In-situ X-ray total reflection testing device suitable for potential adding

Abstract

The in-situ X-ray total reflection testing device comprises a main body, a circular cover, an entrance / exit window film, an O-shaped ring, a reference / counter electrode through hole bolt, a liquid (gas) inlet / outlet through hole bolt, a working electrode tab, a current collector and an inner hexagonal screw. Wherein the main body is provided with an opening for light paths of different wavelengths and a reference / counter electrode through hole bolt corresponding through hole; the liquid (gas) inlet and outlet through hole bolt corresponds to the through hole; the working electrode tab corresponds to the through hole; and the hexagon socket screws are correspondingly provided with holes. The light path opening in the main body is opposite to the light path openings of the two circular covers; the incident window protection film and the emergent window protection film are positioned between the O-shaped ring and the circular covers; and the circular cover and the main body are connected in a sealed and detachable manner. The in-situ testing device is suitable for in-situ testing of a synchrotron radiation total reflection table interface structure capable of controlling parameters such as applied potential current and the like, and meets testing of small-angle / wide-angle scattering of a grazing-in angle, Raman / infrared and the like.

Description

Technical Field

[0001] The invention relates to the field of small scientific experimental devices, in particular to an in-situ X-ray total reflection testing device suitable for applying a potential. Background Art

[0002] Thin film technology is widely used in electronic devices, semiconductors, and energy fields such as electrolytes, optical / electrode coatings, thin film sensors, and solar cells. By regulating the surface thickness, composition, and microstructure of the thin film, the physical, chemical, and mechanical properties of the material can be precisely adjusted to meet the needs of specific applications.

[0003] Take the membrane electrode assembly (MEA) of hydrogen fuel cells as an example. MEA is a composite thin electrode and the core component of proton exchange membrane fuel cells. Membrane electrodes are often used in fuel cells. They include a solid polymer electrolyte membrane with catalyst / ionomer mixed coatings on both sides. For example, the catalyst surface of the membrane electrode in hydrogen fuel cells is attached with ionomers with a thickness of several nanometers to tens of nanometers. The surface morphology and crystallization behavior of these electrolytes determine the material transfer rate of carriers. Therefore, analyzing the surface microstructure of nanoscale ionomers is conducive to studying the evolution mechanism of the various influencing factors of the electrode / electrolyte interface on the microstructure and morphology and the establishment of structure-activity relationship, which is the key to improving the performance of hydrogen fuel cells. The synchrotron radiation grazing-angle small-angle / wide-angle X-ray scattering (GISAXS / GIWAXS) in-situ testing technology is a total reflection surface interface characterization method with the advantages of high collimation and high brightness. It can generate evanescent waves in the thin film sample by adjusting the angle of the incident light to obtain the microscopic structure information of the surface interface sample at different depths, the ordered structure in the plane, the out-of-plane crystal structure, and the functional group information. It is widely used in the field of characterizing inorganic and polymer surfaces.

[0004] Since the performance of membrane electrodes is affected by factors such as voltage and temperature in actual operation and needs to be operated in a complex and challenging environment, previous non-in-situ tests cannot truly reflect the microstructure of the catalyst and ionomer interface under real conditions. Therefore, it is necessary to test the structural changes and reaction behaviors of membrane electrodes under conditions close to actual working conditions. However, the current in-situ test devices for surface and interface structures mainly have the following problems: (1) For example, the existing in-situ infrared / Raman or X-ray absorption spectra (fluorescence method) cannot obtain structural information of samples with very small amounts of material (nanofilms, nanocatalysts, quantum dots) through transmission methods. That is, since there is no effective interaction distance between light and samples, the results usually have a poor signal-to-noise ratio; (2) Grazing angle small angle / wide angle scattering is a type of total reflection technology, and its incident light and outgoing light are on the same side relative to the sample surface. This makes it difficult to observe the microstructural changes of membrane electrodes under applied potential conditions because the external electrodes will form spatial interference with the sample and hinder the propagation of the light path when constructing a primary cell / electrolyzer system.

[0005] In summary, there is an urgent need to propose a device for testing the surface and interface structure of nanomaterials such as ionomers under different atmospheres and variable potential conditions. Summary of the invention

[0006] The purpose of the present invention is to provide an in-situ X-ray total reflection testing device suitable for applying a potential, so as to solve the problems that it is difficult to characterize the anisotropy of the surface interface in the in-plane and out-plane directions under the in-situ testing environment (atmosphere, oxidation / reduction potential), and the heterogeneous structure changes with the environment.

