Design and testing method of in-situ xrd micro-electrolysis cell with foamed metal electrode

Abstract

The application provides a design and testing method of an in-situ X-ray diffraction (XRD) micro-electrolysis cell of a foamed metal base electrode, that is, under preset working conditions of high precision and long-time monitoring, the X-ray in-situ tracking of material structure change is realized by stabilizing the electrolyte liquid level; the specific process of maintaining the constant electrolyte liquid level is as follows: the constant of the liquid level height is maintained by controlling the liquid adding speed through the liquid adding device with a peristaltic pump. In the application, the heavy metal sheet of the anti-air scattering accessory is used to block stray light and direct light, which greatly improves the signal-to-noise ratio of the low-angle diffraction peak, and does not affect the signal amount of the high-angle diffraction peak, so as to improve the sensitivity of the in-situ XRD detection; in the application, the long-time in-situ monitoring and the constant liquid level greatly reduce the interference of other environmental factors, and the purity of the voltage and current driving in-situ reaction is reserved.

Description

Technical Field

[0001] This invention relates to the field of electrochemical technology, and in particular to the design and testing method of an in-situ XRD microelectrolysis cell for foam metal electrodes. Under preset operating conditions with high precision and long-term monitoring, in-situ tracking of material structural changes is achieved by maintaining a constant electrolyte level. Background Technology

[0002] When it comes to catalytic processes involving the liquid phase, offline (or near-in-situ) tests are usually used to examine changes in the catalyst. However, the start-up and shutdown processes often deviate from the actual state of the reaction process, making it difficult to accurately reflect the true changes in the catalyst itself.

[0003] X-ray diffraction (XRD) technology has been widely used to reveal the chemical composition, crystal structure, and electronic structure of materials. Real-time detection of structural changes in catalysts during catalysis using XRD technology can effectively characterize the true active sites of materials. However, in-situ monitoring involves liquid-phase catalysis, and the presence of the liquid phase can affect the precision and accuracy of in-situ XRD testing. Therefore, these inherent contradictions determine the challenge and breakthrough potential of in-situ XRD testing under liquid-phase conditions. Current in-situ XRD techniques are mostly used for all-solid-phase reactions (such as those under thermal, optical, mechanical, and electrical influences), with few involving in-situ XRD operations under liquid-phase conditions (such as electrochemical water oxidation to hydrogen, electrochemical hydrogen peroxide production, and organic substrate oxidation). Under liquid-phase conditions, not only is it necessary to construct a matching electrolytic cell to accommodate acidic or alkaline electrolytes, but also sufficient space is required to accommodate the catalytic monomers (such as the working electrode, reference electrode, and counter electrode required for electrochemical water oxidation catalysis) while minimizing interference with X-ray collection. Furthermore, unlike solid-phase in-situ XRD, catalysts in liquid-phase XRD are mostly supported in powder form on the surface of irregular electrodes such as metal foam and carbon cloth. The low catalyst content and uneven surface significantly affect signal intensity and collection. Therefore, the main problems and challenges currently facing liquid-phase in-situ XRD are as follows:

[0004] 1) The surface of foam metal (such as foam nickel, foam iron, foam cobalt and foam copper) electrodes is uneven, and the detectable XRD diffraction signal is not strong.

[0005] 2) The content of electrochemically active reactants loaded on the surface of the foam metal electrode is low and the particle dispersion is high, so the amount of signal that can be measured is very limited.

[0006] 3) During the electrochemical in-situ reaction, the amount of phase change is relatively low (e.g., the process of a new phase emerging from nothing), and there are interference peaks in both traditional beryllium windows and polytetrafluoroethylene electrolytic cells. Furthermore, signal reception at low potentials and low angles is difficult, which poses a great challenge to in-situ XRD detection.

