In-situ photoelectrocatalytic electrolytic cell and its application in x-ray absorption spectroscopy

Abstract

The application provides an in-situ photoelectrocatalytic electrolytic cell and application thereof in X-ray absorption spectrum. The electrolytic cell comprises a cell body provided with a cell body cavity, a first surface of the cell body is provided with an opening part, and the opening part is respectively communicated with the cell body cavity and outside of the cell body; a plurality of electrode openings are arranged on a second surface opposite to the first surface, and the electrode openings are respectively used for arranging different electrode sets. A cover plate is detachably connected with the cell body, the cover plate is used for closing the opening part, the cover plate is provided with a light window for passing light, the light window is communicated with the cell body cavity, and a light passing film layer is attached to a side of the cover plate close to the cell body cavity. Through improvement on the structure of the electrolytic cell, the electrolytic cell has good air tightness, the application range of the sample to be measured is wider, and the total height of the electrolytic cell is reduced.

Description

Technical Field

[0001] This application relates to the field of devices for photoelectrocatalytic characterization, and in particular to an in-situ photoelectrocatalytic electrolysis cell and its application in X-ray absorption spectroscopy. Background Technology

[0002] In recent years, with the intensification of the greenhouse effect, extreme weather, energy crisis, and the establishment of dual-carbon goals, people urgently hope to develop clean and renewable energy sources to replace non-renewable energy sources such as oil and coal. Compared with traditional fossil fuels, hydrogen energy has the advantages of being green and environmentally friendly. The product of hydrogen reaction is water, which causes zero pollution to the environment, making it the most ideal clean energy source. We know that solar energy is an inexhaustible energy source. The amount of solar energy received by the Earth every day far exceeds the energy required for life. Utilizing solar energy to decompose water into hydrogen through semiconductor photocatalysts is a clean hydrogen production method with great potential. Photoelectrocatalysis is a type of catalytic reaction driven by light and electricity. Specifically, it is a catalytic effect that accelerates the reaction by accelerating charge transfer at the interface between the electrode and electrolyte made of photocatalyst. Photoelectrocatalysis covers a variety of reaction systems, including oxidation and reduction, and is mainly used in the treatment of organic wastewater, degradation of heavy metal wastewater, desulfurization of gas exhaust, and reduction of automobile exhaust, etc. After decades of research, scientists have improved the photoelectrocatalytic performance of the system through methods such as morphology control, co-catalyst modification, construction of heterojunctions, and element doping.

[0003] X-rays were discovered by Röntgen in 1895. X-rays can "see through" and produce images because their absorption strongly depends on the atomic number Z of the element. Since then, X-rays have gradually developed into a very intuitive and effective method for probing the structure of matter; the famous DNA double helix structure is the most typical example. Synchrotron radiation refers to the radiation emitted tangentially by charged particles moving at relativistic velocities when their motion changes direction due to acceleration in an external magnetic field. Synchrotron X-ray absorption spectroscopy, along with other characterization techniques such as electron microscopy, X-ray diffraction, and nuclear magnetic resonance, has played an extremely important role. However, with further in-depth research into the structure and properties of materials, it is becoming increasingly important to obtain dynamic information such as the reactive sites and reaction kinetics of catalysts in photoelectrocatalytic reactions in real time and in situ at the atomic and molecular scale. Synchrotron radiation accelerators can perform in-situ observations in oprando and in-situ modes, allowing for a more direct observation of changes in matter and greatly aiding in the study of reaction mechanisms. Therefore, developing an in-situ photoelectrocatalytic reaction testing device based on synchrotron X-ray absorption spectroscopy can simulate the real photoelectrocatalytic reaction process and monitor every structural change of the catalyst and reaction products in real time online, so as to truly establish and master its kinetic reaction mechanism. The key to developing an in-situ photoelectrocatalytic reaction testing device based on synchrotron X-ray absorption spectroscopy is to manufacture an in-situ electrocatalytic electrolysis cell that is convenient for testing.