[0007] The present invention provides an in-situ X-ray total reflection testing device suitable for applying a potential, comprising:

[0008] main body;

[0009] A hollow cavity is provided at the center of the main body;

[0010] A hollow cavity, capable of passing electrolyte or gas;

[0011] A current collector is provided at the lower side of the hollow cavity, and the sample to be tested is placed on the current collector and connected to an external electrochemical workstation through the working electrode tab;

[0012] Through holes are provided on both sides of the main body, and the through holes correspond to two electrode through-hole bolts, which are used to place the reference electrode and the counter electrode through-hole bolts; two internal threaded through holes are provided on the top of the main body, which penetrate into the central cavity and are used to place the liquid (gas) inlet and outlet through-hole bolts;

[0013] The sample to be tested is fixed by two bolts for liquid (gas) inlet and outlet;

[0014] Both ends of the main body also include symmetrically arranged window films, O-rings, and circular covers;

[0015] An incident window and an exit window are respectively arranged at the center of the circular cover, serving as irradiation channels for light of different wavelengths.

[0016] The hexagon socket screws are inserted through the circular cover, the entrance / exit window membrane and the O-ring in sequence and then tightened to embed into the corresponding screw holes on the main body. By tightening the hexagon socket screws and squeezing the O-rings, a closed environment is constructed for the system to be tested in the center of the main body to prevent the electrolyte from flowing out or gas leakage.

[0017] Wherein, the circular cover is a circular upper cover or a circular bottom cover.

[0018] The electrode through-hole bolts include reference electrode through-hole bolts and counter electrode through-hole bolts.

[0019] The window film includes an incident window film and an exit window film.

[0020] Furthermore, an O-ring is placed in an O-ring groove at the contact point between the main body and the circular cover, and an incident window membrane and an exit window membrane are arranged between the circular cover and the main body, and are inserted into corresponding screw holes on the main body after passing through the circular cover, the incident window membrane or the exit window membrane through an inner hexagon screw. The inner hexagon screw is tightened to tightly fit and fix the circular cover, the incident or exit window membrane to the main body.

[0021] Among them, the incident window film and the exit window film are films with excellent insulation strength, electrical strength, thermal conductivity efficiency, and resistance stability. These characteristics enable them to have high temperature control accuracy in the heating field. In addition, the incident window film and the exit window film occupy a small space and have good flexibility. The size and shape of the incident window film and the exit window film are designed according to the required situation.

[0022] Furthermore, the O-ring is made of metal or non-metal material, used for sealing installation between two or more components, and is made of rubber.

[0023] Furthermore, the reference electrode and the counter electrode are placed in the through-hole bolts corresponding to the through-holes on both sides of the main body, and the bolts are tightened to form an overall sealed test environment.

[0024] Furthermore, the working electrode is placed in a through hole on one side of the main body to form an overall sealed test environment.

[0025] Furthermore, an O-ring groove is provided on the side where the main body contacts the circular cover. The diameter of the O-ring groove is larger than the diagonal size of the central cavity of the main body and smaller than the diagonal size of the main body. The O-ring is squeezed by tightening the hexagon socket screw to seal the incident window membrane and the exit window membrane. The circular cover is provided with a plurality of threaded openings; the positions of the threaded openings coincide with the positions of the threaded openings provided on the main body, and the incident and exit windows are provided at the center of the circular cover.

[0026] Furthermore, the incident window film and the exit window film are made of polyimide, which is a material that can transmit light of different wavelengths and produces almost no background.

[0027] The assembly steps of an in-situ X-ray total reflection test device suitable for applying a potential provided by the present invention are as follows:

[0028] Place the substrate coated with the membrane electrode on the current collector to ensure that there is no gap as much as possible, and tighten the two fixing screws on the lower side of the cavity to fix the substrate. Spin the electrolyte evenly on the substrate as a test sample by spin coating, or deposit inorganic powder on the substrate by magnetron sputtering.

[0029] Place the O-ring into the O-ring groove on the side where the main body contacts the circular cover. Using organic soft materials can make the material fully elastic, which can effectively avoid damage such as bending caused by operating errors compared to rigid or hard materials.