[0007] 4) The consumption and volatilization of the electrolyte solution required for the electrochemical process affect the diffraction signal. How to balance the electrochemical reaction process with accurate in-situ XRD monitoring is also a key issue that urgently needs to be addressed. However, there are currently few reports of mature design schemes and experimental conditions for tracking the electrochemical in-situ processes of foam metal-based electrode materials. Summary of the Invention

[0008] To overcome the shortcomings of existing technologies, the purpose of this invention is to provide a design and testing method for an in-situ XRD microelectrolysis cell for foam metal electrodes. This method enables in-situ X-ray tracking of material structural changes under preset operating conditions with high precision and long-term monitoring, achieved through a constant electrolyte level.

[0009] To achieve the above objectives, the present invention provides the following solution:

[0010] The design and testing method of an in-situ XRD microelectrolysis cell for foam metal electrodes, under preset operating conditions, achieves in-situ X-ray tracking of material structural changes by stabilizing the electrolyte level, including:

[0011] The prepared electrode sheet is placed in the in-situ cell; the electrode sheet includes: a working electrode, a counter electrode, and a reference electrode;

[0012] The original standard sample stage was removed, leaving only the sample stage base. A motor was used to drive the precise movement of the micro-electrolysis cell. The micro-electrolysis cell was fixed to the sample stage base. The height of the electrode plates in the in-situ cell was adjusted.

[0013] The in-situ cell is aligned with the xy horizontal plane and the center of the goniometer to produce optimal diffraction; a heavy metal sheet is placed on the suspension beam of the goniometer; the heavy metal sheet includes any one of platinum sheet, gold sheet and lead sheet;

[0014] With the working electrode in a dry state, the first scanning parameters are set, and an X-ray diffraction pattern is acquired through a two-dimensional detector to determine the position of the reference diffraction peak.

[0015] Electrolyte was added to the in-situ cell, and the Z-height scan was finely adjusted again using measurement software to locate the expected diffraction peak position and optimize the expected diffraction peak intensity.

[0016] The second scanning parameters of the X-ray diffractometer were set in combination with the changes in the applied voltage, and the diffraction patterns of in-situ X-ray diffraction were collected under long-term operating conditions.

[0017] A liquid feeder with a peristaltic pump is used to control the liquid feeding rate and maintain a constant liquid level. Data is collected and automatically saved using measurement software to observe the changes in diffraction peak positions under an applied voltage, and to analyze and obtain changes in lattice constant, grain size, crystallinity, and structure.

[0018] Preferably, the working electrode is a foamed metal electrode sheet, including but not limited to one or more of foamed nickel, foamed iron, foamed copper, and foamed cobalt; the counter electrode is a platinum wire; and the reference electrode is a platinum wire, a silver / silver chloride electrode, or a mercury / mercury oxide electrode.

[0019] Preferably, adjusting the height of the electrode sheet in the in-situ cell includes:

[0020] The height of the electrode sheet is adjusted by using a motor-driven micro-electrolysis cell;

[0021] Based on the Zscan scanning mode, the sample stage base carrying the micro-electrolysis cell is scanned from high to low light intensity to determine whether the height is the set height;

[0022] After determining the height, use a laser to confirm its suitability.

[0023] Preferably, the thickness of the heavy metal sheet is 1.0-5.0 mm, the length is 1.0-5.0 cm, and the height is 1.0-10.0 cm.

[0024] Preferably, the heavy metal sheet is fixed to the suspension beam by a flexible material; the distance between the lower edge of the heavy metal sheet and the surface of the working electrode ranges from 0.1 to 10.0 mm.

[0025] Preferably, the first scanning parameters are: 2theta in the range of 5-120°, scanning speed in the range of 0.1-0.5s / step, and step size in the range of 0.01-0.05° / step.

[0026] Preferably, the second scanning parameters are: a scanning speed of 0.1-0.5 s / step, a step size of 0.01-0.05° / step, and a scanning angle range of 5-120°.

[0027] Preferably, the preset operating conditions include high signal-to-noise ratio data and continuous testing for at least 5 hours; wherein, the high signal-to-noise ratio data has a signal-to-noise ratio higher than 100; the preset operating conditions include, but are not limited to, single or multiple superimposed XRD scans.

[0028] Preferably, the applied voltage is -1.0V to 2.0V.

[0029] Preferably, it is used for precise testing of electrochemical electrode structures under long-term operating conditions.

