Synchrotron radiation in-situ testing device for electrochemical water decomposition reaction

Abstract

The invention relates to a synchrotron radiation in-situ testing device for electrochemical water decomposition reaction, a base assembly of a battery pack is fixedly mounted on a synchrotron radiation sample table, an electrode assembly is fixedly mounted on the base assembly and comprises a working electrode, and an electrolytic tank is mounted on the base assembly and moves between a first position and a second position; when the electrolytic tank is located at the first position, the working electrode is inserted into the electrolytic tank for water electrolysis reaction, and the electrochemical workstation is connected with the electrode assembly to control the water electrolysis process; and when the electrolytic tank is located at the second position, the synchrotron radiation X-rays irradiate the working electrode to monitor the change of the working electrode in the water electrolysis process so as to realize in-situ synchrotron radiation detection. According to the synchrotron radiation in-situ testing device, in-situ synchrotron radiation detection is carried out on the working electrode through synchrotron radiation X-rays, the influence of external factors on an electrode material is eliminated, the authenticity and reliability of detection data are improved, and the electrochemical process of the electrode material is monitored in real time.

Description

Technical Field

[0001] The invention relates to electrochemistry, and more particularly to a synchrotron radiation in-situ testing device for electrochemical water decomposition reaction. Background Art

[0002] As global environmental pollution and energy crisis become increasingly severe, people are no longer just concerned about their own prosperity. Clean and efficient green energy industry has become a new development direction. Due to its large reserves, high calorific value, and carbon-free combustion, hydrogen is considered to be a new energy source with great development prospects. Photoelectrochemical catalytic decomposition of water to produce hydrogen is a method of using photocatalysts to decompose water into hydrogen and byproduct oxygen. Compared with other hydrogen production technologies, it is the greenest way of hydrogen production technology. The energy source of this hydrogen production technology is mainly solar energy, and the byproduct oxygen can be fully utilized without polluting the environment.

[0003] During the electrochemical water splitting process, the electrode materials will undergo a series of physical and chemical changes, which may affect the electrochemical performance of the electrode reaction and even play a decisive role. Existing detection methods mostly observe the changes in the electrode before and after the electrochemical water splitting reaction, lacking real-time monitoring of the reaction process, resulting in an incomplete understanding of the electrode reaction mechanism, which brings difficulties to the subsequent optimization and modification of electrode materials. Summary of the invention

[0004] In order to solve the problem of being unable to conduct real-time monitoring in the above-mentioned prior art, the present invention provides a synchrotron radiation in-situ testing device for electrochemical water decomposition reaction.

[0005] According to the synchrotron radiation in-situ testing device for electrochemical water decomposition reaction of the present invention, it includes a battery pack, an electrolytic cell and an electrochemical workstation, wherein the battery pack includes a base assembly and an electrode assembly, the base assembly is fixedly mounted on the synchrotron radiation sample stage, the electrode assembly is fixedly mounted on the base assembly and includes a working electrode, and the electrolytic cell is mounted on the base assembly and moves between a first position and a second position; when the electrolytic cell is located at the first position, the working electrode is inserted into the electrolytic cell to perform a water electrolysis reaction, and the electrochemical workstation is connected to the electrode assembly to control the water electrolysis process; when the electrolytic cell is located at the second position, the synchrotron radiation X-rays irradiate the working electrode to monitor the changes of the working electrode in the water electrolysis process to realize in-situ synchrotron radiation detection.

[0006] In a preferred embodiment, the electrode assembly further comprises an electrode support and a support clamp, wherein the electrode support is connected to the base assembly, and the working electrode is fixed to the electrode support via the support clamp.

[0007] In a preferred embodiment, the electrode assembly also includes a foam frame, a counter electrode and a reference electrode, wherein the counter electrode and the reference electrode are fixed relative to the working electrode through the foam frame, and the terminals at the upper ends of the counter electrode, the working electrode and the reference electrode are connected to the electrochemical workstation.

[0008] In a preferred embodiment, the counter electrode, the working electrode and the reference electrode are installed through the through holes on the foam frame respectively, and the counter electrode, the working electrode and the reference electrode are installed on the foam frame by interference fit.

