Electrochemical in-situ XRD (X-Ray Diffraction) test mold and test system

Abstract

The invention provides an electrochemical in-situ XRD test mold and a test system.The electrochemical in-situ XRD test mold comprises an upper mold plate and a lower mold plate, a through hole is formed in the middle of the upper mold plate to serve as a window, and the lower mold plate is detachably connected to the upper mold plate; a sealing element is arranged between the upper template and the lower template, and after the battery to be tested is assembled between the upper template and the lower template, two ends of the sealing element respectively abut against the upper template and the lower template; the press-fitting assembly is arranged on the upper template and / or the lower template and is used for adjusting the press-fitting pressure of the to-be-tested battery in the mounting space and ensuring that the to-be-tested battery is in stable contact with the upper template and the lower template; meanwhile, an observation window of the in-situ battery reaction chamber is formed in a positive electrode shell punching mode, and a corresponding window material is selected according to a tested electrode material; therefore, non-destructive observation and real-time online monitoring of the liquid battery are realized, and a corresponding test mold is convenient and efficient to operate, can be repeatedly used, is high in universality and low in cost, and is beneficial to cost reduction and benefit increase of enterprises / related departments.

Description

Technical Field

[0001] The present invention relates to the technical field of battery detection, and particularly to an in-situ XRD test mold and test system for electrochemistry. Background Art

[0002] As is well known, the high-speed development of the electrochemistry industry is inseparable from the continuous experimental operations of various types and high frequencies by researchers. For example, using in-situ XRD to monitor in real time the phase transformation of battery materials, the change of lattice parameters and other crystal structure evolutions during the electrochemical reaction process to study the charge and discharge reaction mechanism of the battery and the attenuation mechanism during the battery recycling process is one of the important research topics for researchers in this field.

[0003] In related technologies, the conventional in-situ XRD test molds used in the electrochemistry field are mostly cumbersome to operate, with relatively difficult test operations and low efficiency; and usually the same mold cannot meet the test requirements of different types and models of batteries, with low repeatability and poor versatility. Enterprises / relevant departments need to develop different in-situ XRD test molds to adapt to the test requirements of various batteries, and the R & D and production costs in this regard are relatively large, and there is room for improvement. Summary of the Invention

[0004] The purpose of the present invention is to provide an in-situ XRD test mold and test system for electrochemistry, which are convenient, efficient, reusable, highly versatile and low-cost in test operation, and help enterprises / relevant departments reduce costs and increase efficiency.

[0005] The technical solution provided by the present invention is as follows:

[0006] On the one hand, the present invention provides an in-situ XRD test mold for electrochemistry, including:

[0007] An upper template, in which a through hole is opened along the thickness direction in the middle as a viewing window;

[0008] A lower template, detachably connected to the lower side of the upper template through an insulating fastener;

[0009] A seal, arranged between the upper template and the lower template, with an installation space inside for accommodating the battery to be tested. After the battery to be tested is assembled between the upper template and the lower template, both ends of the seal respectively abut against the corresponding upper template and lower template;

[0010] A pressing assembly, arranged on the upper template and / or the lower template, for adjusting the pressing pressure of the battery to be tested in the installation space to ensure stable contact between the battery to be tested and the upper template and the lower template.

[0011] According to the electrochemical in-situ XRD test mold provided by the present invention, in actual application, that is, when performing an electrochemical in-situ XRD test, the battery to be tested is placed in the installation space, and the insulating fasteners lock the upper template and the lower template until the ends of the sealing member corresponding to the upper template and the lower template are respectively pressed against the corresponding upper template and the lower template. At the same time, the press-fitting pressure of the battery to be tested in the installation space is adjusted by using a press-fitting assembly until the positive electrode shell and the negative electrode shell of the battery to be tested always maintain good contact with the corresponding upper template and the lower template respectively, thereby realizing the assembly of the battery to be tested in the electrochemical in-situ XRD test mold.

[0012] Since the corresponding assembly operation can be completed by simply placing the battery to be tested in the installation space of the seal, locking the upper template and the lower template, and then adjusting the press-fitting component, the operation steps of the electrochemical in-situ XRD test mold are simple, in line with operating habits, and easy to implement, which effectively reduces the operational difficulty of the corresponding electrochemical in-situ XRD test and improves the corresponding operation efficiency; at the same time, since the press-fitting pressure of the battery to be tested is adjustable, the press-fitting component can be adjusted to make the installation space meet the installation requirements of different types of batteries to be tested, that is, the same electrochemical in-situ XRD test mold can simultaneously meet the testing requirements of multiple types of batteries to be tested, has a wide range of applications and strong practicality, and enterprises / relevant departments do not need to develop corresponding test molds for different types of batteries to be tested, thereby reducing their cost investment in electrochemical in-situ XRD testing and benefiting cost reduction and efficiency improvement.