[0004] Existing photoelectrocatalytic cells have the following main shortcomings: 1) Achieving ultra-thin water layer thickness and sealing through cover plate and cell body compression, and designing electrical contact points on the compressed surface of the cell body to accommodate the working electrode in a limited space, limits the space for test sample electrodes, making it only suitable for materials such as carbon paper and foam; 2) The total height of the electrolysis cell generally exceeds 12 cm, while the space of an X-ray beamline is limited, with some X-ray beamlines having less than 8 cm of space, resulting in limited applicability; 3) Common photoelectrocatalytic reaction cell designs only allow visible light to pass through the quartz glass window on the back in fluorescence mode. To address these issues, this application aims to provide an in-situ photoelectrocatalytic cell to overcome the shortcomings of existing photoelectrocatalytic cells. Summary of the Invention

[0005] In view of the problems of the prior art described above, the technical problem solved by this application is to provide an in-situ photoelectrocatalytic electrolysis cell and its application in X-ray absorption spectroscopy. By improving the structure of the electrolysis cell, the electrical contact mode between the test sample electrode and the working electrode WE is optimized while ensuring good airtightness of the electrolysis cell, thereby expanding the range of applicable test samples. The positions of other electrodes are also optimized, resulting in a reduction in the total height of the electrolysis cell and a wider range of applications.

[0006] To achieve the above and other related objectives, the first aspect of this application provides an in-situ photoelectrocatalytic electrolysis cell, comprising: a cell body, the cell body having a cell body cavity, a first surface of the cell body having an opening, the opening being connected to the cell body cavity and the outside of the cell body respectively; and a second surface opposite to the first surface having a plurality of electrode openings for mounting different electrode kits respectively.

[0007] A cover plate, which is detachably connected to the pool body and is used to close the opening;

[0008] The cover plate is provided with a light window for light to pass through. The light window is connected to the pool cavity, and a light-passing membrane is provided on the side of the cover plate near the pool cavity.

[0009] In one possible implementation of the first aspect, the diameter of the light opening decreases sequentially from the cover side away from the pool body to the cover side closer to the pool body.

[0010] In one possible implementation of the first aspect, the light window includes a transition portion and an opening portion; the opening portion is close to the pool cavity, the diameter of the opening portion is smaller than the diameter of the transition portion, and the transition portion is chamfered or the transition portion is truncated.

[0011] In one possible implementation of the first aspect, the beveling angle is 45 to 60°.

[0012] In one possible implementation of the first aspect, the first surface of the pool body is provided with an annular groove, and a sealing ring is provided in the annular groove.

[0013] In one possible implementation of the first aspect, the electrode kit includes an electrode and a hollow electrode sealing screw; the hollow electrode sealing screw is detachably connected to the electrode opening, the electrode is detachably connected to the hollow electrode sealing screw, and the working end of the electrode is disposed within the cavity of the pool body.

[0014] In one possible embodiment of the first aspect, the electrode is selected from one of a reference electrode RE, a working electrode WE, or a counter electrode CE;

[0015] And / or, a sealing ring is fitted on the outside of the hollow electrode sealing screw.

[0016] In one possible implementation of the first aspect, a water inlet and a water inlet pipe are provided on the third side of the pool body; a water outlet and a water outlet pipe are provided on the fourth side opposite to the third side; both the water inlet pipe and the water outlet pipe are connected to the cavity of the pool body.

[0017] In one possible implementation of the first aspect, the inlet pipe is arranged along the tangent of the pool cavity; and / or, the outlet pipe is arranged along the tangent of the pool cavity;

[0018] And / or, the inlet pipe and the outlet pipe are arranged in parallel.

[0019] In one possible implementation of the first aspect, the light passes through a film layer selected from a PTFE tape layer, a polymer film layer, or a composite layer of a quartz sheet and a polymer film.

[0020] In one possible implementation of the first aspect, the light-passing layer is a composite layer of a quartz sheet and a polymer film; wherein the polymer film has through holes, the quartz sheet covers the through holes, and the quartz sheet is used to cover at least a portion of the light-passing window.

[0021] In one possible implementation of the first aspect, the electrode openings are arranged in parallel.

[0022] In one possible embodiment of the first aspect, the electrolytic cell further includes a bottom plate, the cell body is detachably connected to the bottom plate, and the angle between one side of the cell body and the bottom plate is 30 to 135°.

