In-situ XRD (X-Ray Diffraction) test kit and test method for beryllium window-removed ion battery

Abstract

The invention relates to a beryllium window-free electrochemical in-situ XRD (X-Ray Diffraction) test device and a test method, and belongs to the field of battery test. The test assembly comprises a top cover, a main body, a bottom cover and an in-cavity accessory. The assembled kit can be embedded into an objective table of an XRD diffractometer. Wherein the battery main body is provided with a pole piece fixing groove and is matched with the film-coated sealing top cover, so that a good sealing test environment can be kept when no metal beryllium window exists. Through the optimized structural design, highly toxic metal beryllium commonly adopted by a traditional electrochemical in-situ kit is removed, and by adopting the kit and the corresponding testing method, electrochemical in-situ XRD testing in various electrolyte environments under the sealing condition can be achieved.

Description

Technical Field

[0001] The present invention relates to the field of in-situ XRD technology, and more specifically, to an in-situ XRD detection device and method for the reaction process of ion batteries. Background Art

[0002] Electrochemical in-situ XRD technology is a technology that combines electrochemical experiments with X-ray diffraction (XRD) analysis, and can monitor the structural changes of materials in real time during the electrochemical reaction process. This technology is widely used in fields such as battery materials, electrocatalysts, and corrosion science, helping researchers to deeply understand the crystal structure evolution, phase change behavior, and reaction mechanism of electrode materials during charge and discharge, catalytic reactions, or corrosion processes. The experimental process can be summarized as follows: by applying voltage or current to the material through an electrochemical workstation, during the process of simulating the actual electrochemical environment (such as battery charge and discharge, electrolysis of water, etc.), using X-ray diffraction technology to collect the diffraction pattern of the material in real time and analyze the change of the crystal structure.

[0003] Among them, electrochemical in-situ XRD experiments require a specially designed in-situ electrochemical cell, which must meet the requirements of the electrochemical reaction and allow X-rays to penetrate and collect diffraction signals. In traditional electrochemical in-situ XRD kits, the beryllium window is a key component, mainly because of its high mechanical strength and low atomic number, and its absorption of X-rays is very weak. Therefore, compared with other materials (such as aluminum or glass), the beryllium window can minimize the attenuation of X-rays to ensure the intensity and quality of the diffraction signal. Moreover, the beryllium window not only has high mechanical strength, but also can be closely matched with other parts of the electrochemical cell (such as polymers or metal frames) to ensure the sealing of the electrochemical cell. This sealing is particularly important for long-term experiments or experiments under high-pressure / high-temperature conditions. Beryllium shows chemical inertness in most organic electrolyte environments and is not easy to react with electrolytes or reaction products.

[0004] However, in an aqueous electrolyte environment, metallic beryllium exhibits the reaction activity common to alkaline earth metals, especially with a high reaction rate in acidic and alkaline electrolytes. This makes the corresponding electrochemical in-situ XRD test require a solution without a beryllium window. Moreover, metallic beryllium and any of its valence compounds are significantly toxic, which can cause immune responses, oxidative stress, and DNA damage, and are dangerous chemicals strictly controlled in most countries around the world, including China. And the average price of a single gram of high-purity beryllium remains at 1000 to 3000 yuan all year round, and the beryllium window is a high-cost component in the in-situ XRD kit.

[0005] Therefore, although the classical solutions of existing in-situ XRD kits with beryllium windows are relatively mature and widely used, developing a new type of standardized beryllium-free electrochemical in-situ XRD test kit and test method has important practical significance and promotion value for significantly reducing the experimental cost and the safety risks of operators, and improving the universality of the test kit. Summary of the Invention

[0006] To solve the above problems, the present application provides a beryllium-free electrochemical in-situ XRD test device and test method. The test kit designed with this structure respectively uses a pole piece limiting structure and a polymer film to replace the support and sealing of the metal beryllium window through structural design. It has a delicate structure and is convenient for processing, and can realize continuous monitoring of the long-term charge and discharge behavior of electrodes of aqueous and organic ionic batteries, filling the technical gap in the existing in-situ XRD technology field, and reducing the use threshold and safety risks of this advanced characterization.

