CN116148235B - Solid-state battery transfer and in-situ synchrotron radiation absorption spectrum testing device - Google Patents

Solid-state battery transfer and in-situ synchrotron radiation absorption spectrum testing device Download PDF

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CN116148235B
CN116148235B CN202310415194.0A CN202310415194A CN116148235B CN 116148235 B CN116148235 B CN 116148235B CN 202310415194 A CN202310415194 A CN 202310415194A CN 116148235 B CN116148235 B CN 116148235B
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head
pressure
electrode
battery
upper electrode
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CN116148235A (en
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叶逸凡
丁红鹤
李鑫
徐吉龙
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University of Science and Technology of China USTC
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/42Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4285Testing apparatus
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Secondary Cells (AREA)
  • Testing Electric Properties And Detecting Electric Faults (AREA)

Abstract

The application relates to a solid-state battery transfer and in-situ synchrotron radiation absorption spectrum testing device. The battery transferring and in-situ synchrotron radiation absorption spectrum testing device comprises a fixed sample holder plug, wherein the surface of the fixed sample holder plug is connected with an upper electrode press head, a taper hole is formed in the surface of the upper electrode press head, the lower end face of the upper electrode press head is connected with an insulating press sheet die, a battery assembly to be tested is placed in the insulating press sheet die, a lower electrode press head capable of being inserted from below is further arranged in the insulating press sheet die, the upper electrode press head is connected with an upper working electrode screw, and the lower electrode press head is connected with a lower working electrode screw; the solid-state battery transfer and in-situ synchrotron radiation absorption spectrum testing device not only ensures the transfer of the battery under the condition of inert gas sealing protection, but also satisfies the in-situ acquisition of the electronic structure information of the battery electrode/interface in the working process of the battery under the specific stack pressure.