[0013] In some embodiments, the sealing member comprises an insulating rubber ring;

[0014] A positioning groove is formed on the upper side of the lower template and is arranged around the window. One end of the insulating rubber ring is fixedly embedded in the positioning groove, and the other end is pressed against the lower side of the upper template.

[0015] The upper template, the insulating rubber ring and the lower template are arranged to form the installation space.

[0016] In the electrochemical in-situ XRD test mold provided by the present invention, the insulating rubber ring serves as both a seal and an insulating support, stably supporting the upper and lower mold plates. This helps maintain the flatness of the test mold after assembly and provides installation space for the battery to be tested, making the overall structure of the electrochemical in-situ XRD test mold compact and easy to produce and use. Furthermore, a positioning groove is provided for installing the insulating rubber ring, which facilitates positioning and assembly of the insulating rubber ring and helps prevent the insulating rubber ring from shifting between the upper and lower mold plates. This improves the structural stability of the electrochemical in-situ XRD test mold and ensures that the battery to be tested is stably installed within the corresponding test mold.

[0017] In some embodiments, the press-fit assembly includes a metal screw;

[0018] The lower template is provided with a threaded hole at the center of the positioning groove;

[0019] The metal screw is arranged perpendicular to the lower template, and its threaded end is screwed into the threaded hole and then extends to the installation space;

[0020] After the battery to be tested is assembled between the upper template and the lower template, the threaded end of the metal screw is pressed against the negative electrode shell of the battery to be tested, so as to press the positive electrode shell of the battery to be tested against the upper template.

[0021] The electrochemical in-situ XRD test mold provided by the present invention can, in actual application, ensure good electrical conductivity between the working electrode of the battery to be tested and the corresponding upper template and lower template by rotating the metal screw to adjust the installation pressure of the battery to be tested in the electrochemical in-situ XRD test mold; at the same time, when replacing different types of batteries to be tested, it is only necessary to rotate the metal screw to meet the clamping requirements of the corresponding battery to be tested in the electrochemical in-situ XRD test mold; the battery to be tested clamping and the corresponding pressure adjustment structure are simple, further reducing the difficulty of the electrochemical in-situ XRD test operation, improving the corresponding operation efficiency, and effectively saving the production and use costs of the corresponding test mold.

[0022] In some embodiments, the blocking bars are provided on the upper side of the upper template, and at least two blocking bars are provided around the viewing window;

[0023] At least two of the blocking bars extend into the viewing window near the edge of the viewing window to prevent the battery to be tested from escaping from the upper template.

[0024] According to the electrochemical in-situ XRD test mold provided by the present invention, a baffle is provided to prevent the battery to be tested from escaping from the upper template. Since the metal baffle is entirely higher than the plane of the upper template, on the one hand, after the battery to be tested is assembled into the electrochemical in-situ XRD test mold, its end close to the upper template extends into the window and presses against the baffle, and the movement of the battery to be tested can be restricted by the inner wall of the window without the need to provide an additional limiting structure, which helps to simplify the overall structure of the electrochemical in-situ XRD test mold, approaching its development towards compactness and miniaturization, and further improving its convenience in production and use; at the same time, after the battery to be tested is assembled into the electrochemical in-situ XRD test mold, its positive electrode shell and the upper end surface of the upper template remain in the same plane, which helps to keep the corresponding electrochemical in-situ XRD test system flat as a whole after assembly.

[0025] In some embodiments, the insulating fastener includes an insulating screw and an insulating nut, which are correspondingly arranged and each includes a plurality of insulating screws and an insulating nut.

[0026] The upper template and the lower template are each provided with a guiding hole corresponding to any one of the insulating screws. Any one of the insulating screws sequentially passes through the guiding hole of the upper template and the guiding hole of the lower template from top to bottom, and connects the upper template and the lower template through the corresponding insulating nut.

[0027] Through an in-situ XRD test mold for electrochemistry provided by the present invention, by using insulating screws and insulating nuts to connect the upper template and the lower template, on the one hand, the connection structure is simple, and production and assembly are convenient; at the same time, it can also effectively reduce the probability of short circuit after the positive and negative electrodes of the battery under test are connected.

[0028] In some embodiments, there are a plurality of positive electrode pins, and different positive electrode pins are arranged on different sides of the upper template;

[0029] There are a plurality of negative electrode pins, and different negative electrode pins are arranged on different sides of the lower template.