[0007] The present application provides a beryllium-free electrochemical in-situ XRD test device, which includes: a top cover, a main body, a bottom cover, and in-chamber accessories;

[0008] The top cover is a sheet-like annular structure, with a circle of screw through-holes formed thereon for fixing the top cover to the main body; the overall shape of the main body is a cylindrical shape with a central opening, the center of the upper surface of the main body protrudes upward, the center of the protruding part is an opening, and two bow-shaped limiting structures are arranged at the opening of the upper surface, so that the opening of the upper surface of the main body changes from a circular shape to a quadrilateral structure, one pair of opposite sides of the quadrilateral is parallel, and the other pair of opposite sides is an outward arc shape. A circle of grooves is arranged on the upper surface of the main body for placing a rubber ring to keep the upper cover and the main body sealed. The center of the lower surface of the main body is recessed inward, the center of the recessed part is an opening, and a rubber insulating pad is arranged at the recessed part. The rubber insulating pad is annular, and the inner diameter of the rubber insulating pad is smaller than the inner diameter of the opening of the main body; electrode pin holes are formed at the same positions on the main body and the top cover; the bottom cover is fixed to the lower surface of the main body by screws, and the rubber insulating pad is used to keep the bottom cover and the main body sealed; an annular groove is formed on the lower surface of the bottom cover for placing an insulating inner lining to keep the bottom cover insulated from the outside; the accessories in the cavity include: an insulating cylindrical inner lining, a T-shaped electrode tray, and a metal support spring. The insulating cylindrical inner lining is placed in the central opening of the main body. The upper end of the insulating cylindrical inner lining is close to the bow-shaped limiting structure on the upper surface of the main body, and the lower end of the insulating cylindrical inner lining is placed on the protruding edge of the rubber insulating pad relative to the main body; the T-shaped electrode tray is placed upright in the insulating cylindrical inner lining. The upper end of the T-shaped electrode tray is close to the bow-shaped limiting structure on the upper surface of the main body, and the lower end of the T-shaped electrode tray is located on the bottom cover; the metal support spring is sleeved on the T-shaped electrode tray. The upper end of the metal support spring is closely attached to the lower surface of the top cap of the T-shaped electrode tray, and the lower end of the metal support spring is located on the bottom cover. The metal support spring is used to lift the T-shaped electrode tray so that the upper surface of the T-shaped electrode tray is closely attached to the bow-shaped limiting structure;

[0009] During actual use, a layer of disposable polymer sealing film is covered on the entire upper surface of the main body, and then the upper cover is installed.

[0010] Further, the size of the quadrilateral opening at the top of the main body should not interfere with the X-ray incident / exit optical path of the used diffractometer.

[0011] Further, the T-shaped electrode tray is made of TA2 type titanium material, the metal support spring is a titanium-plated 316 stainless steel spring, the insulating cylindrical inner lining is made of PTFE or PEEK plastic, and the rubber ring and the rubber insulating pad are made of fluororubber material.

[0012] A testing method for an electrochemical in-situ XRD testing device using a beryllium-free window, the method comprising:

[0013] Step 1: Cut the electrode to be tested and the diaphragm according to the inner diameter of the main body of the test kit; cut the counter electrode according to the inner diameter of the insulating cylindrical inner lining;

[0014] Step 2: Place the battery body with the windowed side facing up on a flat surface. After placing a polymer sealing film, align the top cover with the eyelet and nest it above the body, then screw in the top fastening screws in sequence;

[0015] Step 3: Invert the battery body, and sequentially place the test electrode, separator, insulating cylinder liner. After dropping the electrolyte, place the counter electrode, T-shaped electrode tray, and metal support spring in sequence;

[0016] Step 4: Install a sealing insulating gasket on the battery body. After placing the bottom cover aligned with the screw holes, screw in the bottom fixing screws in sequence;

[0017] Step 5: Rotate the battery until the windowed side is facing up. Check the integrity of the polymer film and the potential difference between the top / bottom covers of the battery. After no abnormalities are found, transfer it to the XRD diffractometer, and adjust the placement direction so that the longest exposed direction of the electrode in the slot is the X-ray incident / exit direction;

[0018] Step 6: Connect the kit to the electrochemical test terminal connected inside the diffractometer. After setting the electrochemical test program and the diffractometer scanning program, start them simultaneously, and stop them simultaneously after the test is completed.

[0019] Further, the test electrode is a powder electrode coated on a metal titanium mesh or a metal sheet electrode with self-supporting rigidity.