[0023] In one possible implementation of the first aspect, it further includes a plurality of threaded fasteners, the bottom plate is provided with a bottom plate through hole, the pool body is provided with a pool body threaded hole adapted to the bottom plate through hole, and the threaded fastener passes through the bottom plate through hole and is screwed into the pool body threaded hole;

[0024] And / or, the base plate is made of metal.

[0025] In one possible implementation of the first aspect, the bottom plate through hole includes a bottom plate vertical through hole that is perpendicular to the upper surface of the bottom plate and a bottom plate inclined through hole that is inclined to the upper surface of the bottom plate.

[0026] And / or, the through hole in the base plate is a through hole or a threaded hole.

[0027] In one possible implementation of the first aspect, three electrode openings are provided on a second surface opposite to the first surface, for respectively setting a reference electrode RE kit, a working electrode WE kit, and a counter electrode CE kit.

[0028] In some possible implementations of the first aspect, at least one of the following technical features is also included:

[0029] 1) The cover plate is made of metal;

[0030] 2) The pool body is made of PEEK material;

[0031] 3) The pool cavity is cylindrical;

[0032] 4) The wall thickness of the pool body is 0.2-0.8cm, the height of the pool body is 6-8cm, and the inner diameter of the pool body cavity is 3-6cm;

[0033] 5) The thickness of the cover plate is 0.2 to 0.8 cm. The second aspect of this application provides the application of the in-situ photoelectrocatalytic electrolysis cell described above in X-ray absorption spectroscopy.

[0034] The in-situ photoelectrocatalytic electrolyzer provided in this application has, but is not limited to, the following beneficial effects:

[0035] 1) This application improves the structure of the electrolytic cell so that the ultraviolet or visible light used for sample photoexcitation reaches the sample to be tested through the light window of the cover plate, and the X-ray used for characterization also reaches the sample to be tested through the light window. This realizes in-situ photoelectrocatalytic sample testing, and the types of samples to be tested are widely applicable, without requiring the sample to have light-transmitting properties.

[0036] 2) This application also improves the electrical contact method of the working electrode, that is, a place for the sample electrode to be tested is formed between the electrode and the cover plate. Because the distance of the electrode inserted into the cell cavity is adjustable, the electrolytic cell can be used for more sample electrodes of different thicknesses, thus realizing the flexibility of testing.

[0037] 2) This application also reduces the height of the electrolytic cell by placing each electrode horizontally inside the cell cavity, making the electrolytic cell suitable for different X-ray beamline conditions.

[0038] 3) Compared to the light window of a traditional Kapton membrane, this application uses a material that allows both ultraviolet and visible light to pass through, as well as X-rays, to seal the X-ray window. Preferably, a composite ultrathin quartz sheet is used, which absorbs less X-rays at room temperature and pressure while allowing visible and ultraviolet light to pass through, and also possesses a certain degree of durability. Attached Figure Description

[0039] Figure 1 The image shown is an exploded view of the front (first side) of the in-situ photoelectrocatalytic electrolyzer described in Embodiment 1 of this application.

[0040] Figure 2 The image shown is an exploded view of the back (second side) of the in-situ photoelectrocatalytic electrolyzer described in Embodiment 1 of this application.

[0041] Figure 3 The image shown is a first cross-sectional view of the in-situ photoelectrocatalytic electrolyzer described in Embodiment 1 of this application.

[0042] Figure 4 The image shown is a vertical cross-sectional view of the in-situ photoelectrocatalytic electrolyzer described in Embodiment 1 of this application.

[0043] Figure 5 The image shown is a cross-sectional view of the in-situ photoelectrocatalytic electrolyzer described in Example 1 of this application.