[0030] Place the incident window membrane and the exit window membrane between the main body and the circular upper / bottom cover, press them together, and screw the hexagon socket screws through the threaded holes on the circular cover into the main body to fix it. Screw the reference electrode and counter electrode through-hole bolts on both sides into the corresponding bolt through-holes on the side of the main body, and screw the working electrode tab on one side into the corresponding through-hole on the main body.

[0031] Screw one of the liquid (gas) inlet / outlet through-hole bolts on the top of the main body into the main body to fix the sample surface interface below, and screw the other bolt into the main body after the electrolyte is injected.

[0032] The circular cover of the present invention covers the incident window film and the exit window film, and makes the four hexagon socket screw openings on the main body, the window film and the circular covers on both sides completely correspond. This method of positioning by opening the device eliminates the misalignment phenomenon during the assembly process.

[0033] The present invention provides an in-situ X-ray total reflection testing device suitable for applying a potential, which has the following beneficial effects:

[0034] (1) Based on the structure of the incident light port and the exit light port of the device, the incident window film and the exit window film used have the advantage of good light transmittance; the multimodal combination can meet the research needs of realizing the synchrotron radiation total reflection method of different wavelengths in one device, simplifying the experimental process; combining X-ray total reflection technology with Raman spectroscopy, infrared spectroscopy, etc., the use of this device can not only realize the precise control of the applied potential, current and other information, but also make the experimental results obtained from the test provide more comprehensive information.

[0035] (2) The O-ring is squeezed to seal the rigid parts, and cold packaging is used throughout the entire device process. The assembly process has loose environmental requirements, which facilitates experiments at room temperature.

[0036] (3) The insertion depth of the counter electrode and the reference electrode can be adjusted according to the actual situation, which effectively reduces the electrode polarization caused by the liquid resistance and provides a guarantee for the accuracy of electrochemical in-situ measurement.

[0037] (4) Use materials with high chemical and mechanical stability as the main material. The main material has excellent machinability, hardness and electrical insulation, and can also take into account the corrosion of strong acids and alkalis, expanding the experimental system that can be used.

[0038] (5) By introducing in-situ testing of small-angle / wide-angle scattering of light of different wavelengths at grazing angles into the fine structure characterization test of the catalyst on the surface electrode, real-time characterization test of the fine structure of the catalyst on the electrode during the reaction process is achieved; this makes up for the difference in activity evaluation between the experimental test system and the actual reaction process system, and provides a basis for proposing a correction plan for the activity evaluation of fuel cells in the industrial system.

[0039] (6) The in-situ testing device for surface and interface structure using the synchrotron radiation total reflection method provided by the present invention can be reused multiple times after the test by steps such as disassembly, cleaning, and replacement of electrode materials, which not only reduces costs but also enhances the repeatability of the experiment. The components of the device are modularly processed, and the processing dimensions can be adjusted according to actual conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the prior art descriptions are briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention, and for ordinary technicians in this field, other drawings can be obtained based on these drawings without creative labor.

[0041] Figure 1 A schematic structural diagram of an in-situ X-ray total reflection testing device suitable for applying a potential provided by the present invention.

[0042] Figure 2 A cross-sectional view of an in-situ X-ray total reflection testing device suitable for applying a potential provided by the present invention.

[0043] Figure 3 Cyclic voltammogram of Pt-based catalyst measured by the device of the present invention.

[0044] Figure 4 This is the GIWAXS2D image of Nafion film tested at 95% RH and 25°C.

[0045] Original label description

[0046] 1 Main body

[0047] 2 Round cover × 2

[0048] 3. Entrance / exit window film (polyimide film, also known as Kapton film)

[0049] 4 O-ring

[0050] 5 Reference / counter electrode through-hole bolt × 2

[0051] 6 Inlet / outlet liquid (gas) through-hole bolts × 2

[0052] 7 Working electrode tab

[0053] 8 current collector

[0054] 9 Hexagon socket screw × 8 DETAILED DESCRIPTION

[0055] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand the advantages and effects of the present invention from the contents described in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details of this specification can also be modified and changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0056] In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside", etc. is based on the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention; the terms "first", "second", and "third" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance. In addition, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, an indirect connection through an intermediate medium, or a connection between the two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0057] See also Figure 1 and Figure 2 It should be noted that the illustrations provided in this embodiment are only for illustrating the basic concept of the present invention. Although the illustrations only show components related to the present invention and are not drawn according to the number, shape and size of components in actual implementation, the form, quantity and proportion of each component in actual implementation may be changed arbitrarily, and the component layout may also be more complicated.