[0030] Through an in-situ XRD test mold for electrochemistry provided by the present invention, in actual application, the number of positive electrode pins and negative electrode pins is set according to needs, which is convenient for workers to connect electrode leads to the in-situ XRD test mold for electrochemistry, and helps to further improve the use convenience of the in-situ XRD test mold for electrochemistry.

[0031] In some embodiments, the positive electrode pin is integrally formed on the edge of the upper template;

[0032] The negative electrode pin is integrally formed on the edge of the lower template.

[0033] Through an in-situ XRD test mold for electrochemistry provided by the present invention, setting the corresponding positive electrode pins and negative electrode pins to be integrally formed with the corresponding upper template and lower template helps to simplify the production process of the in-situ XRD test mold for electrochemistry and ensure its production convenience.

[0034] In some embodiments, a clamping arm is arranged on one side edge of the upper template for a clamp of an XRD device to clamp the upper template.

[0035] On the other hand, the present invention also provides an in-situ XRD test system for electrochemistry, including any one of the above-mentioned in-situ XRD test molds for electrochemistry, and further including:

[0036] A battery under test, which is assembled in sequence according to the order of a positive electrode case, a positive electrode material, a separator, a negative electrode material, a stainless steel sheet, a stainless steel spring piece, and a negative electrode case;

[0037] An observation window is opened in the middle of the positive electrode case;

[0038] A positive electrode plate, comprising a window material sheet and a positive electrode material layer disposed thereon, wherein the positive electrode plate is disposed between the positive electrode shell and the positive electrode material and stably covers the observation window;

[0039] The radial dimension of the positive electrode plate is larger than the radial dimension of the observation window.

[0040] The electrochemical in-situ XRD testing system provided by the present invention provides an observation window in the positive electrode shell of the battery to be tested, and the positive electrode sheet is arranged in the battery to be tested and covered with the observation window, thereby coupling the battery to be tested with the in-situ observation device, realizing non-destructive observation and real-time online monitoring of the in-situ battery, and effectively improving the convenience of the corresponding electrochemical in-situ XRD testing operation. At the same time, suitable window material sheets are selected according to different electrode materials to be tested, which can avoid the use of extremely toxic beryllium metal windows, and effectively improve the safety of the corresponding electrochemical in-situ XRD testing operation.

[0041] In some embodiments, when the battery to be tested is assembled between the upper template and the lower template, the positive electrode shell and the negative electrode shell are pressed against the corresponding upper template and the lower template respectively;

[0042] The observation window is arranged corresponding to the viewing window, and the radial dimension of the observation window is larger than the radial dimension of the viewing window;

[0043] The positive electrode shell, the positive electrode sheet and the upper end surface of the upper template are in the same plane.

[0044] By providing an electrochemical in-situ XRD testing system, the size of the positive electrode piece is set to be larger than the size of the observation window, and the size of the observation window is set to be larger than the size of the visual window, thereby reducing the situation where the visual window and the observation window block the X-rays, and leaving a fault tolerance space for the observation operation, so that the X-rays always cover the effective test area, reducing the interference of abnormal samples, and helping to improve the accuracy and representativeness of the data obtained from the corresponding test.

[0045] Compared with the prior art, the electrochemical in-situ XRD test mold and test system provided by the present invention have at least one of the following beneficial effects:

[0046] 1. The electrochemical in-situ XRD test mold of the present invention has simple operation steps and conforms to operating habits, effectively reducing the operational difficulty of the corresponding electrochemical in-situ XRD test and improving test efficiency. At the same time, the setting of the press-fit assembly enables the electrochemical in-situ XRD test mold to simultaneously meet the testing requirements of different types of batteries to be tested. It has a wide range of applications and strong practicality, which is beneficial for enterprises and related departments to reduce costs and increase efficiency.

[0047] 2. In the present invention, an insulating rubber ring is provided as a seal, and a metal screw rod is provided to abut against the negative electrode case of the battery to be tested. By screwing the metal screw rod, the pressing pressure of the battery to be tested in the installation space can be adjusted, so as to achieve good contact between the battery to be tested and the in-situ electrochemical XRD test mold, and at the same time ensure the applicability of the in-situ electrochemical XRD test mold. Moreover, its overall structure is simple and compact, convenient for production and use, with good comprehensive performance and low cost.

