A synchrotron radiation source transmission XRD cell

Abstract

The present application relates to the technical field of button cells, and discloses a synchrotron radiation light source transmission type XRD cell. The cell comprises a positive electrode shell and a negative electrode shell, wherein a first glass carbon gasket, a positive electrode plate, a diaphragm, a negative electrode plate and a second glass carbon gasket are stacked in sequence between the positive electrode shell and the negative electrode shell, and the negative electrode shell is embedded in the positive electrode shell; a first through hole is provided in the middle of the positive electrode shell, and a second through hole is provided in the middle of the negative electrode shell, and a window film is provided at the first through hole and the second through hole; X-rays are injected through the second through hole, and sequentially transmit through the second glass carbon gasket, the negative electrode plate, the diaphragm, the positive electrode plate and the first glass carbon gasket, and are emitted from the first through hole to an external signal receiver. The cell provided by the present application takes into account both X-ray signal output and normal electrochemical cycle characteristics, and realizes in-situ X-ray detection while ensuring the normal performance of the cell without blocking X-rays from entering and exiting the cell.

Description

Technical Field

[0001] The present application relates to the technical field of button cells, and in particular to a synchrotron radiation light source transmission-type XRD cell. Background Art

[0002] X-ray powder diffraction (XRD) is a rapid phase structure detection technology. Thanks to the advantages of low absorption and high penetration of X-rays, X-ray powder diffraction is often used to identify average and overall information, such as phase composition in a mixture, overall stress analysis, etc. At the same time, the charging and discharging process of lithium and sodium batteries is a process accompanied by the delatency of lithium and sodium, during which a series of phase changes are induced. Therefore, in order to study the specific changes in electrode materials during this process, researchers often use in-situ XRD methods to observe electrode materials in real time. However, it is limited by the low light source power and low signal intensity of laboratory X-ray diffractometers.

[0003] Unlike the traditional laboratory reflection mode XRD, the synchrotron radiation light source adopts the transmission mode, that is, the X-rays enter from one end of the in-situ electrolytic cell and are output from the other end. Therefore, unlike the reflection in-situ XRD model which only requires a single-sided path design at the signal end, the transmission in-situ XRD based on synchrotron radiation requires a transparent path design for the entire mold. However, in addition to the requirements for the signal path, the realization of normal electrochemical circulation is also necessary for in-situ XRD. Therefore, it is necessary to fully consider the airtightness of the battery, the necessary pressure between the positive and negative electrodes, and the low path loss of the signal under the transparent path design. Therefore, higher requirements are put forward for the design of the in-situ XRD model than for the reflection type.

[0004] In summary, how to design an in-situ battery design that takes into account both X-ray signal output and normal electrochemical cycle characteristics based on the signal characteristics of the synchrotron radiation transmission X-ray optical path has become a problem that needs to be solved. Utility Model Content

[0005] The technical problem to be solved by the present application is to provide an in-situ battery that takes into account both X-ray signal output and normal electrochemical cycle characteristics, so as to ensure the normal performance of the battery and perform in-situ X-ray detection without blocking the X-rays from entering and exiting the battery.

[0006] In order to solve the above problems, the present application provides a synchrotron radiation light source transmission XRD cell, comprising a positive electrode shell and a negative electrode shell, wherein a first glass carbon gasket, a positive electrode plate, a diaphragm, a negative electrode plate and a second glass carbon gasket are stacked in sequence between the positive electrode shell and the negative electrode shell, and the negative electrode shell is embedded in the positive electrode shell; a first through hole is opened in the middle position of the positive electrode shell, and a second through hole is opened in the middle position of the negative electrode shell, and window films are provided at the first through hole and the second through hole; X-rays are emitted from the second through hole, and are transmitted through the second glass carbon gasket, the negative electrode plate, the diaphragm, the positive electrode plate and the first glass carbon gasket in sequence, and are emitted from the first through hole to an external signal receiver.

[0007] Preferably, the diameter of the first through hole and / or the second through hole is 1 mm to 3 mm.

[0008] Preferably, the diameter of the first through hole and / or the second through hole is preferably 2 mm.

[0009] Preferably, the edge of the window film is respectively sealed at the first through hole and the second through hole through a silicone-based adhesive layer.

[0010] Preferably, the window film is a polyimide film.

[0011] Preferably, the positive electrode plate uses porous carbon paper as the positive electrode fluid.

[0012] Preferably, the positive electrode plate uses nickel foam as the positive electrode fluid.

[0013] Preferably, the positive electrode plate uses aluminum as the positive electrode fluid.

[0014] Preferably, the diameters of the positive electrode sheet and the negative electrode sheet are both smaller than the diameter of the diaphragm.

[0015] Preferably, the negative electrode plate is a lithium plate or a sodium plate.

