Laminated mold battery for in-situ transmission XRD (X-Ray Diffraction) and use method thereof

By designing a stacked mold battery for in-situ transmission XRD and using transmission method for testing, the high design requirements of existing reflection methods are solved, and a comprehensive analysis of the phase structure of positive and negative electrode materials during the charging and discharging process is realized, simplifying the removal process of electrode sheets and separators.

CN121618062APending Publication Date: 2026-03-06NORTH CHINA UNIVERSITY OF TECHNOLOGY +1
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Patent Information

Application Number
CN202511945602.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-22
Publication Date
2026-03-06

AI Technical Summary

Technical Problem

Existing in-situ XRD testing methods for batteries are based on the reflection principle, which leads to high requirements for the design of the in-situ test cell, especially the requirements for the observation window and tooling fixtures. Furthermore, traditional methods are difficult to obtain full information about the battery during the charging and discharging process.

Method used

Design a stacked mold battery for in-situ transmission XRD, including stacked cells and electrolyte, using in-situ cells on side A and side B, with the stacked cells clamped in a sealed cavity, and tested by transmission method. The structure is simple and easy to assemble and disassemble.

Benefits of technology

This method enables the acquisition of rich phase structure information of positive and negative electrode materials under in-situ electrochemical conditions, overcoming the limitation of the reflective method which can only obtain information of the reflective surface, and facilitating the removal of electrode sheets and separators for further analysis.

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Abstract

The invention discloses a lamination mold battery for in-situ transmission XRD (X-Ray Diffraction) and a use method thereof, and belongs to the technical field of lamination mold batteries. The problems that existing in-situ XRD testing methods of the laminated mold battery are all based on the reflection type principle, and the requirement for an in-situ testing pool is high are solved. The laminated mold battery comprises an A-side in-situ pool, a B-side in-situ pool, a laminated cell and an electrolyte, the laminated battery cell is clamped and fixed in a sealed cavity formed by the battery cell fixing shells of the A-side in-situ cell and the B-side in-situ cell, a negative electrode lug region and a positive electrode lug region of the laminated battery cell extend out of the sealed cavity and are respectively in contact with conducting strips on the two sides of the battery cell fixing shells, and the electrolyte is injected into the sealed cavity. The laminated mold battery is simple in design and convenient to assemble and disassemble, and richer phase structure information of the positive electrode active material and the foil, the negative electrode active material and the foil and the like under the in-situ electrochemical condition can be obtained at the same time.
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Description

Technical Field

[0001] This invention belongs to the field of mold battery technology, specifically relating to a stacked mold battery for in-situ transmission XRD and its usage method. Background Technology

[0002] Lithium-ion batteries are used as a power source in many fields, including large-scale energy storage, electric transportation, and consumer electronics, due to their many advantages such as high energy density, long cycle life, good safety, and low cost. Moreover, with the continuous advancement of battery technology, their application areas are constantly expanding.

[0003] Understanding and revealing the phase structure changes of key materials such as the positive and negative electrodes during battery charging and discharging is crucial for studying and improving the performance of current battery systems and for providing fundamental theoretical data support for the development of next-generation battery materials and technologies. Therefore, developing in-situ testing and characterization equipment and methods for battery phase structure analysis is of paramount importance.

[0004] X-ray diffraction (XRD) is an important material analysis and testing technique. It can be used to determine the crystal structure, crystallinity, stress, and orientation of materials, and has been widely applied in fields such as batteries and catalysis. Because lithium ions intercalate and deintercalate between the positive and negative electrodes during charging and discharging, the phase structure of the corresponding positive and negative electrode materials also changes. In-situ XRD is a relatively effective method for better analyzing and studying the phase structure changes that occur in battery materials during charging and discharging.

[0005] Traditional in-situ XRD testing methods for batteries are based on the reflection principle, which places high demands on the design of the in-situ test cell. For example, the in-situ XRD battery test cell mentioned in Chinese utility model patent CN219915460U typically uses a beryllium window for its observation window. According to literature reports, 60% of beryllium ore is distributed in the United States, and China is heavily reliant on imported beryllium. Chinese invention patent application CN116500067A discloses an in-situ XRD measuring instrument for pouch batteries. This XRD diffractometer uses a molybdenum target with higher energy than the conventional copper target, thus achieving penetration of the pouch battery. However, this places higher demands on the pouch battery and the matching tooling fixtures. Summary of the Invention

[0006] To address the technical problem that existing battery in-situ XRD testing methods are all based on the reflection principle and have high requirements for the in-situ test cell, this invention provides a stacked mold battery for in-situ transmission XRD that is simple in design, easy to assemble and disassemble, and further provides its usage method.