[0030] According to specific embodiments provided by the present invention, the present invention discloses the following technical effects:

[0031] This invention provides a design and testing method for an in-situ XRD microelectrolysis cell for foam metal electrodes. Under preset operating conditions of high precision and long-term monitoring, in-situ X-ray tracking of material structure changes is achieved by stabilizing the electrolyte level. The method includes: mounting a prepared electrode sheet in the in-situ cell; the electrode sheet includes a working electrode, a counter electrode, and a reference electrode; removing the original standard sample stage, leaving only the sample stage base, and using a motor to drive the precise movement of the microelectrolysis cell; fixing the microelectrolysis cell onto the sample stage base; adjusting the height of the electrode sheet in the in-situ cell; aligning the in-situ cell with the xy-plane and the center of the goniometer to produce optimal diffraction; and placing a heavy metal sheet on the suspension beam of the goniometer; the heavy metal sheet includes any of platinum, gold, and lead sheets. An invention involves setting first scanning parameters for the working electrode in a dry state and acquiring X-ray diffraction patterns using a two-dimensional detector to determine the reference diffraction peak positions. Electrolyte is added to an in-situ cell, and the Z-height scan is finely adjusted using measurement software to locate the expected diffraction peak positions and optimize the expected diffraction peak intensities. Second scanning parameters of the X-ray diffractometer are set based on changes in the applied voltage, and in-situ X-ray diffraction patterns are collected under long-term operating conditions. A liquid feeder with a peristaltic pump is used to control the liquid feed rate and maintain a constant liquid level. High-precision data is collected and automatically saved using measurement software to observe changes in diffraction peak positions under applied voltage, and to analyze changes in lattice constant, grain size, crystallinity, and structure. This invention significantly improves the signal-to-noise ratio of the diffraction signal and enhances the sensitivity of in-situ XRD detection. Attached Figure Description

[0032] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0033] Figure 1 A flowchart of the testing method provided in an embodiment of the present invention;

[0034] Figure 2 This is a schematic diagram of the electrode mounting position provided in an embodiment of the present invention;

[0035] Figure 3 This is a graph showing the relationship between voltage, current, and time during an electrochemical test, provided in an embodiment of the present invention.

[0036] Figure 4 This is a schematic diagram showing the in-situ XRD changes of the catalyst under different voltage conditions provided in the embodiments of the present invention;

[0037] Figure 5The XRD pattern provided in this embodiment of the invention is without an air scattering device. Detailed Implementation

[0038] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0039] The purpose of this invention is to provide a design and testing method for an in-situ XRD microelectrolysis cell for foam metal electrodes, which can improve the sensitivity of in-situ XRD detection.

[0040] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0041] Figure 1 A flowchart of the testing method provided in the embodiments of the present invention is shown below. Figure 1 As shown, this invention provides a design and testing method for an in-situ XRD microelectrolysis cell of a foam metal electrode. Under preset operating conditions, by stabilizing the electrolyte level, in-situ X-ray tracking of material structure changes is achieved, including:

[0042] Step 100: The prepared electrode sheet is placed in the in-situ cell; the electrode sheet includes: a working electrode, a counter electrode, and a reference electrode;

[0043] Step 200: Remove the original standard sample stage, leaving only the sample stage base; use a motor to drive the precise movement of the micro-electrolysis cell; fix the micro-electrolysis cell onto the sample stage base; adjust the height of the electrode plates in the in-situ cell.

[0044] Step 300: Align the in-situ cell with the xy horizontal plane and the center of the goniometer to produce optimal diffraction; a heavy metal sheet is placed on the suspension beam of the goniometer; the heavy metal sheet includes any one of platinum, gold, and lead sheets;

[0045] Step 400: With the working electrode in a dry state, set the first scanning parameters and acquire an X-ray diffraction pattern using a two-dimensional detector to determine the reference diffraction peak position;

[0046] Step 500: Add electrolyte to the in-situ cell, and use measurement software to finely adjust the Z height scan again to locate the expected diffraction peak position and optimize the expected diffraction peak intensity.