[0044] Explanation of reference numerals in the attached figures

[0045] 1 pool

[0046] 11 Pool cavity

[0047] 12. Opening

[0048] 13 Electrode openings

[0049] 131 WE electrode channels

[0050] 132 RE electrode channels

[0051] 133 CE electrode channel

[0052] 14. Circular groove

[0053] 15. Water inlet pipe

[0054] 16 Water outlet pipes

[0055] 17. Water outlet

[0056] 18. Water Inlet

[0057] 2 Electrode Kit

[0058] 21 electrodes

[0059] 22 Hollow electrode sealing screw

[0060] 3. Cover plate

[0061] 31. Light through the window

[0062] 311 Transition Section

[0063] 312 Opening section

[0064] 4. Base plate

[0065] 41 Threaded fasteners

[0066] 42 Through holes in the base plate Detailed Implementation

[0067] A brief explanation of X-ray absorption spectroscopy in fluorescence mode: The sample is irradiated with an X-ray source. The sample absorbs the X-rays and emits fluorescence radiation of a specific energy. This fluorescence radiation is then captured, generating an X-ray absorption spectrum. During the test, the entire process—from X-ray emission to sample irradiation, excitation of fluorescence radiation, and capture and analysis of the fluorescence radiation—occurs on one side of the sample. Compared to X-ray absorption spectroscopy in transmission mode, this measurement mode offers advantages such as lower sample requirements and applicability to a wider range of materials.

[0068] The following specific embodiments illustrate the implementation of this application. Those skilled in the art can easily understand other advantages and effects of this application from the content disclosed in this specification. Please refer to the appendix. Figure 1-5 It should be noted that the structures, proportions, sizes, etc., illustrated in the accompanying drawings are only for the purpose of assisting those skilled in the art in understanding and reading the content disclosed in the specification, and are not intended to limit the implementation conditions of this application. Therefore, they have no substantial technical significance. Any modifications to the structure, changes in the proportions, or adjustments to the size, without affecting the effects and purposes that this application can produce, should still fall within the scope of the technical content disclosed in this application.

[0069] Example 1

[0070] See Figures 1-5 This example provides an in-situ photoelectrocatalytic electrolysis cell, comprising: a cell body 1, the cell body 1 having a cell cavity 11, an opening 12 on a first surface of the cell body 1 communicating with both the cell cavity 11 and the outside of the cell body 1, and multiple electrode openings 13 on a second surface opposite to the first surface, each for mounting different electrode kits 2; and a cover plate 3, detachably connected to the cell body 1, which is used to close the opening 12. The cover plate 3 has a light-transmitting window 31 communicating with the cell cavity 11, and a light-transmitting membrane is disposed on the cover side near the cell cavity 11. Specifically, the light-transmitting membrane can completely cover the opening of the cell cavity, and the tight connection between the cover plate 3 and the cell body 1 clamps the light-transmitting membrane between the cover plate 3 and the cell body 1, thus forming a good seal in the cell body.

[0071] Specifically, see Figure 1The cover plate 3 covers the opening 12 of the cell body 1. The light-transmitting window 31 provides a window for X-rays used for characterization and visible or ultraviolet light used for exciting the catalytic reaction of the sample to pass through, while ensuring airtightness. The cell body cavity 11 of the cell body 1 provides space for accommodating electrodes and electrolyte, and is the main site where the photoelectrocatalytic reaction occurs. More specifically, the light-transmitting membrane covers the entire cover plate, and the material of the light-transmitting membrane is selected to be able to transmit ultraviolet and visible light, as well as X-rays. More specifically, the ultraviolet or visible light used for sample photoexcitation reaches the sample to be tested through the light-transmitting window of the cover plate, and the X-rays used for characterization also reach the sample to be tested through the light-transmitting window, realizing in-situ photoelectrocatalytic sample testing. Moreover, the types of samples to be tested are widely applicable, and the sample does not need to have light-transmitting properties, for example, silicon wafers can be tested.

[0072] Regarding pool 1:

[0073] See Figure 1 The first surface of the pool body 1 has an annular groove 14, and a sealing ring is installed inside the annular groove 14 to meet the sealing requirements. (Continue reading...) Figure 1 The pool cavity 11 is cylindrical. There is an annular groove on the outer periphery of the cylindrical pool cavity 11. The groove is about 0.3cm deep and is concentric with the pool cavity 11. This annular groove is used to place a black sealing rubber ring to meet the sealing requirements.