[0058] The present invention provides an in-situ X-ray total reflection testing device suitable for applying a potential, wherein a hollow cavity is arranged at the center of the main body of the device;

[0059] A hollow cavity, capable of passing electrolyte or gas;

[0060] A current collector is provided at the lower side of the hollow cavity, which is used to place the sample to be tested thereon and connect to an external electrochemical workstation through the working electrode tab;

[0061] Through holes are provided on both sides of the main body, and the through holes correspond to two electrode through-hole bolts, which are used to place the reference electrode and the counter electrode through-hole bolts; two internal threaded through holes are provided on the top of the main body, which penetrate into the central cavity and are used to place the inlet and outlet liquid (gas) through-hole bolts;

[0062] The sample to be tested is fixed by two bolts for liquid (gas) inlet and outlet;

[0063] The two ends of the main body also include symmetrically arranged window films, O-rings, and circular covers; the center of the circular cover is respectively provided with an incident window and an exit window, which serve as irradiation channels for light of different wavelengths. The hexagon socket screws pass through the circular cover, the inlet / exit window films, and the O-rings in turn, and then are tightened and embedded into the corresponding screw holes on the main body. By tightening the hexagon socket screws and squeezing the O-rings, a closed environment is constructed for the system to be tested in the center of the main body to prevent the outflow of electrolyte or gas leakage.

[0064] The two circular covers of the present invention are specifically circular upper covers or circular bottom covers.

[0065] The two electrode through-hole bolts of the present invention are specifically a reference electrode through-hole bolt and a counter electrode through-hole bolt.

[0066] The two window films of the present invention include an incident window film and an exit window film.

[0067] The O-ring is placed in the O-ring groove where the main body and the circular cover contact. The incident window membrane and the exit window membrane are placed between the circular cover and the main body. The hexagon socket screws penetrate the circular cover, the incident window membrane or the exit window membrane and then are inserted into the corresponding screw holes on the main body. Tighten the hexagon socket screws to tightly fit and fix the circular cover, the incident or exit window membrane to the main body.

[0068] The present invention provides a specific method, wherein the O-ring is made of metal or non-metal material and is used for sealing installation between two or more components, and the rubber material is selected.

[0069] The present invention provides a specific method, in which a reference electrode and a counter electrode are placed in through-hole bolts corresponding to through-holes on both sides of a main body, and the bolts are tightened to form an overall sealed test environment.

[0070] The working electrode is placed in a through hole on one side of the main body to form an overall sealed test environment.

[0071] The sample to be tested is attached to the substrate by evaporation, spin coating, etc. The main body and the substrate are connected by precious metal materials such as Au and Pt that are not easily oxidized as current collectors. The substrate to which the sample to be tested is attached, the current collector, and the working electrode tab together constitute the working electrode.

[0072] The present invention provides a specific method, in which the main body is a rectangular parallelepiped, and there is a rectangular parallelepiped cavity inside the main body, the cavity is used to inject electrolyte, and there are two through holes corresponding to the inlet / outlet liquid (gas) through-hole bolts on the top of the cavity, which are used to inject electrolyte. The two inlet / outlet liquid (gas) through-hole bolts are tightened to fix the sample below. The openings on both sides of the main body are hollow cylinders with internal threads; the reference electrode and the counter electrode through-hole bolts are placed. The cylindrical openings on both sides of the main body are symmetrically positioned, and there is also a through hole on one side for placing the working electrode ear.

[0073] The present invention provides a specific method, wherein an O-ring groove is provided on the side of the main body in contact with the circular cover, the diameter of the O-ring groove is larger than the diagonal dimension of the central cavity of the main body and smaller than the diagonal dimension of the main body, and the O-ring is squeezed by tightening the hexagon socket screw, thereby sealing the incident window membrane and the exit window membrane. The circular cover is provided with a plurality of threaded openings; the positions of the threaded openings coincide with the positions of the threaded openings provided on the main body, and the incident and exit windows are provided at the center of the circular cover.

[0074] The present invention provides a specific method, wherein the incident window film and the exit window film are made of polyimide, which is a material that can transmit light of different wavelengths and produces almost no background.