[0047] Step 600: Set the second scanning parameters of the X-ray diffractometer in combination with the change of the applied voltage, and collect the diffraction pattern of in-situ X-ray diffraction under long-term operating conditions;

[0048] Step 700: Using a liquid dispenser equipped with a peristaltic pump, the liquid dispensing rate is controlled to maintain a constant liquid level. Data is collected and automatically saved using measurement software to observe changes in diffraction peak positions under an applied voltage, and to analyze and obtain changes in lattice constant, grain size, crystallinity, and structure.

[0049] To address the characteristics of different foam metal-based electrode materials, the long-term operating conditions described in this solution include, but are not limited to, single or multiple superimposed XRD scans, in order to more clearly reveal the structural features of the electrode; and it is operable under an applied voltage of -1.0V to 2.0V (relative to the standard hydrogen electrode) to reflect the structural changes of the electrode material in different reduction and oxidation states.

[0050] In this embodiment, taking advantage of the hardware features of the in-situ X-ray diffractometer, a target line focal plane and a two-dimensional detector are added. The standard sample stage is removed, leaving only the sample stage base, which holds a circular in-situ cell (5.0 cm in diameter, 0.85 cm in depth, 0.2 cm in wall thickness, made of PMMA polymer). A nickel foam electrode sheet is placed in the in-situ cell as the working electrode, and an electrode wire is led out using platinum wire. Another platinum wire serves as both the counter and reference electrode, connected to an external electrochemical workstation. A voltage is applied to the working electrode, and in-situ XRD is used to reconstruct the in-situ structural phase transition process. This process involves numerous challenges, such as the positioning of the effective sample electrode sheet height, the adjustment of sample flatness, the complexity introduced by the addition of electrolyte, and the improvement of the signal-to-noise ratio of low-angle diffraction peaks.

[0051] Optionally, the specific steps of the testing process in this embodiment are as follows:

[0052] Test method:

[0053] Step 1: Sample Preparation: Place the prepared electrode sheet into the in-situ cell 4; install the working electrode 1, counter electrode 2, and reference electrode 3, as follows. Figure 2 As shown; electrolyte 5 is provided in the in-situ pool 4.

[0054] The original standard sample stage was removed, leaving only the sample stage base. Its motor was used to drive the precise movement of the micro-electrolysis cell; the micro-electrolysis cell was then fixed to the sample stage base.

[0055] Step 2: Determining the height of the in-situ cell: The height of the electrode sheet in the in-situ cell is adjusted to a suitable height by driving the sample stage base carrying the micro-electrolysis cell with a precision motor (the equipment performs Zscan scanning mode, scanning the micro-electrolysis cell from high to low light intensity). After determining the height, the suitability of the height is confirmed again with a laser.

[0056] Step 3: The in-situ cell is aligned with the xy-plane horizontally and the center of the goniometer. The laser is then used again to center the sample, leveling it within the xy-plane to achieve optimal diffraction. Because the laser system and visualization hardware occupy space above the sample stage, commercial in-situ XRD hardware does not allow for the installation of commercial air scattering protection devices (X-ray diffractometer components) on the existing goniometer. This results in high direct light flux during low-angle testing, directly causing extremely poor signal-to-noise ratio in sample diffraction, making diffraction peaks virtually unobservable. Therefore, an accessory with air scattering protection and direct light blocking was designed for this step. In this implementation, a platinum sheet with a thickness of 1.0 mm, a length of 3.0 cm, and a height of 5.0 cm is used. This sheet is fixed to the beam using clamps and flexible materials, with the lower edge of the sheet approximately 5.0 mm from the working electrode surface, blocking stray and direct light. This significantly improves the signal-to-noise ratio of low-angle diffraction peaks without affecting the signal intensity of high-angle diffraction peaks.

[0057] Step 4: With working electrode 1 dry, set appropriate scanning parameters, such as a 2theta range of 5-80 degrees, a scan rate of 0.1-0.5 s / step, and a step size of 0.02. ° The X-ray diffraction pattern is then acquired using a two-dimensional detector to locate the reference diffraction peak. At this point, the signal-to-noise ratio of the low-angle diffraction peaks is primarily adjusted using a handcrafted anti-air scattering accessory (i.e., a platinum plate).