[0009] In a preferred embodiment, the working electrode includes an electrode support rod, a working electrode sheet and an electrode clip, wherein the terminal at the upper end of the electrode support rod is connected to the electrochemical workstation, the electrode support rod is installed on the foam frame with an interference fit, the electrode clip is fixedly connected to the electrode support rod, and the working electrode sheet is fixed on the electrode clip.

[0010] In a preferred embodiment, the electrode support rod and the electrode clamp are screwed or integrally formed.

[0011] In a preferred embodiment, the working electrode further comprises a clamping bolt, and the working electrode sheet is fixed to the electrode clamp via the clamping bolt.

[0012] In a preferred embodiment, the base assembly includes a motor, a base and a movable sample holder, wherein the movable sample holder is fixedly mounted on the synchrotron radiation sample stage, the base is fixedly mounted on the movable sample holder, and the motor and the electrode assembly are respectively mounted on the base.

[0013] In a preferred embodiment, the base assembly further comprises a top screw and a stopper, wherein the stopper is connected to the motor, and the electrolytic cell is fixed on the stopper by the top screw.

[0014] According to the synchrotron radiation in-situ testing device for the electrochemical water decomposition reaction of the present invention, in-situ synchrotron radiation detection is performed on the working electrode by synchrotron radiation X-rays, which can not only eliminate the influence of external factors on the electrode material and improve the authenticity and reliability of the detection data, but also monitor the electrochemical process of the electrode material in real time. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of the overall structure of a synchrotron radiation in-situ testing device for electrochemical water decomposition reaction according to a preferred embodiment of the present invention.

[0016] Figure 2 yes Figure 1 Exploded view of the battery pack of the synchrotron radiation in-situ testing device.

[0017] Figure 3 yes Figure 2 Schematic diagram of the structure of the electrode assembly of a battery pack.

[0018] Figure 4 yes Figure 3 Exploded view of the working electrode of the electrode assembly. DETAILED DESCRIPTION

[0019] The preferred embodiments of the present invention are given below in conjunction with the accompanying drawings and described in detail.

[0020] like Figure 1 and Figure 2 As shown, according to a preferred embodiment of the present invention, the synchrotron radiation in-situ testing device for electrochemical water splitting reaction comprises a battery pack 1, an electrolytic cell 2 and an electrochemical workstation 3, wherein the battery pack 1 comprises a base assembly A and an electrode assembly 7, the base assembly A is fixedly mounted on the synchrotron radiation sample stage, and the electrode assembly 7 is fixedly mounted on the base assembly A and comprises a working electrode 12 (see Figure 3 ), the electrolytic cell 2 is mounted on the base assembly A and moves between a first position (high position) and a second position (low position); when the electrolytic cell 2 is in the first position, the working electrode 12 is inserted into the electrolytic cell 2 to perform a water electrolysis reaction, and the electrochemical workstation 3 is connected to the electrode assembly 7 to control the water electrolysis process; when the electrolytic cell 2 is in the second position, the synchrotron radiation X-ray irradiates the working electrode 12 to monitor the changes of the working electrode 12 in the water electrolysis process to achieve in-situ synchrotron radiation detection. The working time of the electrochemical workstation 3 can be set according to specific experimental requirements. The electrochemical workstation 3 is powered off, the water electrolysis reaction stops, and the working electrode 12 is subjected to in-situ synchrotron radiation detection by synchrotron radiation X-rays, which can not only eliminate the influence of external factors on the electrode material, improve the authenticity and reliability of the detection data, but also monitor the electrochemical process of the electrode material in real time. In the prior art for transmission testing or fluorescence testing, there are requirements for the element concentration and sample thickness of the test sample, and the incident angle of the X-ray in the transmission or fluorescence test is also different. The synchrotron radiation in-situ testing device according to the present invention has no restrictions on the selection of electrode materials and the incident angle of X-rays, which provides great convenience for studying various properties of electrode materials.

[0021] like Figure 2 As shown, the base assembly A of the battery pack 1 includes a motor 4, a base 5, a movable sample holder 6, a top screw 8 and a limiter 9, wherein the movable sample holder 6 is detachably (for example, by screws) mounted on the synchrotron radiation sample stage, the base 5 is fixedly mounted on the movable sample holder 6, the motor 4 and the electrode assembly 7 are respectively mounted on the base 5, the limiter 9 is connected to the motor 4 by screws, the electrolytic cell 2 is fixed on the limiter 9 by the top screw 8, and the up and down movement of the electrolytic cell 2 is controlled by the reciprocating motion of the motor 4. The motion of the motor 4 is controllable, so the up and down movement distance of the electrolytic cell 2 can be controlled.