[0020] Using the test kit and test method described in this application, the following beneficial effects can be achieved:

[0021] (1) In the present invention, an ultra-thin polymer film with a thickness much lower than that of a metal beryllium window is used as the X-ray incident / exit transmission material. When using a copper target light source (Kα line energy ≈ 8.04 keV), the signal attenuation of the sample obtained is significantly less than that using a metal beryllium window, and the test accuracy is effectively improved;

[0022] (2) The ultra-thin polymer film used in the present invention as the in-situ test sealing window material has excellent water-based / organic-based electrolyte tolerance, enabling it to meet various in-situ electrochemical XRD test scenarios including but not limited to active metal batteries, neutral / acidic or alkaline supercapacitors, neutral / acidic or alkaline aqueous batteries, and electrochemical corrosion in acid-base environments. At the same time, no impurity ions escape from the encapsulation film, and it has good universality;

[0023] (3) The designed structure of the present invention is simple and small in volume, with no special precision and material requirements, which can significantly reduce the manufacturing cost of the device, and can be combined with other kits such as temperature control kits and magnetic field generation kits to achieve in-situ electrochemical tests in complex environments. Description of the Drawings

[0024] Figure 1 It is an axonometric sectional view of the test kit structure according to the embodiment of the present application;

[0025] Figure 2 Isometric view of the main structure of the test suite according to an embodiment of the present application;

[0026] Figure 3 Top view of the installation direction of the test suite according to an embodiment of the present application;

[0027] Figure 4 XRD pattern of the anode of a copper-zinc pair battery using an aqueous electrolyte during charge and discharge obtained by the test method according to an embodiment of the present application.

[0028] Figure 5 XRD pattern of the positive electrode of a lithium-ion battery using an organic electrolyte during charge and discharge obtained by the test method according to an embodiment of the present application; Detailed implementation manners

[0029] In order to keep the following description of the embodiments of the present application clear and concise, detailed descriptions of known functions and known components are omitted in the present application.

[0030] As mentioned above, the in-situ electrochemical XRD technique is a characterization method that combines real-time electrochemical testing and X-ray diffraction analysis. By synchronously collecting the XRD signals of electrode materials during the dynamic operation of devices such as batteries and capacitors, the evolution laws of the crystal structure of materials during reactions such as charge and discharge, ion insertion / extraction (such as phase change paths, lattice distortion, stress distribution, etc.) can be directly analyzed. Among them, the beryllium window is a key component, and its role is to balance the sealing performance of the electrochemical cell and the X-ray penetration: beryllium metal has a high transmittance (about 80% or more) for low-energy X-rays (such as Cu-Kα, 8.04 keV), and at the same time can isolate the volatilization of the electrolyte and maintain a stable reaction environment. However, traditional beryllium windows have defects such as toxicity risk, mechanical brittleness and high cost. Therefore, in the present application, through structural design, while maintaining the X-ray transmission efficiency and sealing durability, the manufacturing cost is reduced and the operation safety is simplified, providing a safer and more sustainable technical solution for long-term in-situ experiments and high-throughput electrochemical material research.

[0031] From Figure 1As can be seen from the sectional view of the device, the overall device is composed of an upper cover 10, a main body 20, a bottom cover 30 and internal accessories (41, 42, 43, 44). Among them, the screw through holes 11 and electrode pin holes 12 on the upper cover correspond to the screw blind holes and pin blind holes on the surface of the lower main body; a fluororubber O-ring 23 for ensuring the sealing of the polymer film is provided between the top cover 10 and the main body 20; an insulating lining 31 with screw through holes is provided on the bottom cover 30, and the through holes correspond to the positions of the blind holes on the bottom surface of the main body. A fluororubber insulating pad 32 is provided between the bottom cover and the main body; the internal accessories include an insulating cylindrical lining 41, a T-shaped electrode tray 42, a tray sealing rubber ring 43, and a metal support spring 44. A circle of screw through holes is provided on the top cover for the screws for fixing the top cover and the main body to pass through; a circle of screw holes with insulating bushings is provided on the bottom cover for the metal screws for fixing the bottom cover and the main body to pass through. An insulating rubber pad is also provided between the bottom cover and the main body to ensure strict insulation between the two; the top of the main body structure is provided with a pole piece limiting structure for conducting electricity, and the top opening size should not interfere with the X-ray incident / exit optical path of the used diffractometer. Generally, it is an arc shape parallel up and down, and a nearly rectangular electrode exposure surface without optical path interference can be formed; the internal accessories are mainly composed of a T-shaped electrode tray, a metal support spring, an insulating cylindrical lining and other insulating / sealing gaskets. The T-shaped electrode tray is made of TA2 type titanium material, the metal support spring is a titanium-plated 316 stainless steel spring, the insulating cylindrical lining is made of PTFE or PEEK plastic, and other insulating / sealing gaskets are made of fluororubber material; when the whole set of components is used, a disposable polymer sealing film is required to be fixed with screws and sealed with an O-ring between the top cover and the main body. This polymer sealing film needs to be a material with a low X-ray blocking rate, generally a PET polyester film.

