An in-situ cell for rapid continuous synchrotron x-ray absorption spectroscopy measurements
Patent Information
- Application Number
- CN202522198882.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-17
- Publication Date
- 2026-10-09
- Estimated Expiration
- 2035-10-17
AI Technical Summary
[0003]现有专利技术公开的多种原位同步辐射电化学池应用范围单一，比如现有的同步辐射电化学原位池的溶液腔体过厚，需要大量的电解液，干扰强，仅能适应于传统荧光模式背入射的X射线吸收谱测量手段，耗时长，且难以实时表征材料局域原子和电子结构在非平衡态下的瞬态变化和动态规律，导致实验数据与实际情况存在偏差，严重制约了原位同步辐射光谱技术对真正电化学反应机制全貌的揭示
[0023]1、本实用新型适用于时间分辨能量色散/透射模式的原位同步辐射X射线吸收谱测量，通过对工作电极表面电解液的实时补给和循环流动，保证X射线穿透溶液层的均匀性，加快产物气体的排除，降低溶液扰动对测试信号的影响，提高测试稳定性；
Smart Images
Figure CN224840035U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of spectral measurement and analysis technology, specifically an in-situ cell for rapid continuous synchrotron radiation X-ray absorption spectrum measurement. Background Technology
[0002] Synchrotron radiation X-ray absorption spectroscopy (XAS) is a powerful tool for obtaining information such as the electronic structure and nearest neighbor structure of atoms in matter. Electrochemical in-situ cells provide an in-situ dynamic research method for XAS.
[0003] The existing patented technologies for in-situ synchrotron radiation electrochemical cells have limited applications. For example, the solution chamber of existing in-situ synchrotron radiation electrochemical cells is too thick, requiring a large amount of electrolyte, which causes strong interference. They can only be used for traditional back-incidence X-ray absorption spectroscopy measurements in fluorescence mode, which is time-consuming and difficult to characterize the transient changes and dynamic laws of local atomic and electronic structures of materials in non-equilibrium states in real time. This leads to deviations between experimental data and actual conditions, which seriously restricts the revelation of the true electrochemical reaction mechanism by in-situ synchrotron radiation spectroscopy.
[0004] Moreover, the existing in-situ cell electrodes are far apart, which limits mass transfer during the reaction process, resulting in lower upper limits for voltage and current density, making it difficult to meet the requirements of actual working conditions.
[0005] Although in-situ synchrotron radiation experiments in energy dispersive / transmission mode greatly improve testing efficiency and time resolution, enabling continuous acquisition and real-time in-situ tracking of active structures, reaction intermediates evolution, electronic transitions, and charge transfer behavior under reaction conditions, revealing the dynamic relationship between material properties and local structures, the X-ray signal in this acquisition mode needs to penetrate the electrolyte to irradiate the electrode, and the optical signal will be severely interfered with and strongly absorbed by the solution layer.
[0006] Therefore, it is necessary to design an in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurements. Utility Model Content
[0007] The purpose of this invention is to provide an in-situ cell for rapid continuous synchrotron radiation X-ray absorption spectrum measurement, in order to solve the problems in the prior art.
[0008] The objective of this utility model can be achieved through the following technical solutions:
[0009] An in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurements, the in-situ cell comprising:
[0010] The outer casing has two through holes on one side, and a counter electrode and a reference electrode are fixed in the two through holes respectively.
[0011] The second outer shell is provided in a corresponding manner to the first outer shell, and both the second outer shell and the first outer shell have a square optical window at their center.
[0012] Both the outer casing 1 and the outer casing 2 are provided with channels, and the two channels are located on both sides of the square optical window. A working electrode is fixedly provided between the outer casing 2 and the outer casing 1.
[0013] Furthermore, a solution cavity is provided on the outer shell and on one side of the square optical window. The solution cavity consists of a trapezoidal liquid storage groove and a reaction chamber, with the trapezoidal liquid storage groove located on one side of the reaction chamber.
[0014] Furthermore, the two channels are arranged opposite to each other.
[0015] Furthermore, the outer casing has through holes on both sides, and an inlet pipe and an outlet pipe are fixedly installed in the two through holes respectively.
[0016] Furthermore, each of the four corners of the outer shell 1 and the outer shell 2 is provided with a round hole, which is connected to a fastening bolt to fix the outer shell 1 and the outer shell 2.
[0017] Furthermore, a waterproof gasket is attached between the first and second outer shells to improve the sealing of the reaction tank.
[0018] Furthermore, both the outer shell 1 and the outer shell 2 are made of polyetheretherketone (PEEK).
[0019] Furthermore, the square optical window is sealed with a Kapton film.