[0022] like Figure 3As shown, the electrode assembly 7 also includes a foam frame 10, a counter electrode 11, a reference electrode 13, an electrode bracket 14 and a bracket clamp 15, wherein the electrode bracket 14 and the base 5 (see Figure 2 ), the working electrode 12 is fixed to the electrode holder 14 through the holder clip 15, the counter electrode 11 and the reference electrode 13 are relatively fixed to the working electrode 12 through the foam holder 10, and the terminals at the upper ends of the counter electrode 11, the working electrode 12 and the reference electrode 13 are connected to the electrochemical workstation 3. The counter electrode 11 can be a platinum electrode or a relatively cheap graphite electrode. The reference electrode 13 can be a mercurous sulfate electrode, a calomel electrode and a silver / silver chloride electrode. In this embodiment, the base 5 has a screw through hole, and the electrode holder 14 is fixed and position-adjustable by screwing the screw through hole through the thread below. In this embodiment, the counter electrode 11, the working electrode 12 and the reference electrode 13 are respectively installed through the through holes on the foam holder 10, and the apertures of the through holes are slightly smaller than the supporting rods of the corresponding electrodes 11, 12, 13, respectively, so that the electrodes 11, 12, 13 can be firmly fixed on the foam holder 10. When the electrolytic cell 2 is driven by the motor 4 to move up and down, the positions of the counter electrode 11 , the working electrode 12 and the reference electrode 13 remain stationary due to the fixing effect of the foam rack 10 and the electrode bracket 14 .

[0023] like Figure 4 As shown, the working electrode 12 includes an electrode support rod 16, a clamping bolt 17, a working electrode sheet 18 and an electrode clamp 19, wherein the terminal at the upper end of the electrode support rod 16 is connected to the electrochemical workstation 3, and the electrode support rod 16 is connected to the electrochemical workstation 3 through a bracket clamp 15 (see Figure 3 ) is clamped and fixed, the outer peripheral surface of the electrode support rod 16 is matched with the through hole of the foam frame 10, the electrode clamp 19 is fixedly connected to the electrode support rod 16, and the working electrode sheet 18 is clamped and fixed on the electrode clamp 19 by the clamping bolt 17. The working electrode sheet 18 can be any material used as a working electrode for electrochemical water decomposition, such as the commonly used TiO 2 , CdZnTe, etc. In this embodiment, the tail of the electrode support rod 16 has a screw hole, and the upper end of the electrode clip 19 is screwed into the screw hole of the electrode support rod 16 for fixing. It should be understood that the fixing method of the electrode support rod 16 and the electrode clip 19 here is only an example and not a limitation. For example, it is also feasible to form the electrode support rod 16 and the electrode clip 19 in one piece, as long as the electrode clip 19 can clamp the working electrode sheet 18.

[0024] By moving the motor 4, the lower ends of the counter electrode 11, the working electrode 12 and the reference electrode 13 are immersed in the electrolyte of the electrolytic cell 2 during the electrolysis process; during the synchrotron radiation test process, the electrolytic cell 2 is lowered so that the lower ends of the counter electrode 11, the working electrode 12 and the reference electrode 13 are no longer immersed in the electrolyte of the electrolytic cell 2, thereby avoiding blocking the working electrode 12 and causing absorption of X-rays, thereby being applied to the in-situ changes of the working electrode 12 during the synchrotron radiation test of electrochemical water decomposition to produce hydrogen.