[0048] 3. The observation window of the present invention is opened on the positive electrode case of the battery to be tested, so that the battery to be tested and the in-situ observation device are coupled into one body, realizing non-destructive observation and real-time online monitoring of the in-situ battery, which helps to significantly reduce the operation difficulty of the in-situ electrochemical XRD test; and, since appropriate window material sheets can be selected according to different electrode materials to be tested, the use of highly toxic beryllium windows can be avoided as much as possible, which helps to improve the safety factor of the corresponding in-situ electrochemical XRD test operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] The above characteristics, technical features, advantages and their implementation manners of the present solution will be further described below in a clear and easy-to-understand manner in conjunction with the drawings in the preferred embodiments.

[0050] Figure 1 is an exploded view mainly showing the overall structure of the in-situ electrochemical XRD test mold in the embodiment of the present invention;

[0051] Figure 2 is an exploded view mainly showing the overall structure of the battery to be tested in the embodiment of the present invention;

[0052] Figure 3 is a cross-sectional view mainly showing the state of the battery to be tested installed in the in-situ electrochemical XRD test mold in the embodiment of the present invention;

[0053] Figure 4 is mainly showing the charge and discharge curve and XRD test spectrum of the relevant battery to be tested in the embodiment of the present invention.

[0054] DESCRIPTION OF THE REFERENCE NUMERALS:

[0055] 1. Upper template; 11. Window; 12. Positive electrode pin; 13. Clamping arm; 14. Stop bar; 2. Lower template; 21. Negative electrode pin; 22. Positioning groove; 3. Insulating fastener; 31. Insulating screw rod; 32. Insulating nut; 4. Insulating rubber ring; 5. Metal screw rod; 6. Battery to be tested; 61. Positive electrode case; 611. Observation window; 62. Positive electrode material; 63. Separator; 64. Negative electrode material; 65. Stainless steel sheet; 66. Stainless steel spring piece; 67. Negative electrode case; 68. Positive electrode plate. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0056] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the specific embodiments of the present invention will be described below with reference to the accompanying drawings. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings and other embodiments can be obtained based on these drawings without inventive work.

[0057] To simplify the drawings, only the parts relevant to the present invention are schematically shown in each figure. They do not represent the actual structure of the product. Furthermore, to simplify the drawings and facilitate understanding, in some figures, only one of the components with the same structure or function is schematically depicted or labeled. As used herein, "one" not only means "only one" but also "more than one."

[0058] In recent years, with the deepening of research on lithium-ion batteries, sodium-ion batteries, organic batteries, and solid-state batteries, new cathode materials, anode materials, and electrolyte materials have continuously emerged. In-situ XRD, as a powerful tool for studying the crystal structure evolution of battery materials during charge and discharge, is of great significance for optimizing battery material design. However, the in-situ XRD test molds currently used in the electrochemical field are mostly cumbersome to operate, have low reproducibility, and are expensive.

[0059] In this regard, in one embodiment, referring to the accompanying drawings of the specification Figures 1 to 3 The invention provides an electrochemical in-situ XRD test mold, which has simple operation steps, conforms to operating habits, is convenient and efficient to use, can be reused, has strong versatility, and is low-cost, which is beneficial for enterprises and related departments to reduce costs and increase efficiency. It includes an upper template 1 and a lower template 2 arranged directly below it, wherein the middle part of the upper template 1 is provided with a through hole along the thickness direction to serve as a window 11 for XRD testing, and the lower template 2 is detachably connected to the upper template 1 by an insulating fastener 3; and a sealing member is provided between the two. After the battery to be tested 6 is assembled between the upper template 1 and the lower template 2, the two ends of the sealing member respectively press against the corresponding upper template 1 and the lower template 2. Of course, the installation space for accommodating the battery to be tested 6 is formed in the sealing member; it also includes a press-fitting assembly for adjusting the press-fitting pressure of the battery to be tested 6 in the installation space to ensure that the battery to be tested 6 is in good contact with the upper template 1 and the lower template 2. During production, the press-fitting assembly is provided on the upper template 1 and / or the lower template 2 according to specific needs.

[0060] In practical applications, after placing the battery 6 to be tested in the installation space within the seal, lock the upper template 1 and the lower template 2, and then adjust the pressing assembly until the battery 6 to be tested is in stable contact with the upper template 1 and the lower template 2, so that the working electrode of the battery 6 to be tested maintains good electrical conductivity with the corresponding upper template 1 and lower template 2. Then, the assembly operation of the corresponding mold can be completed. The assembly operation of this in-situ electrochemical XRD test mold is simple, which helps to significantly reduce the operation difficulty of in-situ electrochemical XRD testing and improve the testing efficiency. At the same time, after the corresponding test mold is assembled, the pressing assembly provided on the upper template 1 and / or the lower template 2 adjusts the battery 6 to be tested to keep good contact with the upper template 1 and the lower template 2. Since the pressing pressure of the battery 6 to be tested in the installation space is adjustable, while ensuring the normal progress of the testing operation, the installation space can adapt to the installation needs of different types of batteries 6 to be tested, effectively improving the applicability of this in-situ electrochemical XRD test mold and reducing the cost input of enterprises / relevant departments in in-situ electrochemical XRD testing, thereby effectively promoting cost reduction and efficiency increase for enterprises / relevant departments.