[0020] Furthermore, the square optical window is closely fitted to the working electrode, and a conductive tape is fixedly provided on the edge of the working electrode. The conductive tape is sandwiched between the first outer shell and the second outer shell and led out.
[0021] Furthermore, the channel is a truncated quadrangular shape, wherein the angle between the truncated quadrangular shape and the horizontal is 45 degrees.
[0022] The beneficial effects of this utility model are:
[0023] 1. This utility model is applicable to in-situ synchrotron X-ray absorption spectrum measurement in time-resolved energy dispersive / transmission mode. By real-time replenishment and circulation of the electrolyte on the surface of the working electrode, the uniformity of X-ray penetration through the solution layer is ensured, the removal of product gases is accelerated, the influence of solution disturbance on the test signal is reduced, and the test stability is improved.
[0024] 2. The in-situ cell structure of this utility model is compact, and the shell is designed with a truncated quadrangular channel, which is highly compatible with beamline stations. At the same time, it has a thin liquid layer reaction micro-region, which can reduce the loss of X-ray signal during the in-situ experiment, thereby obtaining a high signal-to-noise ratio test signal. The compact three-electrode system has efficient mass transfer, thereby obtaining reliable reaction kinetic information of the local atomic and electronic structure of the sample under non-equilibrium conditions.
[0025] 3. This invention results in less additional signal loss when X-rays penetrate the solution, reduces the absorption of X-rays by the solution, improves the stability of the in-situ cell test, increases signal intensity, and allows for faster resolution of subtle changes on the in-situ electrode. Attached Figure Description
[0026] The present invention will be further described below with reference to the accompanying drawings.
[0027] Figure 1 This is an exploded structural diagram of the in-situ pool of this utility model;
[0028] Figure 2 This is a partial structural schematic diagram of the in-situ pool of this utility model;
[0029] Figure 3 This is a side view of the in-situ pool structure of this utility model;
[0030] Figure 4 This is a schematic diagram of the overall structure of the in-situ pool of this utility model.
[0031] The annotations in the attached figures are explained as follows:
[0032] 1. Outer shell 1; 2. Square optical window; 3. Solution chamber; 4. Outer shell 2; 5. Counter electrode; 6. Reference electrode; 7. Working electrode; 8. Inlet pipe; 9. Outlet pipe; 10. Reaction chamber; 11. Liquid storage groove; 12. Bolt; 13. Conductive tape; 14. Channel; 15. Kapton membrane. Detailed Implementation
[0033] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.
[0034] An in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurements, such as Figure 1 , Figure 2As shown, it includes a first outer shell 1, a second outer shell 4 fixedly mounted on the first outer shell 1, a square optical window 2 opened at the center of the second outer shell 4, and a channel 14 opened on the second outer shell 4. The channel 14 is located above the square optical window 2, and the square optical window 2 faces the center of the first outer shell 1.
[0035] A solution cavity 3 is provided on the outer shell 1 and on one side of the square optical window 2. The solution cavity 3 is divided into a trapezoidal liquid storage groove 11 and a reaction chamber 10. The trapezoidal liquid storage groove 11 is located on one side of the reaction chamber 10. A channel 14 is also provided at the center of the outer shell 1, and the two channels 14 are arranged opposite to each other.
[0036] Two through holes are opened on one side of the outer casing 1, and the counter electrode 5 and the reference electrode 6 are placed in the two through holes respectively. Through holes are opened on both sides of the outer casing 1, and the liquid inlet pipe 8 and the liquid outlet pipe 9 are connected in the through holes respectively.
[0037] Round holes are provided at the four corners of the outer casing 1 for placing fastening bolts 12, and round holes are also provided at corresponding positions on the outer casing 4.
[0038] The outer casing 1 and the outer casing 4 are bonded together with a waterproof gasket and then fixed by four bolts 12 passing through round holes to ensure the tightness and stability of each component.
[0039] In this embodiment, both outer shell 1 and outer shell 4 are made of polyetheretherketone (PEEK).
[0040] Kapton film 15 is placed and sealed in the square optical window 2 at the center of the outer shell 1 and the outer shell 2 4 respectively. A working electrode 7 is fixed between the outer shell 1 and the outer shell 2 4, and the square optical window 2 is in close contact with the working electrode 7.
[0041] The edge of the working electrode 7 is fixedly connected with conductive tape 13. The conductive tape 13 is placed in the reaction chamber 10 of the outer shell 1. The working electrode 7 is in the middle of the outer shell 1 and the outer shell 2 4 and is fixed by the conductive tape 13. The conductive tape 13 is led out from between the outer shell 1 and the outer shell 2 4.