[0074] See Figure 2 The second side of the back of the cell body has three electrode openings 13, which are used to set different electrode kits 2, such as the electrode opening for the reference electrode RE, the electrode opening for the working electrode WE, and the electrode opening for the counter electrode CE. The three electrode openings 13 are arranged in a straight line on the back of the cell body, and preferably the electrode openings 13 are arranged in parallel. Compared with the prior art of placing electrodes from the top surface of the cell body, the electrode setting method of this application reduces the height of the electrolytic cell, making the electrolytic cell suitable for different X-ray beamline situations. The electrode kit 2 includes an electrode 21 and a hollow electrode sealing screw 22. The hollow electrode sealing screw 22 is detachably connected to the electrode opening 13, and the electrode 21 is detachably connected to the hollow electrode sealing screw 22. The working end of the electrode 21 is set inside the cell body cavity 11. Specifically, the electrode 21 is inserted into the hollow electrode sealing screw 22, and then a sealing ring, such as a rubber ring, is placed inside. The hollow electrode sealing screw 22 is then screwed into the corresponding electrode opening 13 to achieve electrode fixation and sealing. It is worth noting that the structure of the hollow electrode sealing screw and sealing ring in conjunction with the electrode opening 13 ensures both the electrode can enter the electrolytic cell and the cell remains sealed. Furthermore, the distance between the electrode 21 and the hollow electrode sealing screw 22 is adjustable, meaning the depth to which the electrode extends into the cell cavity 11 is adjustable. Here, the electrode 21 can be one of the reference electrode RE, the working electrode WE, or the counter electrode CE. For more details, please refer to... Figure 4 The WE electrode opening includes a WE electrode channel 131 extending parallel to the opening opening; the RE electrode opening includes a RE electrode channel 132 extending parallel to the opening opening; and the CE electrode opening includes a CE electrode channel 133 extending parallel to the opening opening. These electrode channels ensure that the electrode extends into the electrolytic cell, and the extended channels, along with the sealing ring, improve the airtightness of the electrolytic cell. Further preferred embodiments are described below. Figure 1 , 2 4. The WE electrode channel 131 is located between the RE electrode channel 132 and the CE electrode channel 133, and the WE electrode channel 131 is located at the center of the second surface of the cell body. The light opening 31 is located at the center of the first surface of the cell body. That is, in the use state, the working electrode WE and the light covering the light opening 31 form a space (electrical contact point) for placing the sample electrode under test between the film layer. As mentioned above, the depth of the working electrode WE extending into the cell body cavity 11 is adjustable, that is, the space for placing the sample electrode under test is adjustable, thereby enabling the testing of samples with different thicknesses. For example, carbon paper, conductive glass, silicon wafers of different thicknesses, and more specifically, conductive glass with a thickness of 1 to 10 mm.

[0075] In some preferred examples, see Figure 1 and Figure 5 The third side of the pool body 1 is provided with an inlet 18 and an inlet pipe 15, and the fourth side, opposite to the third side, is provided with an outlet 17 and an outlet pipe 16. Both the inlet pipe 15 and the outlet pipe 16 are connected to the pool body cavity 11. Preferably, the outlet pipe 16 is connected to the outlet 17 via an air pipe sealing screw, and the inlet pipe 15 is connected to the inlet 18 via an air pipe sealing screw, providing good sealing performance. Specifically, the outlet pipe 16 and the inlet pipe 15 extend along the tangent direction of the cylindrical pool body cavity 11, and are horizontal and parallel to each other. When the in-situ photoelectrocatalytic electrolysis cell is working, the electrolyte enters the electrolysis cell from the inlet through the inlet pipe 15, and after filling the entire pool body cavity 11, it is discharged from the outlet through the outlet pipe 16. The tangentially arranged inlet and outlet pipes 15 and 16 not only ensure the smooth flow of electrolyte but also allow air bubbles in the electrolyte to be expelled promptly without affecting the acquisition of X-ray absorption spectrum data. Furthermore, sealing rings can be installed at both the inlet and outlet to improve the airtightness of the electrolytic cell.

[0076] In some specific examples, the material of pool 1 is PEEK, which is resistant to strong alkalis and chemical corrosion, and is also insulating, meeting the corrosion resistance and electrical performance requirements of electrolytic cells. The pool body is a cube with dimensions of 6cm x 6cm x 6cm, the wall thickness of pool 1 is 0.2-0.8cm, the height of pool 1 is 6-8cm, and the inner diameter of the pool cavity 11 is 3-6cm.