[0058] Step 5: Add electrolyte to the in-situ cell 4 to an appropriate height, and then, using the measurement software, perform a fine adjustment of the Z-height scan to locate the expected diffraction peak position and optimize the peak intensity.

[0059] Step 6: Combine the changes in the applied voltage (e.g., from -1.0V to 2.0V (relative to the standard hydrogen electrode)) to set the scanning parameters of the X-ray diffractometer (scan speed 0.1-0.5s / step, step size 0.02° / step, scanning angle range 5-80°) and collect the diffraction patterns of in-situ X-ray diffraction.

[0060] Step 7: As time progresses, the electrolyte level will drop. At this point, a liquid feeder 8 equipped with a peristaltic pump is used to control the liquid feed rate and maintain a constant liquid level. Since the in-situ experiment is a long-term overnight test, measurement software is used to program and automatically save the collected data to track and reconstruct the in-situ phase transition process. This allows for observation of the changes in diffraction peak positions under the applied voltage, and analysis to obtain changes in lattice constant, grain size, crystallinity, and structure.

[0061] To better illustrate the feasibility of implementing this plan, such as Figure 2As shown, this embodiment describes the electrochemical catalytic water splitting of a foam metal catalyst with surface-supported NiFe, NiCo, and FeCo (nickel-iron, nickel-cobalt, iron-cobalt) hydroxides (and hydroxyl oxides). Pt wire was used as the counter electrode and reference electrode, and KOH (0.1-1.0 mol / L) solution was used as the electrolyte. A modified in-situ XRD system was used to test and monitor the structural changes of the catalyst under different voltage conditions in real time. Figure 3 This diagram illustrates the relationship between voltage, current, and time during electrochemical testing, as provided in this embodiment of the invention. The changes in the catalyst for electrochemical water splitting were tested in situ at voltages of 1.3V, 1.4V, and 1.5V relative to the standard hydrogen electrode potential. Stabilization for 300-900 seconds was required before testing at each potential. The different currents in the electrochemical testing system under different potentials reflect the different electrochemical states of the catalyst under different testing conditions.

[0062] like Figure 4 and Figure 5 As shown, in this embodiment, under different electrochemical catalytic water splitting voltages, the same XRD operating conditions (e.g., scan rate 0.1-0.5 s / step, step size 0.02° / step, and scan range 5-50°) were controlled, and X-ray diffraction patterns of the electrochemical in-situ testing process were acquired using a two-dimensional detector. The XRD peak at 2θ = 44.5° (a characteristic peak of the nickel foam substrate) was used for spectral correction. The peaks at 2θ = 25-35° were mainly caused by the electrolyte diffused on the nickel foam substrate. As the voltage increased from 1.3V to 1.5V, the XRD peak at 2θ = 11.8° shifted to a higher angle, indicating that the lattice parameters of this material decreased with increasing water splitting voltage, thus reflecting the structural changes of the material during the electrocatalytic process.

[0063] The beneficial effects of this invention are as follows:

[0064] (1) The present invention has an in-situ cell that can accommodate various electrode forms: an in-situ detection method suitable for electrocatalytic processes of small amounts of active substances on the surface of pleated, hollow foam metal-based electrodes is designed.

[0065] (2) It can detect diffraction signals covering a wide range (from low angle to high angle, 2theta = 5-120°), and has a high signal-to-noise ratio with no spurious peak interference in the entire range, which is better than the currently reported in-situ electrochemical experimental design scheme.

[0066] (3) Reduce the in-situ process of electrocatalysis to obtain information such as phase, cell parameters, crystallinity, and grain size of the active material on the foam metal surface;

[0067] (4) It restores detailed information such as the change trend of the corresponding structure during the voltage change process, which greatly expands the application field of in-situ XRD.

[0068] (5) This invention is applicable to in-situ XRD detection of most thin films and bulk materials with irregular surfaces.

[0069] (6) The air scattering protection device involved in this invention is a novel design that greatly improves the signal-to-noise ratio of the diffraction signal and enhances the sensitivity of in-situ XRD detection.