[0061] In one embodiment, based on the above embodiment, specifically, referring to Figure 1 , both the upper template 1 and the lower template 2 are generally in the shape of a rectangular flat plate structure, and positive electrode pins 12 and negative electrode pins 21 are respectively provided at their edges for welding wires or directly using alligator clips to connect the corresponding electrode leads; among them, the positive electrode pins 12 are provided at the edge of the upper template 1 and are integrally formed with the upper template 1; in this embodiment, to improve the usability of the in-situ electrochemical XRD test mold, several positive electrode pins 12 are provided on the upper template 1. When there are multiple positive electrode pins 12, the multiple positive electrode pins 12 are respectively arranged at different edges of the upper template 1; Figure 1 And Figure 3 shows the situation when the positive electrode pins 12 are set to two, and the two positive electrode pins 12 are respectively arranged on the opposite side surfaces in the horizontal direction of the upper template 1; similarly, several negative electrode pins 21 are also provided, and when there are multiple negative electrode pins 21, the multiple negative electrode pins 21 are respectively arranged at different edges of the lower template 2.

[0062] Of course, according to the clamping needs of the fixture on the XRD device, the upper template 1 and the lower template 2 can also be set to appropriate shapes, such as various flat plate structures like circular, triangular, polygonal, etc.; similarly, the positive electrode pins 12 and the negative electrode pins 21 can also be detachably connected to the corresponding upper template 1 and lower template 2 through connecting parts such as metal bolts and buckles, and the present invention does not specifically limit the number and form of the positive electrode pins 12 and the negative electrode pins 21.

[0063] Referring to Figure 1 And Figure 3To meet the clamping requirements of the XRD equipment fixture, the upper plate 1 is further provided with a clamping arm 13. The clamping arm 13 is also a flat plate and is located on one side edge of the upper plate 1. In this embodiment, to simplify the production process, the clamping arm 13 is integrally formed with the upper plate 1 and extends along the plane of the upper plate 1 away from the viewing window 11. Of course, the clamping arm 13 can also be detachably connected to the upper plate 1 via a connector.

[0064] Furthermore, the insulating fastener 3 includes a plurality of insulating screws 31 and insulating nuts 32. In this embodiment, an insulating screw 31 is provided at each of the four corners corresponding to the upper template 1 and the lower template 2, and an insulating nut 32 is arranged corresponding to it; at the same time, a guide hole is opened on the upper template 1 and the lower template 2 corresponding to any insulating screw 31, and the threaded end of any insulating screw 31 passes through the corresponding guide holes of the upper template 1 and the lower template 2 from top to bottom, and the upper template 1 and the lower template 2 are connected by the insulating nut 32.

[0065] In this embodiment, in order to ensure the flatness of the surface of the upper template 1, any guide hole of the upper template 1 is a countersunk hole, and the nut end of any insulating screw 31 is embedded in the corresponding countersunk hole.

[0066] Further, refer to Figure 1 and Figure 3 , a baffle 14 is provided on the upper side of the upper template 1, and at least two baffles 14 are provided around the viewing window 11, and at least two baffles 14 extend into the viewing window 11 near the edges of the viewing window 11; after the battery to be tested 6 is assembled in the corresponding test mold, one end of its positive electrode shell 61 extends into the viewing window 11 and presses against the baffle 14 to prevent it from falling out of the upper template 1; at the same time, the positive electrode shell 61 of the battery to be tested 6, the observation window 611, and the upper end surface of the upper template 1 are maintained in the same plane to further maintain the flatness of the surface of the corresponding electrochemical in-situ XRD test mold.

[0067] Reference Figure 3 The sealing member includes an insulating rubber ring 4, which is arranged around the viewing window 11. In addition, to improve the installation stability of the insulating rubber ring 4 and the battery under test 6, in this embodiment, a positioning groove 22 is formed on the upper side of the lower template 2 corresponding to the insulating rubber ring 4. One end of the insulating rubber ring 4 close to the lower template 2 is fixedly embedded in the positioning groove 22, and the other end is pressed against the lower side of the upper template 1. An installation space is formed in the space enclosed by the upper template 1, the insulating rubber ring 4 and the lower template 2 to prevent the battery under test 6 from shifting.