[0075] The present invention provides a specific method, wherein the diameter of the O-ring is the same as the size of the O-ring groove on the side where the main body contacts the circular cover. The O-ring is made of natural rubber, nitrile rubber, fluororubber, silicone rubber, EPDM rubber or chloroprene rubber.

[0076] The present invention provides a specific method, wherein the through holes on both sides of the main body are threaded inside for placing reference electrode and counter electrode through hole bolts, and also for sealing. There are two circular through holes on the top of the main body that penetrate downward to the central cavity for injecting electrolyte.

[0077] The invention provides a specific mode, wherein the outer diameter of the circular cover matches the main body, and the thickness is moderate. The circular cover is provided with four symmetrically distributed screw holes and internal threads.

[0078] The assembly steps of an in-situ testing device for surface and interface structure using a synchrotron radiation total reflection method provided by the present invention are as follows:

[0079] Place the substrate coated with the membrane electrode on the current collector, ensuring that there is as little gap as possible, and tighten the two fixing screws on the lower side of the cavity to fix the substrate.

[0080] Place the O-ring into the O-ring groove on the side where the main body contacts the circular cover. Using organic soft materials can make the material fully elastic, which can effectively avoid damage such as bending caused by operating errors compared to rigid or hard materials.

[0081] Place the incident window membrane and the exit window membrane between the main body and the circular cover, press them together, and screw the hexagon socket screws through the threaded holes on the circular cover into the main body to fix it. Screw the reference electrode and counter electrode through-hole bolts on both sides into the corresponding bolt through-holes on the side of the main body, and screw the working electrode tab on one side into the corresponding through-hole in the main body.

[0082] Screw one of the liquid (gas) inlet / outlet through-hole bolts on the top of the main body into the main body to fix the substrate with membrane electrode plated below, and inject electrolyte into the other one. After injection, tighten the through-hole bolt.

[0083] The circular cover of the present invention covers the incident window film and the exit window film, and makes the four hexagon socket screw openings on the main body, the window film and the circular covers on both sides completely correspond. This method of positioning by opening the device eliminates the misalignment phenomenon during the assembly process.

[0084] Example

[0085] See also Figure 1 and Figure 2 The present invention provides an in-situ testing device for surface and interface structure using a synchrotron radiation total reflection method. The in-situ testing device comprises: a main body 1, a circular cover 2×2, a window film 3 (polyimide film, also known as Kapton film), an O-ring 4, a reference / counter electrode through-hole bolt 5×2, an inlet / outlet liquid (gas) through-hole bolt 6×2, a working electrode ear 7, a current collector 8, and a hexagon socket screw 9×8.

[0086] The circular cover 2 for fixing the main body is circular, and four screw through holes with equal diameters and evenly distributed along the circular cover are sequentially arranged on the periphery of the circular cover 2. There is a rectangular parallelepiped space in the middle of the circular cover 2, which is used for the incident light and the outgoing light to pass through respectively.

[0087] The window film 3 includes an incident window film 3 and an exit window film 3 , and the circular cover is squeezed and tightly fitted to the main body by tightening the hexagon socket screw.

[0088] The size of the O-ring 4 corresponds to the size of the groove, and is placed in the O-ring groove on the side where the main body 1 contacts the circular cover 2. The material of the O-ring 4 is generally selected to be an organic polymer material.

[0089] The membrane electrode is plated on the substrate by electroplating and attached to the current collector 8 of the main body 1.

[0090] The main body of the in-situ test device, as the main carrier, is installed in combination with the circular cover 2, the incident window membrane 3 or the exit window membrane 3, and the O-ring 4. The central space of the main body 1 is used as a container for the electrolyte, and the lower side is the current collector 8. The internal threaded holes on both sides of the main body 1 are to provide the space required for the electrodes. The through-hole bolts placed on the top provide channels for feeding and discharging. The hexagon socket screw through holes on the main body 1 used to connect with the circular cover 2 are exactly the same as the hexagon socket screw through holes evenly distributed on the circular covers 2 on both sides. The hexagon socket screws connect the main body, the window membrane, and the circular covers on both sides together, so that the main body 1, the circular cover 2, the input / exit window membrane 3 and the O-ring 4 fit tightly together. The current collector 8 serves as a carrier for the working electrode. The O-ring groove on the side where the main body 1 contacts the circular cover 2 serves as a placement channel for the O-ring.