[0070] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. The same or similar parts between the various embodiments can be referred to each other.

[0071] This document uses specific examples to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of the present invention. Furthermore, those skilled in the art will recognize that, based on the ideas of the present invention, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. A design and testing method for an in-situ XRD microelectrolysis cell with foamed metal electrodes, characterized by achieving in-situ X-ray tracking of material structure changes under preset working conditions with high precision and long-term monitoring, by stabilizing the electrolyte level. include: The prepared electrode sheet is then placed in the in-situ cell; The electrode sheet includes: a working electrode, a counter electrode, and a reference electrode; the working electrode is a foamed metal electrode sheet. The original standard sample stage was removed, leaving only the sample stage base. A motor was used to drive the precise movement of the micro-electrolysis cell. The micro-electrolysis cell was fixed to the sample stage base. The height of the electrode plates in the in-situ cell was adjusted. The in-situ cell is aligned with the xy-plane and the center of the goniometer to produce optimal diffraction; a heavy metal sheet is placed on the suspension beam of the goniometer; the heavy metal sheet includes any one of platinum, gold, and lead sheets; the heavy metal sheet is fixed to the suspension beam by a flexible material; the distance between the lower edge of the heavy metal sheet and the surface of the working electrode ranges from 0.1 to 10.0 mm. With the working electrode in a dry state, the first scanning parameters are set, and an X-ray diffraction pattern is acquired through a two-dimensional detector to determine the position of the reference diffraction peak. Electrolyte was added to the in-situ cell, and the Z-height scan was finely adjusted again using measurement software to locate the expected diffraction peak position and optimize the expected diffraction peak intensity. The second scanning parameters of the X-ray diffractometer were set in combination with the changes in the applied voltage, and the diffraction patterns of in-situ X-ray diffraction were collected under long-term working conditions of 5-24 hours. A liquid feeder with a peristaltic pump is used to control the liquid feeding rate and maintain a constant liquid level. High-precision data is collected and automatically saved using measurement software to observe the changes in diffraction peak positions under an applied voltage, and to analyze and obtain changes in lattice constant, grain size, crystallinity, and structure.

2. The design and testing method of the in-situ XRD microelectrolysis cell for foam metal electrodes according to claim 1, characterized in that, The foamed metal electrode sheet includes one or more of foamed nickel, foamed iron, foamed copper, and foamed cobalt; the counter electrode is a platinum wire; and the reference electrode is a platinum wire, a silver / silver chloride electrode, or a mercury / mercury oxide electrode.

3. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to claim 1, characterized in that, Adjusting the height of the electrode plates in the in-situ cell includes: The height of the electrode sheet is adjusted by using a motor-driven micro-electrolysis cell; Based on the Z scan mode, the light intensity of the sample stage base carrying the micro-electrolysis cell is scanned from high to low to determine whether the height is the set height; After determining the height, use a laser to double-check its suitability.

4. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to claim 1, characterized in that, The thickness of the heavy metal sheet is 1.0-5.0 mm, the length is 1.0-5.0 cm, and the height is 1.0-10.0 cm.

5. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to claim 1, characterized in that, The first scanning parameters are as follows: 2theta ranges from 5 to 120°, the scanning speed ranges from 0.1 to 0.5 s / step, and the step size ranges from 0.01 to 0.05° / step.

6. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to claim 1, characterized in that, The second scanning parameters are as follows: scanning speed is 0.1-0.5 s / step, step size is 0.01-0.05° / step, and scanning angle range is 5-120°.

7. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to claim 1, characterized in that, The preset operating conditions include high signal-to-noise ratio data and continuous testing for at least 5 hours; wherein, the signal-to-noise ratio of the high signal-to-noise ratio data is higher than 30; the preset operating conditions include, but are not limited to, single or multiple superimposed XRD scans.

8. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to claim 1, characterized in that, The applied voltage is -1.0V to 2.0V.

9. The design and testing method of the in-situ XRD microelectrolysis cell for the foam metal electrode according to any one of claims 1-8, characterized in that, It is used for precise testing of electrochemical electrode structures under long-term operating conditions.

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