[0068] The press-fitting assembly includes a metal screw 5. Specifically, a threaded hole is provided at the center of the positioning groove 22 corresponding to the lower template 2. The metal screw 5 is perpendicular to the lower template 2, and its threaded end is screwed into the threaded hole from bottom to top until it extends into the installation space. In practical applications, one end of the negative electrode case 67 of the battery 6 to be tested extends into the insulating rubber ring 4 and abuts against the metal screw 5, while one end of its positive electrode case 61 extends into the viewing window 11. The metal screw 5 is screwed until one end of its positive electrode case 61 tightly abuts against the lower side of the retaining bar 14, and the installation pressure of the battery 6 to be tested in the installation space is adjusted until the battery 6 to be tested is in stable contact with both the upper template 1 and the lower template 2, then the assembly of the battery 6 to be tested in the corresponding test mold can be completed.

[0069] In the embodiment of the present invention, the metal screw 5 can also be arranged on the upper template 1 as needed, or the press-fitting assembly can be set in the form of an automatic press-fitting structure, etc. Of course, the installation position and form of the press-fitting assembly should not be regarded as specific limitations on the protection scope of the present invention.

[0070] Next, taking the application of this in-situ electrochemical XRD test mold in the in-situ battery test scenario as an example, the technical solution of the present invention will be further elaborated in detail.

[0071] In one embodiment, an in-situ electrochemical XRD test system is provided. Referring to Figure 2 And Figure 3 , it includes a battery 6 to be tested. The battery 6 to be tested is assembled in sequence according to the positive electrode case 61, positive electrode material 62, separator 63, negative electrode material 64, stainless steel sheet 65, stainless steel spring piece 66 and negative electrode case 67 to form an in-situ battery reaction chamber, that is, the standard button cell manual assembly process is adopted in this embodiment; among them, an observation window 611 is provided through the thickness direction at the center of the positive electrode case 61, and a positive electrode tab 68 is provided at the observation window 611. Specifically, the positive electrode tab 68 includes a viewing window material thin sheet coated with a positive electrode material 62 layer, which is press-fitted between the positive electrode case 61 and the positive electrode material 62, and one side of the viewing window material thin sheet abuts tightly against the positive electrode case 61.

[0072] In actual tests, the electrode material can be selected from one of metal-organic covalent compounds, thiophene-based organic cathodes, covalent metal-organic compound anodes, silicon-carbon anodes, lithium iron phosphate, sodium iron vanadium phosphate, lithium manganate, sodium manganate, lithium carbonate, and high-entropy lithium-rich cathode materials 62; in this embodiment, according to the different electrode materials to be tested, a specific window material with chemical inertness and good conductivity can be selected to make a window material thin sheet. For example, a graphite paper or aluminum foil with a thickness of 0.01 to 0.3 mm (including but not limited to) can be selected to make a window material thin sheet, and then the electrode material to be tested is coated on its surface. After drying, it is cut into circular pieces of a specified size by a positive electrode slicing machine to form a positive electrode plate 68, which is then covered on the observation window 611; in this way, the use of toxic beryllium windows can be effectively avoided, ensuring the safety and reliability of the corresponding test process.

[0073] It should be noted that in this embodiment, the pressing pressure needs to be determined according to different window materials, and the pressing pressure of the corresponding battery 6 to be tested is less than 60 kg; the in-situ battery reaction chamber formed by its assembly can also be used for Raman testing (in this case, quartz is selected to make the window material thin sheet). Moreover, the radial dimension of the positive electrode plate 68 needs to be larger than the radial dimension of the observation window 611 to avoid the positive electrode shell 61 blocking the X-ray spot of the XRD device; at the same time, the diameter dimension of the observation window 611 needs to be larger than the irradiation area of the X-ray spot emitted by the XRD device.

[0074] Of course, referring to Figure 3 , the electrochemical in-situ XRD test system further includes the electrochemical in-situ XRD test mold described in any of the above embodiments. After the battery 6 to be tested is assembled in the corresponding test mold, its positive electrode shell 61 and negative electrode shell 67 are respectively pressed against the stop strip 14 of the upper template 1 and the lower template 2, and the observation window 611 is kept corresponding to the window 11; at the same time, the upper end surfaces of the positive electrode shell 61, the positive electrode plate 68 of the battery 6 to be tested and the upper template 1 are in the same plane. In this embodiment, it should also be noted that the radial dimension of the observation window 611 is set to be larger than the radial dimension of the window 11.