Description

Solid-state battery transfer and in-situ synchrotron radiation absorption spectrum testing device
Technical Field
The application relates to the field of battery testing, in particular to a solid-state battery transfer and in-situ synchrotron radiation absorption spectrum testing device.
Background
Solid state batteries are widely regarded as safer than liquid batteries because of their use of nonflammable solid state electrolytes, but unlike liquid electrolyte batteries, solid state batteries need to maintain a specific stack pressure during the operating cycle to avoid contact loss between the electrodes and the solid state electrolyte. How to effectively adjust the stack pressure of the battery through the device, so that the battery can work at the optimal performance, and the in-situ characterization test of the battery in the working state can be met, which is one of the difficulties in the research process of the solid-state battery. Because the solid-state Li-S cells are prepared in a glove box filled with inert gas, the solid-state Li-S cells are particularly sensitive to air components, and how to ensure that the devices are tested without transferring the air to other testing equipment after the device is prepared is also the key to determining whether the signal of the cell in the most realistic state can be detected. In particular, some characterization tests in synchrotron radiation spectroscopy require that the prepared battery be placed on a laboratory station instrument of a light source to perform the test, which means that researchers need to make an in-situ test characterization device that can match the laboratory station instrument. The method is limited by the current battery working device, and the electronic structure information of the electrode/interface in the working state of the solid-state Li-S battery in the most realistic (original preparation state) is difficult to obtain based on the synchronous radiation absorption spectrum technology. The application aims to provide an in-situ device capable of realizing basic functions, which can ensure that a self-sealing maintenance device of a Li-S battery maintains an initial preparation state and can ensure a synchronous radiation in-situ test scheme under a specific stack working pressure of the battery.
Disclosure of Invention
The application aims to solve the problems and provide a device which can not only meet the normal working stack pressure of a Li-S battery device, but also play a role in good self-sealing, so as to realize the transfer of the battery device without exposing air and finally realize the synchrotron radiation absorption spectrum test of the battery device in a working state. Compared with the conventional stripped battery internal material after the circulation work, the device can obtain the dynamic change information of the contact interface of the electrode material and the solid electrolyte under the working condition of the complete device, thereby providing good theoretical guidance for improving the battery performance.
The application realizes the above purpose through the following technical scheme:
the application provides a battery transferring and in-situ synchrotron radiation absorption spectrum testing device, which comprises a fixed sample holder plug, wherein the surface of the fixed sample holder plug is connected with an upper electrode pressing head, the surface of the upper electrode pressing head is provided with a taper hole, the lower end surface of the upper electrode pressing head is connected with an insulating pressing die, a battery component to be tested is placed in the insulating pressing die, a lower electrode pressing head which can be inserted from below is further arranged in the insulating pressing die, the upper electrode pressing head is connected with an upper working electrode screw, the lower electrode pressing head is connected with a lower working electrode screw, the lower electrode pressing head is also connected with a lower supporting plate, the lower supporting plate is connected with a driving structure which moves up and down, and based on the position of the lower supporting plate, the upper electrode pressing head and the lower electrode pressing head extrude electrodes of the battery component with set stack pressure.
As a further optimization scheme of the application, the fixed sample holder plug comprises a flat plate with screw holes on the surface, the screw holes on the surface of the flat plate are connected with fastening screws, the surface of the fastening screws is also sleeved with T-shaped insulating cylinders, the fastening screws are matched with the T-shaped insulating cylinders to connect the upper electrode pressure head and the flat plate, and an upper insulating plate is further arranged between the upper electrode pressure head and the flat plate; an upper sealing ring and a lower sealing ring are respectively arranged at the upper end face and the lower end of the insulating tabletting mold; and a lower insulating plate is arranged between the lower electrode pressing head and the lower supporting plate.
As a further optimization scheme of the application, the driving structure comprises a rod piece, the upper end of the rod piece is connected with the upper electrode pressure head, the lower part of the rod piece is sleeved with a lower supporting plate, and the height of the lower supporting plate is adjusted based on the set stacking pressure.
As a further optimization scheme of the application, the rod piece is a pressing fixed screw rod, the pressing fixed screw rod penetrates through the lower supporting plate, a fastening nut is connected to the penetrating end, and the stacking pressure is adjusted based on the position of the fastening nut adjusted by a torque wrench.
As a further optimization scheme of the application, the rod piece is a guide rod, the lower supporting plate is sleeved on the surface of the guide rod to move up and down, the lower end face of the lower supporting plate is fixedly connected with a driving source, the driving end of the driving source is connected with a movable sleeve, the movable sleeve is in threaded connection with a movable screw rod, the movable screw rod is fixedly connected with a connecting plate, the movable screw rod is fixedly connected with the guide rod through the connecting plate, the driving source drives the movable sleeve to rotate, and the movable sleeve moves up and down on the surface of the movable screw rod.
As a further optimization scheme of the application, the upper end face of the lower supporting plate is provided with a pressure detection assembly, the pressure detection assembly comprises a pressure column, the surface of the pressure column is fixedly connected with a pressure measuring plate, the surface of the guide rod is fixedly connected with a fixed plate, the surface of the pressure measuring plate is provided with a pressure sensor, and when the lower electrode pressure head is matched with the battery assembly to be contacted with the upper electrode pressure head, the pressure sensor on the surface of the pressure measuring plate is contacted with the fixed plate.
As a further optimization scheme of the application, the upper electrode pressure head comprises a pressure head assembly, wherein the pressure head assembly comprises a beryllium sheet and a protection sheet, and the protection sheet is arranged below the beryllium sheet; the lower electrode pressure head comprises a calibration tube capable of moving up and down, the upper end face of the calibration tube is flush with the upper end face of the lower electrode pressure head, the lower movement limit distance of the calibration tube is the thickness distance of the protective sheet, and the side wall of the lower electrode pressure head is provided with an injection molding tube assembly.