[0091] As an example, the thickness of the circular cover 2 of the in-situ test device may not be limited to 0.5-2 cm, but on the one hand, the material of the circular cover 2 needs to be considered, and on the other hand, the thickness of the circular cover 2 needs to be considered. The overall center of gravity offset caused by the two will affect the structural stability of the entire in-situ test device. Therefore, in order to make the overall stability high and the material cost not too high and easy to process, the thickness of the circular cover 2 should not be too thick, and the length, width and height of the central cavity of the circular cover 2 can be designed according to the required conditions to ensure the range of the incident and outgoing light.

[0092] As an example, the incident window film and the exit window film have a transmittance of more than 60%, although the aluminum film also has a high transmittance of light at different wavelengths. Compared with the traditional in-situ test device using thick aluminum film and titanium plate and other materials, the present invention uses a polymer film Kapton film with good transmittance of light at different wavelengths as the window film, taking into account the in-situ test research of grazing angle small angle / wide angle scattering using low-energy light of different wavelengths (5-8keV), so that one device can perform multiple experiments, eliminating the measurement errors caused by different devices and simplifying the experimental process. At the same time, in order to ensure the airtightness during the experimental test process, the thickness of the Kapton film cannot be too thin.

[0093] The diameter of the O-ring groove on the side where the main body 1 contacts the circular cover 2 needs to be designed according to the circular cover 2 and the central area, and can be specifically designed as appropriate.

[0094] As an example, the O-ring 4 is an O-ring with elastic deformation and recovery ability. Its material can be nitrile rubber, chloroprene rubber, butyl rubber, etc. The sealing ring sealing method is adopted, and the whole process is cold packaged, and there is no need to heat and melt the polymer material for sealing. The sealing performance is good and will not cause damage to the in-situ test device. The sealing ring in the present invention can select the above O-ring.

[0095] As an example, the electrode leads of the reference electrode and the counter electrode may be but are not limited to copper wires, and the size of the electrode leads is selected according to actual needs.

[0096] In addition, the present invention provides an assembly method for an in-situ surface and interface structure test device suitable for synchrotron radiation total reflection method. Figure 2 , the installation and removal steps are as follows:

[0097] Place the substrate plated with the working electrode into the current collector on the main body, and then screw one of the inlet / outlet liquid (gas) through-hole bolts into the middle cavity of the main body until it contacts the sample on the lower current collector.

[0098] The O-ring 4 is placed in the O-ring groove on the side where the main body 1 contacts the circular cover 2 , and the incident window film and the exit window film are pressed against the inner side of the circular cover 2 .

[0099] After passing four hexagon socket screws through the circular cover 2, the incident window membrane or the exit window membrane in sequence and into the main body 1, tighten the screws to ensure that the circular covers 2, the incident / exit window membranes 3 and the O-rings 4 on both sides are in complete and tight contact with the main body 1 under the action of the hexagon socket screws.

[0100] The electrolyte is injected into the cavity area in the center of the body through the liquid (gas) through-hole bolts. The through-hole bolts are tightened in the corresponding openings to achieve a sealing effect. Ensure that the middle cavity area is in a sealed state, and screw the counter electrode and reference electrode through-hole bolts on both sides and the sensor into the body to complete the assembly.

[0101] As an example, the surface interface structure in-situ testing device suitable for synchrotron radiation disclosed in the present invention can be applied to the in-situ testing experiment of Nafion resin film on Pt substrate material, and the testing steps can be:

[0102] 1. Place the working electrode (about 1×2cm) containing the sample. 2 ) was placed on the current collector and 0.1 M HClO was added 4 Liquid electrolyte, and insert Pt wire counter electrode and Ag / AgCl reference electrode. The light inlet is facing the direction of Nafion resin film, and the position of the in-situ test device is adjusted to allow the incident light to pass through the incident window, and the experiment begins;

[0103] 2. Connect each electrode to an electrochemical workstation and perform cyclic voltammetry (e.g. Figure 3) Determine the battery working state to check the electrochemical activity of the working electrode loaded with samples to ensure that the battery is in a stable working state for experimental testing;

[0104] 3. Use constant potential method / constant current method to control voltage / current and observe the change of current / voltage over time (enter steady state) to ensure that the battery is tested in a stable working state;

[0105] 4. Select appropriate exposure time and incident angle to collect data;

[0106] 5. Turn off the electrochemical workstation.