[0007] To solve the above-mentioned technical problems, the technical solution of the present invention is as follows: A stacked mold battery for in-situ transmission XRD includes stacked cells and electrolyte, and also includes an in-situ cell on side A and an in-situ cell on side B. The in-situ cell on side A and the in-situ cell on side B each include a cell fixing shell and conductive sheets fixed on both sides of the cell fixing shell. The stacked battery cell is clamped and fixed in a sealed cavity formed by the battery cell fixing shell of the in-situ cell on side A and side B. The negative electrode tab area and the positive electrode tab area of ​​the stacked battery cell extend out of the sealed cavity. The two outermost negative electrode tab areas are in contact with two conductive sheets on the same side of the in-situ cell on side A and side B, respectively. The two outermost positive electrode tab areas are in contact with two conductive sheets on the other side of the in-situ cell on side A and side B, respectively. The electrolyte is injected into the sealed cavity.

[0008] Furthermore, the in-situ cell on side A and the in-situ cell on side B each include a cell fixing shell and two conductive plates. The cell fixing shell consists of a shell and two ear structures. The surface of the shell has a cell groove. The two ear structures are fixed on both sides of the shell. The two conductive plates are fixed on the two ear structures, and their edges extend out of the ear structures.

[0009] Furthermore, the in-situ pool on side A and the in-situ pool on side B are the same.

[0010] Furthermore, the shell and the two ear structures are integrally formed.

[0011] Furthermore, the housing and the cell recess are coaxial.

[0012] Furthermore, one surface of the ear structure is in the same plane as the surface of the housing with the battery cell groove.

[0013] Furthermore, an annular groove is formed on the outer surface of the casing on the outer edge of the cell groove, and a sealing ring is provided inside the annular groove.

[0014] Furthermore, at least four screw holes are opened on the outer surface of the housing on the outer edge of the annular groove. The in-situ cell on side A and the in-situ cell on side B are fixedly connected by bolts and clamp and fix the stacked cells.

[0015] Furthermore, the stacked cell includes several positive electrode sheets and several negative electrode sheets. The negative electrode sheet includes a negative electrode foil layer and a negative electrode active coating layer. The negative electrode foil layer consists of a negative electrode tab region and a negative electrode active coating region. The negative electrode active coating layer is fixed on the inner and outer surfaces of the negative electrode active coating region. The positive electrode sheet includes a positive electrode foil layer and a positive electrode active coating layer. The positive electrode foil layer consists of a positive electrode tab region and a positive electrode active coating region. The positive electrode active coating layer is fixed on the inner and outer surfaces of the positive electrode active coating region. The positive electrode sheets and negative electrode sheets are stacked alternately, and adjacent positive electrode sheets and negative electrode sheets are separated by a separator. The negative electrode tab regions of adjacent negative electrode sheets are in contact, and the positive electrode tab regions of adjacent positive electrode sheets are in contact.

[0016] Furthermore, the negative active coating on one side of each negative electrode completely covers the positive active coating on the opposite side of the positive electrode, and the positive electrode tab region of the positive electrode is at least partially exposed. The separator completely covers the negative active coating on the side of the adjacent negative electrode, and the negative electrode tab region of the negative electrode is at least partially exposed.

[0017] Furthermore, the outermost surface of the stacked battery is a negative electrode sheet, or the outer surface is a bare positive electrode foil layer and the inner surface is a positive electrode sheet with a positive active coating.

[0018] Furthermore, the outermost surface of the stacked battery is a positive electrode sheet, or the outer surface is a bare negative electrode foil layer and the inner surface is a negative electrode active coating.