[0077] Regarding cover plate 3:

[0078] In a preferred embodiment, the diameter of the light opening 31 decreases sequentially from the side of the cover plate furthest from the pool body 1 to the side of the cover plate closest to the pool body 1, in order to meet the oblique illumination requirements of the light path in fluorescence mode. Specifically, see [reference needed]. Figure 3 The light window 31 includes a transition portion 311 and an opening portion 312. The opening portion 312 is located at the bottom of the transition portion 311. The diameter of the opening portion 312 is smaller than the diameter of the transition portion 311. The transition portion 312 is either beveled or truncated cone-shaped, which is beneficial for meeting the oblique illumination requirements of the light path in fluorescence mode. When the transition portion 312 is beveled, the bevel angle is 45° to 60°, for example, 45°, 50°, or 60°.

[0079] In a preferred embodiment, the light passes through a film layer selected from a PTFE tape layer, a polymer film layer, or a composite layer of a quartz sheet and a polymer film, wherein the polymer film layer is an ultrathin, transparent polymer, and the polymer film in the composite layer can be a mature Kapton membrane. This is suitable for photoelectrocatalytic reactions at room temperature and pressure. Specifically, it allows X-rays to pass through at room temperature and pressure, as well as visible and ultraviolet light, overcoming the limitation of traditional electrolytic cells that can only transmit visible light from the back in fluorescence mode. More specifically, the light passes through a composite layer of a quartz sheet and a polymer film; wherein the polymer film has through holes, the quartz sheet covers the through holes, and the quartz sheet is used to cover at least part of the light opening 31, that is, by utilizing the high light transmittance of the quartz sheet and the durability of the polymer film, a composite layer of a quartz sheet and a polymer film is formed, wherein the polymer film in the composite layer is a Kapton film with a thickness of 0.03 to 0.08 mm (e.g., 0.03 mm, 0.04 mm, 0.05 mm, 0.06 to 0.08 mm), and the quartz sheet has a thickness of 0.03 to 0.1 mm (e.g., 0.03 mm, 0.04 mm, 0.05 mm, 0.06 to 0.1 mm). The composite method of the quartz sheet and the Kapton film can be by adhesive bonding, for example, the quartz sheet and the Kapton film can be bonded together by the adhesive properties of Kapton, or it can be fixed and sealed by using quick-drying adhesive on a flat horizontal surface. To reiterate how the composite layer of quartz sheet and polymer film is locked between the pool body and the cover plate, taking the composite layer of quartz sheet and Kapton film as an example, the quartz sheet and Kapton film are bonded together as a whole quartz sheet / Kapton composite film through the above-mentioned bonding method. This composite film is placed between the cover plate 3 and the pool body 1. The screws on the cover plate 3 are tightened to press the quartz sheet / Kapton composite film, thus sealing the pool body 1.

[0080] In some specific examples, the cover plate 3 is made of metal, with sufficient rigidity to support deformation. The thickness of the cover plate 3 is 0.2 to 0.8 cm. There is a circular light-emitting window 31 with a diameter of 1 to 2 cm at the center of the cover plate, and the center of the light-emitting window 31 is the center of the cover plate. Preferably, the light-emitting window has a chamfered angle of 45° to 60° around it to meet the requirements of oblique light path in fluorescence mode.

[0081] More specifically, the cover plate 3 has four threaded holes at its four corners for fixing screws. The center of each threaded hole is 1.5cm from the edge, corresponding to M5 screws. The front of the pool body 1 (i.e., the first side) contacts the cover plate 3, and the front of the pool body 1 also has threaded holes corresponding to the four fixing threaded holes on the cover plate. In use, the cover plate and the pool body are tightly connected by M5 screws, and the compression of the rubber ring causes deformation, achieving a seal.

[0082] In a preferred embodiment, the electrolytic cell further includes a base plate 4, which is used to fix the in-situ photoelectrocatalytic electrolytic cell composed of the cover plate 3 and the cell body 1, allowing the cell body to be stably fixed in front of the detector of the synchrotron radiation beamline. Specifically, the cell body 1 and the base plate 4 are detachably connected, and the angle between one side of the cell body 1 and the base plate 4 is 30° to 135°. To meet the requirement of oblique light path in fluorescence mode, the angle can be 45°, 90°, or 135°. Specifically, the angle between one side of the cell body 1 and the base plate 4 is 30° to 135°, see reference [reference needed]. Figure 1 Taking the left side of pool 1 as an example, referring to section 3, in this case, the angle between the left side of pool 1 and the base plate 4 is 90°. The positions of pool 1 and the base plate are adjusted to accommodate the oblique beam requirements in the subsequent fluorescence mode.