[0025] The specific application process of the synchrotron radiation in-situ test device for electrochemical water splitting reaction according to the present invention includes: placing the electrolyte corresponding to the working electrode 12 into the electrolytic cell 2 (such as TiO 2 When using Na as the working electrode 2 SO 4 When CdZnTe is used as the working electrode, H 2 SO 4 The electrolytic cell 2 is fixed to the stopper 9 with a top screw 8. After the movable sample holder 6 is fixed to the sample stage of the synchrotron radiation by screws, the positions of the counter electrode 11, the working electrode 12 and the reference electrode 13 on the foam holder 10 are adjusted, and the position of the motor 4 is adjusted so that during the electrochemical water decomposition reaction, the counter electrode 11, the working electrode 12 and the reference electrode 13 are all immersed in the electrolyte and do not touch the bottom and wall of the electrolytic cell 2. At the same time, sufficient margin should be left for the motor 4 to move downward to ensure that after the electrolytic cell 2 moves downward, the wall of the electrolytic cell 2 will not block the working electrode 12, so that the X-ray can directly irradiate the surface of the working electrode 12 during detection, and will not be absorbed and weakened by the wall of the electrolytic cell 2. After the counter electrode 11, working electrode 12, reference electrode 13 and motor 4 are adjusted to the appropriate positions, the electrode support rod 16 is clamped and fixed by the bracket clamp 15. Under the action of the foam rack 10, the counter electrode 11 and the reference electrode 13 are also fixed. After adjusting and fixing the position of the X-ray beam, it is possible to ensure that the physical and chemical in-situ changes of the same point of the working electrode 12 are detected. It should be understood that during the entire electrolysis process, the position of the working electrode 12 remains unchanged, and the position of the X-ray remains unchanged, thereby ensuring that the same point on the working electrode 12 is always detected.

[0026] The above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. The above embodiment of the present invention can also be modified in various ways. That is, all simple, equivalent changes and modifications made according to the claims and the description of the present invention fall within the scope of protection of the claims of the present invention. The contents not described in detail in the present invention are all conventional technical contents.

Claims

1. A synchrotron radiation in-situ testing device for electrochemical water splitting reaction, characterized in that: The synchrotron radiation in-situ testing device comprises a battery pack, an electrolytic cell and an electrochemical workstation, wherein the battery pack comprises a base assembly and an electrode assembly, the base assembly is fixedly mounted on a synchrotron radiation sample stage, the electrode assembly is fixedly mounted on the base assembly and comprises a working electrode, the electrolytic cell is mounted on the base assembly and moves between a first position and a second position; when the electrolytic cell is located at the first position, the working electrode is inserted into the electrolytic cell to perform a water electrolysis reaction, and the electrochemical workstation is connected to the electrode assembly to control the water electrolysis process; when the electrolytic cell is located at the second position, the synchrotron radiation X-rays irradiate the working electrode to monitor changes in the working electrode during the water electrolysis process to achieve in-situ synchrotron radiation detection.

2. The synchrotron radiation in-situ testing device according to claim 1, characterized in that: The electrode assembly also includes an electrode support and a support clip, wherein the electrode support is connected to the base assembly, and the working electrode is fixed to the electrode support via the support clip.

3. The synchrotron radiation in-situ testing device according to claim 1, characterized in that: The electrode assembly also includes a foam frame, a counter electrode and a reference electrode, wherein the counter electrode and the reference electrode are fixed relative to the working electrode through the foam frame, and the upper terminals of the counter electrode, the working electrode and the reference electrode are connected to the electrochemical workstation.

4. The synchrotron radiation in-situ testing device according to claim 3, characterized in that: The counter electrode, the working electrode and the reference electrode are respectively installed through the through holes on the foam frame, and the counter electrode, the working electrode and the reference electrode are installed on the foam frame by interference fit.

5. The synchrotron radiation in-situ testing device according to claim 4, characterized in that: The working electrode comprises an electrode support rod, a working electrode sheet and an electrode clip, wherein the terminal at the upper end of the electrode support rod is connected to the electrochemical workstation, the electrode support rod is installed on the foam frame by interference fit, the electrode clip is fixedly connected to the electrode support rod, and the working electrode sheet is fixed on the electrode clip.

6. The synchrotron radiation in-situ testing device according to claim 5, characterized in that: The electrode support rod and the electrode clamp are screwed or integrally formed.

7. The synchrotron radiation in-situ testing device according to claim 5, characterized in that: The working electrode also includes a clamping bolt, and the working electrode sheet is fixed on the electrode clamp by the clamping bolt.

8. The synchrotron radiation in-situ testing device according to claim 1, characterized in that: The base assembly comprises a motor, a base and a movable sample rack, wherein the movable sample rack is fixedly mounted on the synchrotron radiation sample stage, the base is fixedly mounted on the movable sample rack, and the motor and the electrode assembly are respectively mounted on the base.

9. The synchrotron radiation in-situ testing device according to claim 8, characterized in that: The base assembly also includes a top screw and a stopper, wherein the stopper is connected to the motor, and the electrolytic cell is fixed on the stopper through the top screw.

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