[0032] From Figure 2 As can be seen from the isometric view of the main body of the kit, there is a cylindrical cavity in the center of the main body, and there are two arc-shaped limiting structures 21 on the top surface; after the kit is assembled, the nearly rectangular X-ray transmission window on the top is in the same plane as the upper surface of the outer top cover 10 to ensure the effectiveness of the X-ray optical path; a groove 22 is provided on the top for placing the fluororubber O-ring 23.

[0033] From Figure 3 As can be seen from the top view of the installation direction of the test kit, the arrow direction is the X-ray incident direction. The placement direction of this kit needs to make the longest side of the nearly rectangular transmission window parallel to the ray incident / exit direction.

[0034] The following combines the drawings and specific embodiments to illustrate the test method in the present invention:

[0035] Example 1:

[0036] See Figure 1, customize the battery height and radius based on the size of the sample stage of the Bruker D2 XRD diffractometer. Process the top cover, main body, and bottom cover of the test kit from 316 stainless steel; process the insulating cylinder liner from PTFE material; process the T-shaped electrode tray from TA2 titanium material; customize the stainless steel spring; process other insulating / sealing gaskets from fluororubber; use the TM produced by Series 3012 membrane as the sealing membrane material for the transmission window.

[0037] Taking the study of the inhibitory effect of additives on the by-products on the surface of copper foil during the deposition of zinc on the surface of copper foil in a neutral electrolyte as an example:

[0038] Step 1, cut the copper mesh electrode and glass fiber diaphragm to be tested according to the inner diameter of the main body of the test kit; cut the counter electrode of metal zinc sheet according to the inner diameter of the insulating cylinder liner;

[0039] Step 2, place the battery main body with the window side facing up on a plane. After placing a polymer sealing membrane, align the top cover with the eye position and nest it above the main body, and then screw in the top fastening screws in sequence;

[0040] Step 3, invert the battery main body, and sequentially place the test electrode sheet, diaphragm, and insulating cylinder liner. After dropping 150 μL of zinc sulfate or zinc sulfate electrolyte with additives, sequentially place the counter electrode, T-shaped electrode tray, and metal support spring;

[0041] Step 4, install a sealing insulating gasket on the battery main body. After placing the bottom cover in alignment with the screw holes, screw in the bottom fixing screws in sequence;

[0042] Step 5, rotate the battery so that the window side faces up, check the integrity of the polymer membrane, and check the potential difference between the top / bottom covers of the battery. After there are no abnormalities, transfer it into the XRD diffractometer, adjust the placement direction so that the longest exposed direction of the electrode sheet in the slot is the X-ray incident / exit direction;

[0043] Step 6, connect the kit to the electrochemical test terminal connected in the diffractometer, set the electrochemical test program to 2 mA / cm 2 , deposit for 5 hours and then continue to dissolve for 5 hours; set the diffractometer scanning program to continuously scan at 2θ = 6 - 40°, with a single scan time of about 7 minutes, and set 85 cycles; after the program settings are completed, start the electrochemical test and XRD continuous scanning test simultaneously; the obtained XRD data is processed to obtain Figure 4 . Among them Figure 4 a is the test result of a single zinc sulfate electrolyte, Figure 4b is the test result after adding the additive. It can be seen that after adding the additive to inhibit by-products, the characteristic peak of by-products on the copper surface (2θ = 7.8°) completely disappears during the deposition / dissolution process of zinc. This indicates that this additive can effectively inhibit the by-products of zinc deposition.

[0044] Example 2:

[0045] In this example, the same kit prepared in Example 1 is also used. Taking the research on the energy storage mechanism of the nickel-cobalt-manganese (NCM811) cathode of a lithium-ion battery in an organic electrolyte as an example:

[0046] Step 1: In the glove box, cut the NCM811-type lithium-ion battery cathode to be tested and the commercial lithium battery separator according to the inner diameter of the main body of the test kit; cut the lithium metal sheet counter electrode according to the inner diameter of the insulating cylinder liner.