[0019] This invention also provides a method for using the above-mentioned in-situ transmission XRD stacked mold battery, the steps of which are as follows: S1. Place the in-situ transmission XRD stacked mold cell on the sample stage of the transmission X-ray diffractometer for in-situ electrochemical testing. After the test is completed, remove the in-situ transmission XRD stacked mold cell. S2. Remove the in-situ cell on side B of the stacked cell from the in-situ cell on side A after the in-situ XRD test is completed, and then remove the stacked cell.

[0020] Furthermore, when the interference of the positive electrode diffraction signal that does not participate in the reaction on the positive electrode in-situ charge and discharge signal is excluded, the outermost part of the stacked cell is a negative electrode sheet, or the outer surface is a bare positive electrode foil layer and the inner surface is a positive electrode active coating.

[0021] Furthermore, when the interference of the non-reactive negative electrode diffraction signal on the negative electrode in-situ charge and discharge signal is excluded, the outermost part of the stacked cell is a positive electrode sheet, or the outer surface is a bare negative electrode foil layer and the inner surface is a negative electrode active coating.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows: The in-situ transmission XRD stacked mold battery of the present invention has a simple structure and is easy to assemble and disassemble. It can simultaneously obtain richer phase structure information such as positive electrode active material and foil, negative electrode active material and foil under in-situ electrochemical conditions.

[0023] The in-situ transmission XRD stacked mold battery of the present invention can obtain all the information of the in-situ battery by means of transmission, which solves the problem that the existing test method of reflective in-situ battery can only obtain the information of the reflective surface component.

[0024] The in-situ transmission XRD stacked mold battery of the present invention, since the stacked cells do not undergo laser welding or ultrasonic welding as in traditional cells, makes it easier to remove the positive electrode, negative electrode and separator in the stacked cells for other tests and analyses. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the A / B side in-situ cell structure of the stacked mold battery for in-situ transmission XRD according to the present invention.

[0026] Figure 2 This is a schematic diagram of the A / B side in-situ cell structure and sealing ring of the stacked mold battery for in-situ transmission XRD according to the present invention.

[0027] Figure 3 This is a schematic diagram of the stacked cell structure of the stacked mold battery for in-situ transmission XRD of the present invention, wherein a is a schematic diagram of the negative electrode, b is a schematic diagram of the separator, and c is a schematic diagram of the positive electrode. In the figure, 1-cell fixing shell, 101-cell groove, 102-annular groove, 2-conductive sheet, 3-sealing ring, 4-negative electrode active coating, 5-negative electrode foil layer, 6-separator, 7-positive electrode active coating, 8-positive electrode foil layer.

[0028] Figure 4 This is a schematic diagram of the method of using the stacked mold battery for in-situ transmission XRD of the present invention. In the figure, the stacked mold battery consists of an in-situ cell on side A, a negative electrode, a separator, a positive electrode, and an in-situ cell on side B from left to right. The detector is part of a transmission X-ray diffractometer.

[0029] Figure 5The figures show the in-situ transmission XRD test results of a stacked mold battery used in Example 1 of this invention. In the figures, the positive electrode (003) refers to the 003 crystal plane diffraction peak of the positive electrode active coating, the positive electrode (101) refers to the 101 crystal plane diffraction peak of the positive electrode active coating, the positive electrode (104) refers to the 104 crystal plane diffraction peak of the positive electrode active coating, the positive electrode (015) refers to the 015 crystal plane diffraction peak of the positive electrode active coating, and the positive electrode (107) refers to the 003 crystal plane diffraction peak of the positive electrode active coating. The 107 crystal plane diffraction peak, positive electrode (110) refers to the 110 crystal plane diffraction peak of the positive electrode active coating, negative electrode (002) refers to the 002 crystal plane diffraction peak of the negative electrode active coating, aluminum foil (111), aluminum foil (200), and aluminum foil (220) refer to the 111, 200, and 220 crystal plane diffraction peaks of the positive electrode foil layer (aluminum foil) respectively, and copper foil (111) and copper foil (200) refer to the 111 and 200 crystal plane diffraction peaks of the negative electrode foil layer (copper foil) respectively. Detailed Implementation

[0030] To further understand the present invention, preferred embodiments of the present invention are described below. However, it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, and not for limiting the scope of the claims of the present invention.