[0075] To further clarify the assembly process of the corresponding in-situ battery reaction chamber, an example is given below for illustration:

[0076] In one embodiment, a test method for an in-situ battery reaction chamber for in-situ XRD and Raman testing is provided. Taking the example that the positive electrode material 62 is a metal-organic covalent compound, the in-situ XRD detection method of the corresponding liquid battery includes the following steps:

[0077] S1. Manually assemble the corresponding in-situ battery reaction chamber; specifically, stack the positive electrode sheet 68 to be tested and the glass fiber separator 63 into the positive electrode case 61 in sequence, drop 200 ul of electrolyte, and then sequentially buckle the negative electrode material 64, the stainless steel sheet 65, the stainless steel spring piece 66, and the negative electrode case 67 onto the glass fiber separator 63, and send it to the battery sealer for compaction and sealing to form an in-situ battery reaction chamber; and control the packaging pressure within 50 kg.

[0078] S2. Place the in-situ battery reaction chamber in the installation space of the electrochemical in-situ XRD test mold, keeping its observation window facing the upper template 1 of the corresponding test mold; adjust the insulating fastener 3 to lock the upper template 1 and the lower template 2; screw the metal bolt to adjust the pressing pressure in the corresponding test mold; then measure the voltage of the in-situ battery reaction chamber on the Blue Electric battery test equipment until the battery cycle requirements are met.

[0079] Certainly, in one embodiment, a test method for an in-situ battery reaction chamber for in-situ XRD and Raman tests is also provided, including the following operating steps:

[0080] S1. Manually assemble the corresponding in-situ battery reaction chamber; specifically, stack the positive electrode sheet 68 to be tested and the glass fiber separator 63 into the positive electrode case 61 in sequence, drop 170 ul of electrolyte, and then sequentially buckle the negative electrode material 64, the stainless steel sheet 65, the stainless steel spring piece 66, and the negative electrode case 67 onto the glass fiber separator 63, and send it to the battery sealer for compaction and sealing to form an in-situ battery reaction chamber; and control the packaging pressure within 40 kg.

[0081] S2. Place the in-situ battery reaction chamber in the installation space of the electrochemical in-situ XRD test mold, keeping its observation window facing the upper template 1 of the corresponding test mold; adjust the insulating fastener 3 to lock the upper template 1 and the lower template 2; screw the metal bolt to adjust the pressing pressure in the corresponding test mold; then measure the voltage of the in-situ battery reaction chamber on the Blue Electric battery test equipment until the battery cycle requirements are met.

[0082] In one embodiment, a test method for an in-situ battery reaction chamber for in-situ XRD and Raman tests is also provided, including the following operating steps:

[0083] S1. Manually assemble the corresponding in-situ battery reaction chamber; specifically, stack the positive electrode sheet 68 to be tested and the glass fiber separator 63 into the positive electrode case 61 in sequence, drop 120 ul of electrolyte, and then sequentially buckle the negative electrode material 64, the stainless steel sheet 65, the stainless steel spring piece 66, and the negative electrode case 67 onto the glass fiber separator 63, and send it to the battery sealer for compaction and sealing to form an in-situ battery reaction chamber; and control the packaging pressure within 40 kg.

[0084] S2. Place the in-situ battery reaction chamber in the installation space of the electrochemical in-situ XRD test mold, with its observation window facing the upper template 1 of the corresponding test mold; adjust the insulating fastener 3 to lock the upper template 1 and the lower template 2; screw the metal bolt to adjust the pressing pressure in the corresponding test mold; then measure the voltage of the in-situ battery reaction chamber on the Blue Power battery test equipment until the battery cycling requirements are met.

[0085] In the above test method of the in-situ battery reaction chamber for in-situ XRD and Raman tests, when a metal-organic covalent compound is selected as the positive electrode material 62, the corresponding positive electrode material 62 can be [Fe2(CAN)3(H2O)4]·4H2O, Ni3(HATQ)2, MIL-47[V IV (O)(bdc)], etc. And when 120 ul of electrolyte is dropped into the battery 6 to be tested, the structural changes of lattice expansion and contraction during the reaction process are as Figure 4 shown in the charge-discharge curve and XRD test spectrum. The spectrum has a high signal-to-noise ratio, no miscellaneous peak interference, and meets the requirements of in-situ XRD tests.