[0107] After the test process is completed, first unscrew the liquid (gas) through-hole bolts to discharge the electrolyte in the hollow part of the body. Then remove other components in order from top to bottom and from outside to inside.

[0108] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. An in-situ X-ray total reflection test device suitable for applying a potential, characterized in that: include: main body; A hollow cavity is provided at the center of the main body; A hollow cavity, capable of passing electrolyte or gas; A current collector is provided at the lower side of the hollow cavity, and the sample to be tested is placed on the current collector and connected to an external electrochemical workstation through the working electrode tab; Through holes are provided on both sides of the main body, and the through holes correspond to two electrode through-hole bolts, which are used to place the reference electrode and the counter electrode through-hole bolts; two internal threaded through holes are provided on the top of the main body, which penetrate into the central cavity and are used to place the liquid (gas) inlet and outlet through-hole bolts; The sample to be tested is fixed by two bolts for liquid (gas) inlet and outlet; Both ends of the main body also include symmetrically arranged window films, O-rings, and circular covers; An incident window and an exit window are respectively arranged at the center of the circular cover, serving as irradiation channels for light of different wavelengths.

2. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1, characterized in that: The hexagon socket screws are passed through the circular cover, the entrance / exit window membrane and the O-ring in sequence and then tightened to be embedded into the corresponding screw holes on the main body; by tightening the hexagon socket screws and squeezing the O-rings, a closed environment is constructed for the system to be tested centered on the main body.

3. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1 or 2, characterized in that: The O-ring is placed in the O-ring groove at the contact point between the main body and the circular cover. The incident window membrane and the exit window membrane are arranged between the circular cover and the main body. The hexagon socket screw passes through the circular cover, the incident window membrane or the exit window membrane and is then embedded in the corresponding screw hole on the main body. The hexagon socket screw is tightened to tightly fit and fix the circular cover, the incident or exit window membrane to the main body.

4. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1 or 3, characterized in that: The O-ring is made of metal or non-metal material, specifically rubber material.

5. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1, characterized in that: The reference electrode and the counter electrode are placed in the through-hole bolts corresponding to the through-holes on both sides of the main body, and the bolts are tightened to form an overall sealed test environment.

6. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1, characterized in that: The working electrode is placed in a through hole on one side of the main body to form an overall sealed test environment.

7. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1, characterized in that: An O-ring groove is provided on the side of the main body that contacts the circular cover. The diameter of the O-ring groove is larger than the diagonal size of the central cavity of the main body and smaller than the diagonal size of the main body. The O-ring is squeezed by tightening the hexagon socket screw to seal the incident window membrane and the exit window membrane. The circular cover is provided with a plurality of threaded openings. The position of the threaded opening coincides with the position of the threaded opening arranged on the main body, and the incident and exit windows are arranged at the center of the circular cover.

8. The in-situ X-ray total reflection testing device suitable for applying potential according to claim 1, characterized in that: The incident window film and the exit window film are made of polyimide.

9. An assembly method for an in-situ X-ray total reflection test device suitable for applying a potential, characterized in that: The steps of this method are as follows: Place the substrate coated with the membrane electrode on the current collector to ensure that there is as little gap as possible, and tighten the two fixing screws on the lower side of the cavity to fix the substrate; evenly spin-coat the electrolyte on the substrate as a test sample by spin coating, or deposit inorganic powder on the substrate by magnetron sputtering; Place the O-ring into the O-ring groove on the side where the body contacts the round cover; Place the incident window membrane and the exit window membrane between the main body and the circular upper / bottom cover, press them together, and screw the hexagon socket screws through the threaded holes on the circular cover into the main body to fix it; screw the reference electrode and counter electrode through-hole bolts on both sides into the corresponding bolt through-holes on the side of the main body, and screw the working electrode tab on one side into the corresponding through-hole on the main body; Screw one of the liquid (gas) inlet / outlet through-hole bolts on the top of the main body into the main body to fix the sample surface interface below, and screw the other bolt into the main body after the electrolyte is injected.

10. The assembly method of the in-situ X-ray total reflection testing device suitable for applying potential according to claim 9, characterized in that: The circular cover covers the incident window film and the exit window film, and makes the four hexagon socket screw openings on the main body, the window film and the circular covers on both sides completely correspond.

Images