[0016] Compared with the prior art, the present invention has at least one of the following beneficial technical effects:

[0017] The transparent passage design with double openings in the middle of the positive and negative shells constitutes a double opening system, which can meet the needs of transmission X-rays of synchrotron radiation light sources. Since glassy carbon itself absorbs less X-rays, glassy carbon is selected as the gasket material to set the first glassy carbon gasket and the second glassy carbon gasket. It can be clamped on both sides of the positive and negative pole pieces under the premise of avoiding the gasket openings, and give sufficient pressure to the positive and negative electrodes in the through-hole interval, thereby ensuring the normal electrochemical cycle in the interval, so that the obtained electrochemical in-situ XRD data is true and valid. In this way, the normal performance of the battery is guaranteed without blocking the X-rays from entering and exiting the battery, and in-situ X-ray detection is performed. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0019] Figure 1 Schematic diagram of the overall structure of the synchrotron radiation light source transmission XRD cell provided in an embodiment of the present application.

[0020] Explanation of the reference numerals: 1. positive electrode shell; 11. first through hole; 2. first glassy carbon gasket; 3. positive electrode plate; 4. diaphragm; 5. negative electrode plate; 6. second glassy carbon gasket; 7. negative electrode shell; 71. second through hole; 8. window film; 9. silicone-based adhesive layer. DETAILED DESCRIPTION

[0021] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0022] It should be understood that when used in this specification and the appended claims, the terms "include" and "comprises" indicate the presence of described features, integers, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or combinations thereof.

[0023] It should also be understood that the terms used in this application specification are only for the purpose of describing specific embodiments and are not intended to limit the application. As used in this application specification and the appended claims, the singular forms "a", "an" and "the" are intended to include plural forms unless the context clearly indicates otherwise.

[0024] It should be further understood that the term “and / or” used in the specification and appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes these combinations.

[0025] Please refer to Figure 1The present application uses a button cell as a substrate to provide a synchrotron radiation source transmission XRD cell for transmission in-situ X-ray detection. The manufacturing method is simple and easy, and the raw materials are abundant and easy to obtain. The transmission path of the X-ray is shown by the arrow in the attached figure.

[0026] Specifically, the battery includes a positive electrode shell 1 and a negative electrode shell 7, and a first glass carbon gasket 2, a positive electrode plate 3, a diaphragm 4, a negative electrode plate 5 and a second glass carbon gasket 6 are stacked in sequence between the positive electrode shell 1 and the negative electrode shell 7, and the negative electrode shell 7 is embedded and fixed in the positive electrode shell 1. A first through hole 11 is provided in the middle of the positive electrode shell 1, and a second through hole 71 is provided in the middle of the negative electrode shell 7. Window films 8 are provided at the first through hole 11 and the second through hole 71. X-rays are injected into the battery through the second through hole 71, and are transmitted through the second glass carbon gasket 6, the negative electrode plate 5, the diaphragm 4, the positive electrode plate 3 and the first glass carbon gasket 2 in sequence, and are emitted from the first through hole 11 to an external signal receiver.

[0027] Here, the transparent passage design with double openings in the middle of the positive electrode shell 1 and the negative electrode shell 7 constitutes a double opening system, which can meet the needs of transmission X-rays of synchrotron radiation light sources. Since glassy carbon itself absorbs less X-rays, glassy carbon is selected as the gasket material to set the first glassy carbon gasket 2 and the second glassy carbon gasket 6. It can be clamped on the opposite sides of the positive electrode plate 3 and the negative electrode plate 5 under the premise of avoiding the gasket openings, and give sufficient pressure to the positive and negative electrodes in the through-hole interval, thereby ensuring the normal electrochemical cycle in the interval, so that the obtained electrochemical in-situ XRD data is true and valid. In this way, it is achieved that the normal performance of the battery is guaranteed without blocking the X-rays from entering and exiting the battery, and in-situ X-ray detection is performed.

[0028] In a specific embodiment, a first through hole 11 is opened in the middle of the positive electrode shell 1 and a second through hole 71 is opened in the middle of the negative electrode shell 7 by perforation processes such as laser cutting, drill drilling or electrospark machining. Then, according to the general button battery assembly process, the positive electrode shell 1, the first glass carbon gasket 2, the positive electrode plate 3, the diaphragm 4, the negative electrode plate 5, the second glass carbon gasket 6 and the negative electrode shell 7 are stacked in order, and a certain amount of electrolyte is dripped on both sides of the diaphragm 4 to complete the assembly of the button battery for the transmission electrochemical in-situ XRD test of the synchrotron radiation light source. The assembled button battery is connected to an external charging and discharging device and placed on an external sample rack to perform the charging and discharging in-situ XRD test.