[0047] Step 2: In the glove box, place the battery body with the window side facing up on a plane. After placing a polymer sealing film, align the top cover with the eye position and nest it above the main body, and then screw in the top fastening screws in sequence.

[0048] Step 3: In the glove box, invert the battery body, and sequentially place the electrode to be tested, the separator, and the insulating cylinder liner. After dropping 150 μL of commercial lithium-ion battery electrolyte, sequentially place the counter electrode, the T-shaped electrode tray, and the metal support spring.

[0049] Step 4: In the glove box, place a sealed insulating gasket on the battery body. After placing the bottom cover in alignment with the screw holes, sequentially screw in the bottom fixing screws.

[0050] Step 5: In the glove box, rotate the battery so that the window side faces up, check the integrity of the polymer film, and check the potential difference between the top and bottom covers of the battery. After there are no abnormalities, transfer it from the glove box to the XRD diffractometer, and adjust the placement direction so that the longest exposed direction of the electrode in the slot is the X-ray incident / exit direction.

[0051] Step 6: Connect the kit to the electrochemical test terminal connected inside the diffractometer, set the electrochemical test program to 0.15 mA / cm 2 , first charge and then discharge within 10 hours; set the diffractometer scanning program to continuously scan at 2θ = 30 - 50°, with a single scan time of about 4 minutes, and set 146 cycles; after the program settings are completed, start the electrochemical test and the XRD continuous scanning test simultaneously; the obtained XRD data is processed to obtain Figure 5 . It can be seen that during the charging process, multiple characteristic peaks shift to the right, and gradually shift back to the left during the discharging process. This indicates that in this test, for the NCM811 cathode of the commercial lithium-ion battery used, when lithium ions are embedded, multiple crystal planes are squeezed closer, the crystal plane spacing decreases, and the crystal plane structure recovers after lithium ions are removed.

[0052] By using the detection kit and method provided in the present application, the device has a simple structure, is easy to operate, non-toxic and harmless, and has a low X-ray signal attenuation rate, with good universality in applications.

[0053] Although the present invention has been illustrated by exemplary embodiments, its scope of protection covers any and all embodiments based on the present invention that are equivalent elements, modifications, deletions, combinations (including combinations across embodiment solutions), adaptive adjustments or changes; the interpretation of the claims should follow the broad understanding of their literal expressions, not limited to the specific examples described in the specification or the implementation process. Such examples do not constitute a restrictive interpretation of the claims, but are only an enumeration of non-exclusive examples; in summary, this specification and the embodiments are only for illustrative reference, and the true scope and core spirit are defined by the maximum legal extension of the claims and their equivalent solutions.

[0054] The above description is intended to illustrate rather than limit the technical solutions of the present invention. For example, any example or its technical solution can be used in cross-combination with other embodiments; those skilled in the art can design embodiments not explicitly listed based on the teachings of the present invention in combination with the prior art. Moreover, the grouping of technical features in the specific implementation is only for simplified description and should not be understood as having an implicit association between any feature not claimed in the claims and the necessity of the patent. The scope of protection of the present invention is defined by the maximum legal extension of the appended claims and their equivalent solutions. Each claim independently constitutes a technical embodiment, and these embodiments can form new technical solutions through any permutation and combination. In addition, the actual implementation of the present invention may only include some features of a specific embodiment and does not necessarily cover all details.

[0055] The above embodiments are only exemplary implementation solutions for illustrating the present invention, and their function is to explain rather than limit the actual scope of protection of the present invention, which is defined by the maximum legal extension of the appended claims and their equivalent solutions; based on the technical essence and scope of protection of the present invention, those skilled in the art can make adaptive adjustments, technical equivalent replacements or creative modifications (such as structural simplification, function expansion or process optimization, etc.) to the implementation solutions. Such adjustments and modifications should be regarded as falling within the scope of protection of the present invention if they do not deviate from the core technical features and innovative essence defined by the claims, and are subject to the legal constraints of the patent right regardless of whether they directly refer to the specific details in the embodiments.