[0031] like Figure 1-3 As shown, the in-situ transmission XRD stacked mold battery of the present invention includes an A-side in-situ cell, a B-side in-situ cell, stacked cells, and electrolyte. The in-situ cell on side A and the in-situ cell on side B each include a cell fixing shell 1 and conductive sheets 2 fixed on both sides of the cell fixing shell. The stacked battery cell is clamped and fixed in the sealed cavity formed by the battery cell fixing shell 1 of the in-situ cell on side A and the in-situ cell on side B, and the negative electrode tab area and the positive electrode tab area of ​​the stacked battery cell extend out of the sealed cavity. The two outermost negative electrode tab areas are in contact with the two conductive plates 2 on the same side of the in-situ cell on side A and the in-situ cell on side B, respectively, and the two outermost positive electrode tab areas are in contact with the two conductive plates 2 on the other side of the in-situ cell on side A and the in-situ cell on side B, respectively. The electrolyte is injected into the sealed cavity.

[0032] In some embodiments, the A-side in-situ cell and the B-side in-situ cell each include a cell fixing shell 1 and two conductive sheets 2. The cell fixing shell 1 consists of a shell and two ear structures. The surface of the shell has a cell groove 101, and the two ear structures are fixed to both sides of the shell. Preferably, the shell and the two ear structures are integrally formed. Preferably, the shell and the cell groove 101 are coaxial. Preferably, one surface of the ear structure is in the same plane as the surface of the shell with the cell groove 101. The two conductive sheets 2 are fixed to the two ear structures, and their edges extend out of the ear structures. Preferably, the material of the cell fixing shell 1 is polytetrafluoroethylene, polyetheretherketone, polyphenylene sulfide, polyphenylene sulfone, polysulfone, polyethersulfone, perfluoroalkoxy resin, fluorinated ethylene propylene copolymer, etc.; the material of the conductive sheets 2 is metal. The cell fixing shell 1 provides structural support for the stacked cells, and the cell groove 101 is used for positioning the stacked cells so that the stacked cells can be well clamped and fixed within the cell fixing shell 1. Two conductive pieces 2 are used to connect the positive electrode tab region and the negative electrode tab region, respectively. The two tab structures fix the conductive pieces 2 and are used to clamp the conductive piece 2 on one side and the positive electrode tab region, as well as the conductive piece 2 on the other side and the negative electrode tab region.

[0033] In some embodiments, an annular groove 102 is preferably formed on the outer surface of the casing outside the outer edge of the cell groove 101. At least four screw holes are formed on the outer surface of the casing outside the outer edge of the annular groove 102. A preferred in-situ transmission XRD stacked mold battery also includes a sealing ring 3, which is placed in the annular groove 102. After the cell grooves 101 of the A-side in-situ cell and the B-side in-situ cell are combined facing each other, a cavity is formed. The stacked cell is placed in the cavity, and the A-side and B-side in-situ cells are fixed by bolts, which provide sufficient clamping force to secure the stacked cell. The sealing ring 3 achieves a seal on the stacked cell, isolating it from the influence of external air and moisture on its performance and preventing electrolyte leakage inside the stacked cell.

[0034] In some implementations, it is preferred that the in-situ pools on side A and side B are the same.

[0035] In this invention, the stacked battery cell has an existing structure, including several positive electrode sheets and several negative electrode sheets. The negative electrode sheet includes a negative electrode foil layer 5 and a negative electrode active coating 4. The negative electrode foil layer 5 is composed of a negative electrode tab region and a negative electrode active coating region. The negative electrode active coating 4 is fixed on the inner and outer surfaces of the negative electrode active coating region. The positive electrode sheet includes a positive electrode foil layer 8 and a positive electrode active coating 7. The positive electrode foil layer 8 is composed of a positive electrode tab region and a positive electrode active coating region. The positive electrode active coating 7 is fixed on the inner and outer surfaces of the positive electrode active coating region. The positive electrode sheets and negative electrode sheets are stacked alternately, and adjacent positive electrode sheets and negative electrode sheets are separated by a separator 6. The negative electrode tab regions of adjacent negative electrode sheets are in contact, and the positive electrode tab regions of adjacent positive electrode sheets are in contact.