[0083] In a preferred embodiment, see Figure 2 It also includes multiple threaded fasteners 41. The base plate 4 has a base plate through hole 42, and the pool body 1 has a pool body threaded hole adapted to the through hole of the base plate 4. The threaded fasteners 41 pass through the base plate through hole 42 and are screwed into the pool body threaded hole. A specific implementation method is provided where one side of the pool body 1 has an angle of 30° to 135° with the base plate 4. The base plate through hole 42 includes a vertical base plate through hole perpendicular to the upper plane of the base plate 4 and an inclined base plate through hole inclined to the upper plane of the base plate 4. Different inclination angles are achieved by selecting different base plate through holes 42 through the threaded fasteners 41, with an angle range of 30°-135°. Of course, the base plate through hole 42 can be a through hole or a threaded hole.

[0084] As mentioned above, the in-situ photoelectrocatalytic electrolysis cell provided in this application can be applied to different sample electrodes, such as carbon paper of a certain thickness, conductive glass, silicon wafers, etc., and can be applied to different catalyst host materials, providing a real-time, online in-situ photoelectrocatalytic electrolysis cell.

[0085] Example 2

[0086] The installation and usage methods for the in-situ photoelectrocatalytic electrolyzer are provided below:

[0087] a1. Install the black sealing rubber ring in the annular groove, and attach a composite layer of quartz sheet and Kapton film to the inside of the cover plate;

[0088] a2. Place the electrode coated with the sample to be tested in the belly of the pool body cavity, and fix the cover plate and the pool body tightly together with the four corner screws;

[0089] a3. Pass the working electrode WE through the hollow electrode sealing screw and fit it into a suitable sealing rubber ring. Then, press the sample electrode to be tested, which is placed in the cylindrical electrolytic cell, through the opening of the WE electrode. By adjusting the four corner fixing screws and the hollow electrode sealing screw, ensure that the working electrode WE, the sample electrode to be tested, and the cover plate are tightly fitted together.

[0090] a4. Pass the counter electrode CE and the reference electrode RE through the hollow electrode sealing screws respectively, and put them into the appropriate sealing rubber rings. Then, enter the cylindrical electrolytic cell through the openings of the CE electrode and the WE electrode, and tighten the seal.

[0091] a5. Secure the in-situ photoelectrocatalytic electrolysis cell to the base plate using base plate fixing screws.

[0092] a6. Screw the gas pipe sealing screw into the inlet and outlet, insert the corrosion-resistant rubber hose into the gas pipe sealing screw and the external storage tank to complete the electrolyte circulation setup.

[0093] a7. Attach the alligator clips from the external electrochemical workstation circuit to the copper pillars on each electrode to complete the circuit setup.

[0094] a8. Inject the electrolyte into the cell cavity through the inlet and into the external storage tank through the outlet. The electrolyte level shall not be lower than the height of the substrate coated with the sample and not higher than the height of the outlet.

[0095] a9. Conduct photoelectrocatalytic reaction and in-situ X-ray photoelectrocatalytic reaction tests.

[0096] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any form or substance. It should be noted that those skilled in the art can make various improvements and additions without departing from the method of the present invention, and these improvements and additions should also be considered within the scope of protection of the present invention. Any modifications, alterations, and equivalent changes made by those skilled in the art based on the above-disclosed technical content without departing from the spirit and scope of the present invention are equivalent embodiments of the present invention. Furthermore, any modifications, alterations, and evolutions made to the above embodiments based on the essential technology of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. An in-situ photoelectrocatalytic electrolysis cell, characterized in that, include: The pool body (1) has a pool body cavity (11), and the first side of the pool body (1) has an opening (12), which is connected to the pool body cavity (11) and the outside of the pool body (1) respectively; the second side opposite to the first side has a plurality of electrode openings (13), which are used to install different electrode kits (2). Cover plate (3), which is detachably connected to the pool body (1), and the cover plate (3) is used to close the opening (12). The cover plate (3) is provided with a light window (31) for light to pass through. The light window (31) is connected to the pool cavity (11), and a light-passing membrane is provided on the cover plate side near the pool cavity (11). Three electrode openings (13) are provided on the second surface opposite to the first surface, respectively for setting the reference electrode RE kit, the working electrode WE kit and the counter electrode CE kit; the electrode kit (2) includes an electrode (21) and a hollow electrode sealing screw (22); the hollow electrode sealing screw (22) is detachably connected to the electrode opening (13), the electrode (21) is detachably connected to the hollow electrode sealing screw (22), and the working end of the electrode (21) is set inside the pool cavity (11); The light passes through a composite layer of a quartz sheet and a polymer film; wherein the polymer film has through holes, the quartz sheet covers the through holes, and the quartz sheet is used to cover at least part of the light opening (31).