[0042] The trapezoidal liquid storage groove 11 in the solution chamber 3 has a depth of 10 mm, and the upper and lower bases are 6 mm × 12 mm. The reaction chamber 10 has a depth of 1 mm, and its length and width are 20 mm × 20 mm. Both the outer shell 1 and the outer shell 4 have a channel 14 at their center, which gradually narrows towards the square optical window 2. The channel 14 is a truncated pyramid shape, with the truncated pyramid making a 45-degree angle with the horizontal. The outer diameter of the channel 14 is 40 mm, and the inner diameter is 10 mm.
[0043] In this embodiment, the reference electrode 6 is a silver-silver chloride electrode, a mercury-mercury oxide electrode, or a standard hydrogen electrode, and the counter electrode 5 is a platinum wire or a carbon rod, which is inserted and fixed in the corresponding empty slot through a sealing ring.
[0044] During the in-situ test, the outer shell 1 and the outer shell 4 are fixed with bolts 12. Then, the electrolyte is injected into the reaction chamber 10 and the storage groove 11 through the liquid inlet pipes 8 on both sides of the outer shell 1. The liquid outlet pipe 9 is used to discharge the electrolyte. After the electrolyte circulation is stable, the counter electrode 5 and the reference electrode 6 are inserted into the corresponding counter electrode hole and reference electrode hole on the top of the outer shell 1 to construct a complete three-electrode electrochemical in-situ reaction cell system. The time-resolved energy dispersive X-ray absorption spectroscopy synchronous acquisition experiment is then started.
[0045] A liquid storage groove 11 connected above the reaction chamber 10 is used to realize the adjustment and replenishment of the thin liquid layer at the working electrode; by designing a millimeter-thick reaction chamber and tightly fitting the square optical window with the working electrode, a micron-level solution layer is realized in the optical path; the compact three-electrode arrangement and solution circulation settings achieve a current density closer to the actual working condition and reduce the impact of solution disturbance on the signal; the square optical window 2 is made of polyimide film (Kapton film) to reduce the loss of X-rays passing through the window; the truncated quadrangular incident and exit channels on the shell can increase the light flux.
[0046] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of this utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed utility model.
Claims
1. An in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement, characterized in that, The in-situ pool includes: The outer casing (1) has two through holes on one side, and the counter electrode (5) and the reference electrode (6) are fixed in the two through holes respectively. Outer shell 2 (4), the outer shell 1 (1) and outer shell 2 (4) are respectively provided, and a square optical window (2) is provided at the center of both outer shell 2 (4) and outer shell 1 (1); Both the outer shell 1 (1) and the outer shell 2 (4) are provided with channels (14), and the two channels (14) are located on both sides of the square optical window (2). A working electrode (7) is fixedly provided between the outer shell 2 (4) and the outer shell 1 (1).
2. The in-situ cell for rapid continuous synchrotron radiation X-ray absorption spectroscopy measurement according to claim 1, characterized in that, A solution cavity (3) is provided on the outer shell (1) and on one side of the square optical window (2). The solution cavity (3) is composed of a trapezoidal liquid storage groove (11) and a reaction chamber (10). The trapezoidal liquid storage groove (11) is located on one side of the reaction chamber (10).
3. The in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement according to claim 1, characterized in that, The two channels (14) are arranged opposite each other.
4. The in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement according to claim 2, characterized in that, The outer casing (1) has through holes on both sides, and an inlet pipe (8) and an outlet pipe (9) are fixedly installed in the two through holes respectively.
5. The in-situ cell for rapid continuous synchrotron radiation X-ray absorption spectroscopy measurement according to claim 4, characterized in that, The outer shell 1 (1) and the outer shell 2 (4) are provided with round holes at the four corners, and the round holes are connected to fastening bolts (12) for fixing the outer shell 1 (1) and the outer shell 2 (4).
6. The in-situ cell for rapid continuous synchrotron radiation X-ray absorption spectroscopy measurement according to claim 1, characterized in that, A waterproof gasket is attached between the outer shell one (1) and the outer shell two (4) to improve the sealing of the reaction tank.
7. The in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement according to any one of claims 1-6, characterized in that, Both the outer shell one (1) and the outer shell two (4) are made of polyetheretherketone.
8. The in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement according to claim 1, characterized in that, The square optical window (2) is sealed with a Kapton film (15).
9. The in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement according to claim 2, characterized in that, The square optical window (2) is closely fitted with the working electrode (7). The working electrode (7) is fixed with a conductive tape (13) at its edge. The conductive tape (13) is sandwiched between the outer shell (1) and the outer shell (4) and led out.
10. The in-situ cell for rapid continuous synchrotron X-ray absorption spectroscopy measurement according to any one of claims 1-6, characterized in that, The channel (14) is a quadrangular frustum, wherein the angle between the frustum and the horizontal is 45 degrees.