[0036] In some embodiments, the material of the positive electrode foil layer 8 is not particularly limited and is set according to the testing requirements, such as aluminum foil. The material of the positive electrode active coating 7 is a positive electrode active material, which is not particularly limited and is set according to the testing requirements, such as ternary positive electrode material. The material of the negative electrode foil layer 5 is not particularly limited and is set according to the testing requirements, such as copper foil. The material of the negative electrode active coating 4 is a negative electrode active material, which is not particularly limited and is set according to the testing requirements, such as graphite material.

[0037] In this invention, the separator 6 is a prior art material, preferably a porous structure. After the electrolyte is injected, some of the electrolyte will fill the pores of the separator 6. The separator 6 is used to isolate the positive and negative electrodes to prevent internal short circuits and to transfer lithium ions between the positive and negative electrodes.

[0038] In some embodiments, the negative electrode active coating 4 on the negative electrode side needs to completely cover the positive electrode active coating 7 on the opposite positive electrode side, and the positive electrode tab region of the positive electrode needs to be at least partially exposed. Similarly, the separator 6 needs to completely cover the negative electrode active coating 4 on the adjacent negative electrode side, and the negative electrode tab region of the negative electrode needs to be partially exposed. Therefore, the size of the separator 6 needs to be larger than the size of the negative electrode active coating 4 on the negative electrode side; generally, the length and width directions need to be ≥2mm. The size of the negative electrode active coating 4 on the negative electrode side needs to be larger than the size of the positive electrode active coating 7 on the positive electrode side; generally, the length and width directions need to be ≥2mm. During stacking, the negative electrode tab region and the positive electrode tab region are located opposite each other on both sides of the separator 6.

[0039] In this invention, there are no special restrictions on the electrolyte; for example, the electrolyte commonly used in lithium-ion batteries can be used.

[0040] In this invention, since the outermost coating cannot participate in the reaction, the design of the stacked cell can be adjusted as needed. When it is necessary to eliminate the interference of the non-reactive positive electrode diffraction signal on the positive electrode in-situ charge and discharge signal, the outermost layer of the stacked battery can be a negative electrode sheet, or the outermost layer of the stacked battery can be a positive electrode sheet with a single-sided coating (i.e., the outer surface of the positive electrode sheet is a bare positive electrode foil layer 8 and the inner surface is a positive electrode active coating 7, and the positive electrode active coating 7 on the inner surface is also opposite to the negative electrode active coating 4 of the adjacent negative electrode sheet, with a separator 6 in between). When it is necessary to eliminate the interference of the non-reactive negative electrode diffraction signal on the negative electrode in-situ charge and discharge signal, the outermost layer of the stacked battery can be a positive electrode sheet, or the outermost layer of the stacked battery can be a negative electrode sheet with a single-sided coating (i.e., the outer surface of the negative electrode sheet is a bare negative electrode foil layer 5 and the inner surface is a negative electrode active coating 4, and the negative electrode active coating 4 on the inner surface is also opposite to the positive electrode active coating 7 of the adjacent positive electrode sheet, with a separator 6 in between).

[0041] The assembly method of the stacked cell with the in-situ transmission XRD of the present invention and the in-situ cells on side A and side B is as follows: The stacked cell is placed in the cell groove 101 of the in-situ cell on side A, with the direction aligned with the stacking of the stacked cells and the slotting direction of the cell groove 101. A sealing ring 3 is placed, and electrolyte is injected into the in-situ cell on side A. The in-situ cell on side B is then closed (or the in-situ cell on side B can be closed first, and electrolyte injected into both the in-situ cells on side A and side B through the gap). The bolts are then used to secure the cells. The stacked cells are clamped and fixed in the sealed cavity formed by the cell fixing shell 1 of the in-situ cell on side A and side B, and the negative electrode tab area and positive electrode tab area of ​​the stacked cells extend out of the sealed cavity. The two outermost negative electrode tab areas are in contact with the two conductive sheets 2 on the same side of the in-situ cell on side A and side B, respectively, and the two outermost positive electrode tab areas are in contact with the two conductive sheets 2 on the other side of the in-situ cell on side A and side B, respectively, thus obtaining a stacked mold battery for in-situ transmission XRD.