Claims

1. An electrochemical in-situ XRD testing device without a beryllium window, the device comprising: Top cover, main body, bottom cover, and cavity accessories; The top cover is a sheet-like annular structure, and a circle of screw through holes is provided on the annular structure for fixing the top cover on the main body; the overall shape of the main body is a cylinder with a central opening, the center of the upper surface of the main body bulges upward, the center of the bulge is an opening, and two arch-shaped limiting structures are provided at the opening of the upper surface, so that the opening of the upper surface of the main body changes from a circular structure to a quadrilateral structure, a pair of sides of the quadrilateral are parallel, and the other pair of sides are outwardly arc-shaped, a circle of grooves is provided on the upper surface of the main body for placing a rubber ring, so that the upper cover and the main body are kept sealed, the center of the lower surface of the main body is concave inwardly, and the center of the concave part is an opening, and a rubber insulating pad is provided at the concave part, the rubber insulating pad is annular, and the inner diameter of the rubber insulating pad is smaller than the inner diameter of the opening of the main body; electrode pin holes are provided at the same position on the main body and the top cover; the bottom cover is fixed to the lower surface of the main body by screws, and the rubber insulating pad is used to keep the bottom cover and the main body sealed. Maintain sealing; an annular groove is provided on the lower surface of the bottom cover for placing the insulating inner village so that the bottom cover is insulated from the outside; the accessories in the cavity include: an insulating cylindrical liner, a T-shaped electrode tray, and a metal support spring. The insulating cylindrical liner is placed in the central opening of the main body, the upper end of the insulating cylindrical liner is close to the arched limiting structure on the upper surface of the main body, and the lower end of the insulating cylindrical liner is placed on the raised edge of the rubber insulating pad relative to the main body; the T-shaped electrode tray is placed in the insulating cylindrical liner, the upper end of the T-shaped electrode tray is close to the arched limiting structure on the upper surface of the main body, and the lower end of the T-shaped electrode tray is located on the bottom cover; the metal support spring is sleeved on the T-shaped electrode tray, the upper end of the metal support spring is close to the lower surface of the top cap of the T-shaped electrode tray, and the lower end of the metal support spring is located on the bottom cover. The metal support spring is used to hold up the T-shaped electrode tray so that the upper surface of the T-shaped electrode tray is close to the arched limiting structure; During actual use, the entire upper surface of the main body is covered with a disposable polymer sealing film, and then the upper cover is installed.

2. The electrochemical in-situ XRD testing device without a beryllium window as claimed in claim 1, characterized in that: The size of the quadrilateral opening at the top of the body should not interfere with the X-ray incident / exit optical path of the diffractometer used.

3. The electrochemical in-situ XRD testing device without a beryllium window as claimed in claim 1, characterized in that: The T-shaped electrode tray is made of TA2 titanium material, the metal support spring is a titanium-plated 316 stainless steel spring, the inner lining of the insulating cylinder is PTFE or PEEK plastic, and the rubber ring and rubber insulating pad are made of fluororubber.

4. A testing method using the electrochemical in-situ XRD testing device without beryllium window according to claim 1, the method comprising: Step 1: Cut the electrodes and diaphragms to be tested according to the inner diameter of the test kit body; Cut the counter electrode according to the inner diameter of the insulating cylinder lining; Step 2: Place the battery body with the window side facing up on a flat surface, place a piece of polymer sealing film, align the top cover with the eye position and nest it on top of the body, and screw in the top fastening screws in sequence; Step 3: Invert the battery body, place the electrode to be tested, the diaphragm, and the insulating cylinder lining in turn, add the electrolyte, and then place the counter electrode, T-shaped electrode tray, and metal support spring in turn; Step 4: Place the sealing insulating gasket on the battery body, align the bottom cover with the screw holes, and screw in the bottom fixing screws one by one; Step 5: Rotate the battery to face the window side upward, check the integrity of the polymer film, check the potential difference between the top and bottom covers of the battery, and transfer it to the XRD diffraction tester after all are normal. Adjust the placement direction so that the longest exposure direction of the pole piece in the slot is the X-ray incident / emission direction; Step 6: Connect the kit to the electrochemical test terminal in the diffractometer, set the electrochemical test program and the diffractometer scanning program, start them simultaneously, and stop them simultaneously after the test is completed.

5. The testing method of the electrochemical in-situ XRD testing device using a beryllium window-free method as claimed in claim 4, characterized in that: The electrode to be tested is a powder electrode coated on a metal titanium mesh or a metal sheet electrode with self-supporting rigidity.

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