[0029] In a specific embodiment, the diameter of the first through hole 11 and / or the second through hole 71 is 1 mm to 3 mm, for example, 1 mm, 2 mm or 3 mm, and other sizes that meet the requirements. In this embodiment, the diameter of the first through hole 11 and / or the second through hole 71 is preferably 2 mm to match the irradiation area of ​​the synchrotron radiation line station and ensure that the signal path is unobstructed, thereby taking into account the synchrotron radiation spot size (<1 mm) and reducing the impact of the double-opening system on the normal electrochemical cycle, and further optimizing the operation effect of the overall design of the battery.

[0030] In a specific embodiment, the electrochemical in-situ cell further includes a silicone-based adhesive layer 9, and the window film 8 is respectively sealed at the first through hole 11 and the second through hole 71 by the silicone-based adhesive layer 9. When assembling the window film 8, the silicone-based adhesive is first applied to the periphery of the first through hole 11 and the second through hole 71 to form the silicone-based adhesive layer 9, and the edge of the window film 8 cut into a disc size is attached to the silicone-based adhesive layer 9, and the window film 8 can be fixed after the silicone-based adhesive layer 9 solidifies. In this regard, the silicone-based adhesive has a good sealing effect, which can reduce the volatilization of the internal electrolyte during the cycle process and improve the smoothness of the signal path. At the same time, the bonding process along the periphery of the first through hole 11 and the second through hole 71 also effectively prevents the destruction of the internal conductive network, thereby ensuring the overall conductive properties of the battery.

[0031] In a specific embodiment, the window film 8 is a polyimide film. The polyimide material is non-toxic and absorbs very little X-rays, which can reduce the loss of signals during the transmission process, thereby enhancing the output of the signal at the positive electrode shell 1.

[0032] In a specific embodiment, the positive electrode plate 3 can select porous carbon paper, nickel foam, aluminum and other materials as the positive electrode fluid, thereby effectively reducing the absorption of X-rays by the fluid, and further increasing the output of the signal. Here, since aluminum can absorb X-rays, when the positive electrode plate 3 selects aluminum as the positive electrode fluid, it needs to be made into a thin sheet, and the thickness is preferably reduced to less than 6 microns.

[0033] In a specific embodiment, the diameters of the positive electrode sheet 3 and the negative electrode sheet 5 are both smaller than the diameter of the diaphragm 4 to avoid short circuit between the positive electrode sheet 3 and the negative electrode sheet 5 , thereby preventing a short circuit of the battery.

[0034] In a specific embodiment, the negative electrode plate 5 is a lithium plate or a sodium plate, so that the overall structural design of the battery can be applied to lithium batteries or sodium batteries. Furthermore, the lithium plate or the sodium plate is required to have a smooth surface and no inert oxide layer to ensure normal charging and discharging behavior.

[0035] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed in the present application, and these modifications or replacements should be included in the protection scope of the present application. Therefore, the protection scope of the present application shall be based on the protection scope of the claims.

Claims

1. A synchrotron radiation source transmission XRD cell, characterized in that: It comprises a positive electrode shell and a negative electrode shell, wherein a first glass carbon gasket, a positive electrode plate, a diaphragm, a negative electrode plate and a second glass carbon gasket are stacked in sequence between the positive electrode shell and the negative electrode shell, and the negative electrode shell is embedded in the positive electrode shell; A first through hole is provided in the middle of the positive electrode shell, and a second through hole is provided in the middle of the negative electrode shell, and window films are provided at the first through hole and the second through hole; X-rays are injected through the second through hole, and sequentially transmit through the second glass carbon gasket, the negative electrode plate, the diaphragm, the positive electrode plate and the first glass carbon gasket, and are emitted from the first through hole to an external signal receiver.

2. A synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The diameter of the first through hole and / or the second through hole is 1 mm to 3 mm.

3. A synchrotron radiation source transmission XRD cell according to claim 2, characterized in that: The diameter of the first through hole and / or the second through hole is preferably 2 mm.

4. The synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The edges of the window film are respectively glue-sealed at the first through hole and the second through hole through a silicon-based glue layer.

5. A synchrotron radiation source transmission XRD cell according to claim 1 or 4, characterized in that: The window film is a polyimide film.

6. The synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The positive electrode plate uses porous carbon paper as the positive electrode fluid.

7. The synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The positive electrode plate uses nickel foam as the positive electrode fluid.

8. The synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The positive electrode plate uses aluminum as the positive electrode fluid.

9. The synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The diameters of the positive electrode sheet and the negative electrode sheet are both smaller than the diameter of the diaphragm.

10. The synchrotron radiation source transmission XRD cell according to claim 1, characterized in that: The negative electrode plate is selected from lithium plate or sodium plate.

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