[0042] like Figure 4 As shown, the method of using the stacked mold battery for in-situ transmission XRD of the present invention includes the following steps: S1. Place the in-situ transmission XRD stacked mold cell on the sample stage of the transmission X-ray diffractometer for in-situ electrochemical testing. After the test is completed, remove the in-situ transmission XRD stacked mold cell. S2. Remove the in-situ cell from side B of the stacked cell using the in-situ transmission XRD test. Then remove the stacked cell. Since the stacked cell has not undergone laser welding or ultrasonic welding as traditional cells, the positive electrode, negative electrode and separator 6 in the stacked cell are easier to remove and can be used for other tests and analyses.

[0043] When it is necessary to eliminate the interference of non-reactive positive electrode diffraction signals on the positive electrode in-situ charge and discharge signals, the outermost layer of the stacked battery can all be negative electrode sheets, or the outermost layer of the stacked battery can be a single-sided coated positive electrode sheet (i.e., the outer surface of the positive electrode sheet is a positive electrode foil layer 8 and the inner surface is a positive electrode active coating 7); when it is necessary to eliminate the interference of non-reactive negative electrode diffraction signals on the negative electrode in-situ charge and discharge signals, the outermost layer of the stacked battery can all be positive electrode sheets, or the outermost layer of the stacked battery can be a single-sided coated negative electrode sheet (i.e., the outer surface of the negative electrode sheet is a negative electrode foil layer 5 and the inner surface is a negative electrode active coating 4).

[0044] The terminology used in this invention generally has the meanings commonly understood by those skilled in the art, unless otherwise stated.

[0045] To enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described in detail below with reference to embodiments. The embodiments described are merely specific descriptions of the claims of the present invention, and the claims include, but are not limited to, the content of the described embodiments.

[0046] Example 1 The in-situ transmission XRD-based stacked mold battery includes an A-side in-situ cell, a B-side in-situ cell, stacked cells, electrolyte, and sealing rings. The A-side and B-side in-situ cells have the same structure. The A-side in-situ cell includes a cell fixing shell 1 and two conductive plates 2. The cell fixing shell 1 consists of a shell and two ear structures. The surface of the shell has a cell groove 101. An annular groove 102 is formed on the outer surface of the shell outside the outer edge of the cell groove 101. At least four screw holes are formed on the outer surface of the shell outside the outer edge of the annular groove 102. The two ear structures are fixed on both sides of the shell, and the two conductive plates 2 are fixed on the two ear structures, with their edges extending out of the ear structures. The sealing ring 3 is placed in the annular groove 102.

[0047] The laminated battery cell has an existing structure, comprising several positive electrode sheets and several negative electrode sheets. Each negative electrode sheet includes a negative electrode foil layer 5 and a negative electrode active coating layer 4. The negative electrode foil layer 5 consists of a negative electrode tab region and a negative electrode active coating region. The negative electrode active coating layer 4 is fixed on the inner and outer surfaces of the negative electrode active coating region. Each positive electrode sheet includes a positive electrode foil layer 8 and a positive electrode active coating layer 7. The positive electrode foil layer 8 consists of a positive electrode tab region and a positive electrode active coating region. The positive electrode active coating layer 7 is fixed on the inner and outer surfaces of the positive electrode active coating region. The positive and negative electrode sheets are stacked alternately, and a separator 6 is provided between adjacent positive and negative electrode sheets. The negative electrode tab regions of adjacent negative electrode sheets are in contact, and the positive electrode tab regions of adjacent positive electrode sheets are in contact. The positive electrode foil layer 8 is made of aluminum foil, and the negative electrode foil layer 5 is made of copper foil. The positive electrode active coating layer 7 uses a ternary positive electrode material, and the negative electrode active coating layer 4 uses graphite material. The separator 6 is made of polyethylene material. The size of the separator 6 needs to be larger than the size of the negative electrode active coating 4 on the negative electrode side. Generally, the length and width need to be ≥2mm. The size of the negative electrode active coating 4 on the negative electrode side needs to be larger than the size of the positive electrode active coating 7 on the positive electrode side. Generally, the length and width need to be ≥2mm.