2. The in-situ photoelectrocatalytic electrolyzer according to claim 1, characterized in that, Includes at least one of the following technical features: a) The diameter of the light opening (31) decreases sequentially from the side of the cover plate away from the pool body (1) to the side of the cover plate close to the pool body (1); b) The first surface of the pool body (1) is provided with an annular groove (14), and a sealing ring is provided in the annular groove (14); c) An inlet (18) and an inlet pipe (15) are provided on the third side of the pool body (1); an outlet (17) and an outlet pipe (16) are provided on the fourth side opposite to the third side; the inlet pipe (15) and the outlet pipe (16) are both connected to the pool body cavity (11); d) The electrode openings (13) are arranged in parallel; e) The electrolytic cell also includes a bottom plate (4), the cell body (1) is detachably connected to the bottom plate (4), and the angle between one side of the cell body (1) and the bottom plate (4) is 30~135°. f) The cover plate (3) is made of metal; and / or the pool body (1) is made of PEK; and / or the pool body cavity (11) is cylindrical; and / or the pool body (1) has a wall thickness of 0.2~0.8cm and a height of 6~8cm; the inner diameter of the pool body cavity (11) is 3~6cm; and / or the cover plate (3) has a thickness of 0.2~0.8cm.

3. The in-situ photoelectrocatalytic electrolyzer according to claim 2, characterized in that, In technical feature a), the light opening (31) includes a transition portion (311) and an opening portion (312); the opening portion (312) is close to the pool cavity (11), the diameter of the opening portion (312) is smaller than the diameter of the transition portion (311), and the transition portion (311) is chamfered or the transition portion is in the shape of a truncated cone.

4. The in-situ photoelectrocatalytic electrolyzer according to claim 3, characterized in that, The bevel angle is 45~60°.

5. The in-situ photoelectrocatalytic electrolyzer according to claim 1, characterized in that, The electrode (21) is selected from one of the reference electrode RE, the working electrode WE, or the counter electrode CE; and / or, a sealing ring is fitted on the outside of the hollow electrode sealing screw (22).

6. The in-situ photoelectrocatalytic electrolyzer according to claim 2, characterized in that, In technical feature c), the inlet pipe (15) is arranged along the tangent of the pool cavity (11); and / or, the outlet pipe (16) is arranged along the tangent of the pool cavity (11); And / or, the inlet pipe (15) and the outlet pipe (16) are arranged in parallel.

7. The in-situ photoelectrocatalytic electrolyzer according to claim 2, characterized in that, Technical feature e) also includes multiple threaded fasteners (41), the bottom plate (4) is provided with a bottom plate through hole (42), the pool body (1) is provided with a pool body threaded hole adapted to the bottom plate (4) through hole, and the threaded fastener (41) passes through the bottom plate through hole (42) and is screwed to the pool body threaded hole; And / or, the base plate (4) is made of metal.

8. The in-situ photoelectrocatalytic electrolyzer according to claim 7, characterized in that, The bottom plate through hole (42) includes a bottom plate vertical through hole that is perpendicular to the upper plane of the bottom plate (4) and a bottom plate inclined through hole that is inclined to the upper plane of the bottom plate (4); And / or, the bottom plate through hole (42) is a through hole or a threaded hole.

9. The application of the in-situ photoelectrocatalytic electrolysis cell as described in any one of claims 1 to 8 in X-ray absorption spectroscopy.

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