of the electrochemical cell.
[0090] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that the elements inherent in a process, method, article, or apparatus that includes a list of elements are included. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element. Additionally, portions of the technical solutions provided in the embodiments of this application that are consistent with the implementation principles of corresponding technical solutions in the prior art have not been described in detail to avoid excessive elaboration.
[0091] This article 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. It should be noted that those skilled in the art can make several improvements and modifications to the present invention without departing from the principles of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims
1. A flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device, characterized in that, Includes electrochemical cell components and infrared spectroscopy detection components; The electrochemical cell assembly includes, in sequence, a working electrode side end plate, a working electrode, a reference electrode, a first multi-channel thin-layer flow channel, an ion exchange membrane, a second multi-channel thin-layer flow channel, a counter electrode, and a counter electrode side end plate; an infrared detection window is provided on the working electrode side end plate; the working electrode is fitted to the infrared detection window; a working electrode side fluid inlet is provided on the working electrode side end plate, and a peristaltic pump is connected to the working electrode side fluid inlet; a counter electrode side fluid inlet is provided on the counter electrode side end plate. The infrared spectral detection component includes an incident optical path structure for transmitting a first infrared detection light into the infrared detection window and a detection optical path structure for detecting a second infrared detection light output from the infrared detection window.
2. The flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 1, characterized in that, Both the first and second multi-channel thin-layer flow channels are polytetrafluoroethylene (PTFE) flow channels; the ion exchange membrane is a perfluorosulfonic acid type proton exchange membrane. The counter electrode is a platinum sheet electrode, gold sheet electrode, nickel sheet electrode, or copper sheet electrode with mesh or foam holes; the edge of the counter electrode is provided with a sealing gasket, which is a polytetrafluoroethylene sheet or a polysiloxane sheet with a thickness of 0.1mm-1mm.
3. The flow field-controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 2, characterized in that, The infrared detection window includes an infrared detection through hole opened on the working electrode side end plate, and an infrared transparent crystal embedded in the infrared detection through hole; The working electrode is a gold nanofilm or silver nanofilm deposited on the first end face of the infrared transparent crystal, with a thickness of 50nm-200nm.
4. The flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 3, characterized in that, The infrared detection through-hole is a circular through-hole; the infrared transparent crystal is a silicon crystal, a zinc selenide crystal, or a germanium crystal. The infrared transparent crystal is a cylindrical crystal with its second end protruding from the outside of the working electrode side plate; the second end of the infrared transparent crystal includes a middle end face perpendicular to the central axis of the infrared transparent crystal, and an incident end face and an exit end face symmetrically located on both sides of the middle end face and inclined relative to the middle end face; and the incident end face and the exit end face are both planar. Alternatively, the infrared-transmitting crystal may be a hemispherical crystal.
5. The flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 1, characterized in that, The infrared spectroscopy detection component includes a housing, and a through hole is formed on one side wall of the housing; the second end of the infrared transparent crystal is embedded in the through hole.
6. The flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in any one of claims 1 to 5, characterized in that, The incident angle of the incident light path structure into the infrared detection window is adjustable.
7. The flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 6, characterized in that, The infrared spectroscopy detection component includes a slide rail; the incident light path structure includes an infrared light source and a first transmission light path structure; the detection light path structure includes a second transmission light path structure and an infrared spectrometer. The optical elements of the first transmission optical path structure and the second transmission optical path structure are the same and are opposite to each other; at least a portion of the optical path structure in both the first transmission optical path structure and the second transmission optical path structure is disposed on the slide rail.
8. The flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 6, characterized in that, The first transmission optical path assembly includes a first collimating optical element, a first sliding reflective element, and a first focusing element arranged sequentially along the optical path; the second transmission optical path assembly includes a second focusing element, a second sliding reflective element, and a second collimating optical element arranged sequentially along the optical path. The infrared detection window is located at the focal point of the first focusing element and the second focusing element; The slide rail is a straight track extending in a set direction; the first sliding reflective element and the second sliding reflective element can slide synchronously on the slide rail in the set direction; The first infrared detection light output by the infrared light source is sequentially modulated into parallel light by the first collimating optical element and incident on the first sliding reflective element along the set direction. After being reflected by the first sliding reflective element, it is incident on the first focusing element and then converged by the first focusing element to be incident on the infrared detection window. The second infrared detection light output from the infrared detection window is modulated into parallel light by the second focusing element and incident on the second sliding reflective element. After being reflected by the second sliding reflective element, it is incident on the second collimating optical element along the set direction. After being modulated into a diverging beam by the second collimating optical element, it is incident on the infrared spectrometer.
9. The flow-field controlled coupled surface-enhanced infrared spectroscopy electrochemical device as described in claim 8, characterized in that, The first sliding reflective element and the second sliding reflective element are planar reflective mirrors formed by two adjacent facets on the same prism; and the angle between the two planar reflective mirrors and the set direction is the same. The slide rail is equipped with an adjustment knob connected to the prism, which is used to adjust the position of the prism on the slide rail.
10. The infrared detection device for electrochemical cell reaction as described in claim 8, characterized in that, The first collimating optical element and the second collimating optical element are concave reflectors formed by two parabolic surfaces on the same prism element.