[0048] The stacked cells are placed in the cell groove 101 of the in-situ cell on side A, with the direction consistent with the stacking of the stacked cells and the slotting direction of the cell groove 101. Electrolyte is injected, and the in-situ cell on side B is closed. The stacked cells are clamped and fixed in the sealed cavity formed by the cell fixing shell 1 of the in-situ cells on side A and side B. The negative electrode tab area and the positive electrode tab area of ​​the stacked cells extend out of the sealed cavity. The two outermost negative electrode tab areas are in contact with the two conductive sheets 2 on the same side of the in-situ cells on side A and side B, respectively. The two outermost positive electrode tab areas are in contact with the two conductive sheets 2 on the other side of the in-situ cells on side A and side B, respectively. This yields a stacked mold battery for in-situ transmission XRD.

[0049] The method of using the in-situ transmission XRD stacked mold cell: S1. Place the in-situ transmission XRD stacked mold cell on the sample stage of the transmission X-ray diffractometer (DEEP-TXRD type transmission diffractometer produced by Beijing Zhongyan Huanke Technology Co., Ltd.) for in-situ electrochemical testing. Use a molybdenum target, set the voltage to 40kV and the current to 40mA. After the test is completed, remove the in-situ transmission XRD stacked mold cell. S2. Remove the in-situ cell on side B of the stacked cell from the in-situ cell on side A after the in-situ XRD test is completed, and then remove the stacked cell.

[0050] Test results as follows Figure 5 As shown. From Figure 5 It can be seen that the collected in-situ XRD information includes the characteristic diffraction peak information of the positive electrode active coating material (ternary positive electrode material), the positive electrode foil material (aluminum foil), the negative electrode active coating material (graphite material), and the negative electrode foil material (copper foil). Based on the characteristic diffraction peak information, the changes of the corresponding materials during battery charging or discharging can be determined. Figure 5 The left side corresponds to the charge-discharge curve of the battery over time, and the right side corresponds to the change in diffraction intensity at the 2θ angle over time. When the battery is charged and discharged, the charge-discharge curve on the left shows that the battery voltage changes over time. At this time, a chemical reaction of lithium ions intercalating and deintercalating between the positive and negative electrodes occurs inside the battery. The diffraction peak positions of the (003), (101), (104), (015), (107), and (110) crystal planes of the ternary positive electrode material shift over time, and the diffraction peak positions of the (002) crystal plane of the graphite material also shift over time. The shift in the diffraction peak positions between the positive and negative electrodes is caused by the lattice distortion caused by lithium ions being extracted or intercalated between the positive and negative electrode lattices. In this embodiment, aluminum foil and copper foil are positive and negative current collectors, respectively. They only play the role of collecting current during battery charging and discharging, without changing or participating in the reaction. Therefore, the positions of the diffraction peaks of the (111), (200), and (220) crystal planes of aluminum foil and the (111) and (200) crystal planes of copper foil do not change with the charging and discharging time.

[0051] The battery and its usage method provided by this patent can reveal the phase structure change law of key materials such as positive and negative electrodes during the charging and discharging process. This is very important for studying and improving the performance of current material systems and can also provide basic theoretical data support for the development of next-generation battery materials and battery technologies.

[0052] Obviously, the above embodiments are merely examples for clear illustration and are not intended to limit the embodiments. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all embodiments here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A coin cell for in-situ transmission XRD comprising a coin cell and an electrolyte, characterized in that, The A-side in-situ cell and the B-side in-situ cell are further included; The A-side in-situ cell and the B-side in-situ cell respectively include an electric core fixing shell (1) and a conductive sheet (2) fixed on both sides of the electric core fixing shell; The laminated core cell is clamped and fixed in the sealed cavity formed by the electric core fixing shell (1) of the A-side in-situ cell and the B-side in-situ cell, and the negative tab area and the positive tab area of the laminated core cell protrude out of the sealed cavity, the two outermost negative tab areas are respectively in contact with the two conductive sheets (2) on the same side of the A-side in-situ cell and the B-side in-situ cell, and the two outermost positive tab areas are respectively in contact with the two conductive sheets (2) on the other side of the A-side in-situ cell and the B-side in-situ cell; The electrolyte is injected into the sealed cavity.