[0086] The implementation principle of this embodiment is as follows: A test window of the in-situ battery reaction chamber is formed by drilling holes in the positive electrode shell 61. The corresponding window material is selected according to the electrode material to be tested. Then, the button cell assembly method is used and the pressing pressure is selected according to different window materials to assemble the in-situ battery reaction chamber, so as to realize non-destructive observation and real-time online monitoring of the liquid battery; at the same time, the operation steps of the corresponding electrochemical in-situ XRD test mold are simple and in line with the operation habits. The operation difficulty of the corresponding electrochemical in-situ XRD test is low, the efficiency is high, and it can meet the test requirements of different types of batteries 6 to be tested. It has a wide application range, strong versatility, good comprehensive performance, and is conducive to cost reduction and efficiency increase for enterprises / relevant departments.

[0087] It should be noted that the above embodiments can be freely combined as needed. The above are only the preferred embodiments of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. An in-situ electrochemical XRD test mold, characterized in that Comprising: An upper template, with a through hole opened along the thickness direction in the middle thereof to serve as a viewing window; A lower template, detachably connected to directly below the upper template through an insulating fastener; A seal, disposed between the upper template and the lower template, with an installation space provided therein for accommodating a battery under test, and after the battery under test is assembled between the upper template and the lower template, both ends of the seal respectively abut against the corresponding upper template and lower template; A press-fitting assembly, disposed on the upper template and / or the lower template, for adjusting the press-fitting pressure of the battery under test within the installation space to ensure stable contact between the battery under test and the upper template and the lower template.

2. The in-situ electrochemical XRD test mold according to claim 1, wherein The seal includes an insulating rubber ring; A positioning groove is opened on the upper side surface of the lower template and is arranged around the viewing window. One end of the insulating rubber ring is fixedly embedded in the positioning groove, and the other end abuts against the lower side surface of the upper template; The upper template, the insulating rubber ring and the lower template enclose to form the installation space.

3. The in-situ electrochemical XRD test mold according to claim 2, wherein The press-fitting assembly includes a metal screw; A threaded hole is opened at the center of the positioning groove on the lower template; The metal screw is arranged perpendicular to the lower template, and after its threaded end is screwed into the threaded hole, it extends into the installation space; After the battery under test is assembled between the upper template and the lower template, the threaded end of the metal screw abuts against the negative electrode shell of the battery under test to abut the positive electrode shell of the battery under test against the upper template.

4. The in-situ electrochemical XRD test mold according to claim 1, wherein Blocking strips are disposed on the upper side surface of the upper template and at least two are arranged around the viewing window; At least two of the blocking strips extend into the viewing window range near the edge of the viewing window to prevent the battery under test from slipping out of the upper template.

5. The in-situ electrochemical XRD test mold according to claim 1, wherein The insulating fastener includes an insulating screw and an insulating nut, which are correspondingly arranged and both include a plurality of them; For any one of the insulating screws, the upper template and the lower template are respectively provided with guiding holes. Any one of the insulating screws sequentially passes through the guiding hole of the upper template and the guiding hole of the lower template from top to bottom, and connects the upper template and the lower template through the corresponding insulating nut.

6. The in-situ electrochemical XRD test mold according to claim 1, wherein A plurality of positive electrode pins, with different positive electrode pins disposed on different side surfaces of the upper template; A plurality of negative electrode pins, with different negative electrode pins disposed on different side surfaces of the lower template.

7. The in-situ electrochemical XRD test mold according to claim 6, wherein The positive electrode pins are integrally formed on the edge of the upper template; The negative electrode pins are integrally formed on the edge of the lower template.

8. The in-situ electrochemical XRD test mold according to claim 1, wherein The clamping arm is arranged on one side edge of the upper template for the fixture of the XRD device to clamp the upper template.

9. An electrochemical in-situ XRD testing system, characterized in that: An in-situ electrochemical XRD test mold according to any one of claims 1-8 above further comprises: The battery under test, which is assembled in sequence of the positive electrode shell, the positive electrode material, the separator, the negative electrode material, the stainless steel sheet, the stainless steel spring piece and the negative electrode shell. The observation window is opened at the center of the positive electrode shell. The positive electrode plate includes a thin window material sheet and a positive electrode material layer disposed thereon. The positive electrode plate is disposed between the positive electrode shell and the positive electrode material and stably covers the observation window. The radial dimension of the positive electrode plate is larger than the radial dimension of the observation window.

10. An in-situ electrochemical XRD test system according to claim 9, wherein When the battery under test is assembled between the upper template and the lower template, the positive electrode shell and the negative electrode shell respectively abut against the corresponding upper template and lower template. The observation window and the viewing window are correspondingly arranged, and the radial dimension of the observation window is larger than the radial dimension of the viewing window. The upper end surfaces of the positive electrode shell, the positive electrode plate and the upper template are in the same plane.

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