2. The laminated pouch cell for in-situ transmission XRD of claim 1, wherein, The A-side in-situ cell and the B-side in-situ cell respectively include an electric core fixing shell (1) and two conductive sheets (2), the electric core fixing shell (1) is composed of a shell and two ear structures, the surface of the shell is provided with an electric core groove (101), the two ear structures are respectively fixed on both sides of the shell, and the two conductive sheets (2) are respectively fixed on the two ear structures and have edges extending out of the ear structures.

3. The laminated pouch cell for in-situ transmission XRD of claim 2, wherein, Possess one or more of the following characteristics: The A-side in-situ cell and the B-side in-situ cell are the same; The shell and the two ear structures are integrally formed; The shell and the electric core groove (101) are coaxial; One surface of the ear structure is in the same plane as the surface of the shell provided with the electric core groove (101); The laminated mold cell for in-situ transmission XRD further includes a sealing ring (3), an annular groove (102) is provided on the surface of the shell outside the outer edge of the electric core groove (101), and the sealing ring (3) is installed in the annular groove (102).

4. The laminated pouch cell for in-situ transmission XRD of claim 3, wherein, A plurality of screw holes are provided on the surface of the shell outside the outer edge of the annular groove (102), the A-side in-situ cell and the B-side in-situ cell are fixed and connected by bolts, and the laminated core cell is clamped and fixed.

5. The laminated pouch cell for in-situ transmission XRD of claim 1, wherein, The laminated core cell includes a plurality of positive plates and a plurality of negative plates, the negative plate includes a negative foil layer (5) and a negative active coating layer (4), the negative foil layer (5) is composed of a negative tab area and a negative active coating area, the negative active coating layer (4) is fixed on the inner and outer surfaces of the negative active coating area, the positive plate includes a positive foil layer (8) and a positive active coating layer (7), the positive foil layer (8) is composed of a positive tab area and a positive active coating area, and the positive active coating layer (7) is fixed on the inner and outer surfaces of the positive active coating area, the positive plate and the negative plate are alternately stacked, and the adjacent positive plate and the adjacent negative plate are separated by a separator (6), the negative tab area of the adjacent negative plate is in contact, and the positive tab area of the adjacent positive plate is in contact.

6. The laminated pouch cell for in-situ transmission XRD of claim 5, wherein, The negative active coating layer (4) on one side of each negative plate completely covers the positive active coating layer (7) on the opposite side of the adjacent positive plate, and the positive tab area of the positive plate is at least partially exposed, and the separator (6) completely covers the negative active coating layer (4) on the side of the adjacent negative plate, and the negative tab area of the negative plate is at least partially exposed.

7. The laminated pouch cell for in-situ transmission XRD of claim 5, wherein, The outermost side of the laminated core cell is a negative plate, or the outer surface of the positive plate is a bare positive foil layer (8) and the inner surface is a positive active coating layer (7).

8. The laminated pouch cell for in-situ transmission XRD of claim 5, wherein, The outermost side of the laminated battery is a positive electrode sheet, or the outer surface is a bare negative electrode foil layer (5) and the inner surface is a negative electrode active coating layer (4) of a negative electrode sheet.

9. The method of using a laminated pouch cell for in situ transmission XRD according to any one of claims 1-8, wherein, The steps are as follows: S1. Place the in-situ transmission XRD laminated mold battery on the sample stage of the transmission X-ray diffractometer for in-situ electrochemical testing. After the test is completed, remove the in-situ transmission XRD laminated mold battery; S2. Remove the B-side in-situ cell from the A-side in-situ cell of the tested in-situ transmission XRD laminated mold battery, and then remove the laminated battery.

10. The method of using a laminated pouch cell for in-situ transmission XRD of claim 9, wherein, When the interference of the positive electrode diffraction signal not participating in the reaction on the positive electrode in-situ charge-discharge signal is excluded, the outermost side of the laminated battery is a negative electrode sheet, or the outer surface is a bare positive electrode foil layer (8) and the inner surface is a positive electrode active coating layer (7) of a positive electrode sheet; When the interference of the negative electrode diffraction signal not participating in the reaction on the negative electrode in-situ charge-discharge signal is excluded, the outermost side of the laminated battery is a positive electrode sheet, or the outer surface is a bare negative electrode foil layer (5) and the inner surface is a negative electrode active coating layer (4) of a negative electrode sheet.

Citation Information

Patent Citations

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