As a further optimization scheme of the application, an inner groove is formed in the lower electrode pressure head, the inner groove is divided into an upper section and a lower section, the diameter of the upper section groove body is larger than that of the lower section groove body, the calibration pipe slides in the upper section groove body, an inner sliding groove is formed in the lower electrode pressure head above the lower section groove body, an inner sliding wedge block is arranged in the inner sliding groove, one end of the inner sliding wedge block is connected with a pull rope assembly, a wedge surface is also arranged at the edge position of the lower end face of the calibration pipe, one end of the pull rope assembly penetrates through the outer part of the lower electrode pressure head, and the end of the pull rope assembly is fixedly connected with a fixed block; the calibration pipe is a hollow annular pipe, a rod inserting piece is arranged in the middle of the calibration pipe, the lower end of the calibration pipe is connected with an internal pulling spring, and the internal pulling spring is arranged in the lower section of the inner groove.
As a further optimization scheme of the application, the surface of the lower electrode pressure head is also fixedly connected with an upper dynamic sealing component and a lower dynamic sealing component.
In a second aspect, the application provides a method of testing the absorption spectrum of synchrotron radiation in situ and for a battery, the method comprising,
installing the device as described above in an inert gas environment;
extruding the cell assembly at a set stack pressure;
closing the taper hole on the surface of the upper electrode pressure head, and transferring the device to a sample frame of the experimental station cavity;
vacuumizing the experimental station cavity, and simultaneously opening a taper hole on the surface of the sealed upper electrode pressure head;
the battery is in a working state through the electrode screw, the synchronous radiation light irradiates the battery through the taper hole on the surface of the upper electrode pressure head, and the detector of the experimental station collects fluorescent/electronic signals emitted after the synchronous radiation light excites the battery material.
As a further preferred embodiment of the present application,
prior to installation of the device as described above in an inert gas environment;
and measuring the thickness of the protective sheet in the pressure head assembly, and when the thickness of the protective sheet is lower than a preset threshold value, adding the protective sheet with corresponding thickness to be attached to the surface of the protective sheet of the pressure head assembly.
The application has the beneficial effects that: the method not only ensures the transfer of the battery under the condition of inert gas sealing protection, but also satisfies the in-situ acquisition of the electronic structure information of the battery electrode/interface in the working process of the battery under the specific stack pressure.
Drawings
FIG. 1 is a schematic view of the overall structure of the present application;
FIG. 2 is an exploded schematic view of all components of the present application;
FIG. 3 is a schematic view of another drive configuration of the present application;
FIG. 4 is a schematic view of the structure of the upper electrode indenter of the present application;
FIG. 5 is a schematic view of the structure of the lower electrode indenter of the present application;
FIG. 6 is a schematic view showing the structure of the lower electrode holder of the present application after the calibration tube has been moved down.
In the figure: 1. a fastening screw; 2. a T-shaped insulating cylinder; 3. an upper electrode pressing head; 4. an upper working electrode screw; 5. an upper insulating plate; 6. fixing a sample holder plug; 7. an upper sealing ring; 8. insulating tabletting mold; 9. a lower sealing ring; 10. a lower electrode indenter; 11. a lower working electrode screw; 12. a lower insulating plate; 13. pressing and fixing a screw rod; 14. a lower support plate; 15. a fastening nut; 16. moving the screw rod; 17. a connecting plate; 18. a driving source; 19. a guide rod; 20. moving the sleeve; 21. a pressure detection assembly; 22. a ram assembly; 23. a rod inserting piece; 24. calibrating a tube; 25. an inner chute; 26. a sliding wedge; 27. an inner pull spring; 28. an inner tank; 29. a fixed block; 30. a pull cord assembly; 31. an injection molded tube assembly; 32. an upper dynamic seal assembly; 33. a lower dynamic seal assembly.
Detailed Description
The subject matter described herein will now be discussed with reference to example embodiments. It is to be understood that these embodiments are merely discussed so that those skilled in the art may better understand and implement the subject matter described herein and that changes may be made in the function and arrangement of the elements discussed without departing from the scope of the disclosure herein. Various examples may omit, replace, or add various procedures or components as desired. In addition, features described with respect to some examples may be combined in other examples as well.
Example 1
As shown in fig. 1 and 2, a solid-state battery transferring and in-situ synchrotron radiation absorption spectrum testing device comprises a fixed sample holder plug 6, wherein the surface of the fixed sample holder plug 6 is connected with an upper electrode pressing head 3, a taper hole is formed in the surface of the upper electrode pressing head 3, the lower end surface of the upper electrode pressing head 3 is connected with an insulating pressing die 8, a battery component to be tested is placed in the insulating pressing die 8, a lower electrode pressing head 10 capable of being inserted from below is further arranged in the insulating pressing die 8, the upper electrode pressing head 3 is connected with an upper working electrode screw 4, the lower electrode pressing head 10 is connected with a lower working electrode screw 11, the lower electrode pressing head 10 is further connected with a lower supporting plate 14, the lower supporting plate 14 is connected with a driving structure capable of moving up and down, and based on the position of the lower supporting plate 14, the upper electrode pressing head 3 and the lower electrode pressing head 10 squeeze the electrode of the battery component with a set stack pressure.
It should be noted that, the embodiment can provide a device for the solid Li-S battery without exposing air transfer, and the battery can realize the absorption spectrum test under the working condition of a certain stack pressure (0-200 MPa, pressure is adjustable); in this embodiment, the fixed sample holder plug 6 can be regarded as a holder body of the whole device, any one of the holder body forms is within the scope of the present application, and in practice, the fixed sample holder plug 6 is an insert that can be mated with a sample holder of a synchrotron radiation absorption spectrum experiment station, and includes a cylindrical structure, in which a hole with a diameter of 10.1 mm is formed, a threaded hole of M4 is formed on a side, the cylindrical structure can be mated and inserted onto a sample holder of a synchrotron radiation absorption spectrum experiment station, and the threaded hole of M4 on the side is used for screw fastening.
The fixed sample holder plug 6 further comprises a flat plate with screw holes formed in the surface, the screw holes in the surface of the flat plate are connected with fastening screws 1, the surface of the fastening screws 1 is further sleeved with T-shaped insulating cylinders 2, the fastening screws 1 are matched with the T-shaped insulating cylinders 2 to connect the upper electrode pressing heads 3 with the flat plate, and an upper insulating plate 5 is further arranged between the upper electrode pressing heads 3 and the flat plate; an upper sealing ring 7 and a lower sealing ring 9 are respectively arranged at the upper end face and the lower end of the insulating tabletting mold 8; a lower insulating plate 12 is provided between the lower electrode head 10 and the lower support plate 14.
The upper sealing ring 7 and the lower sealing ring 9 are sealing O-shaped rings, and the insulating tabletting mold 8 is made of PEEK insulating materials; the T-shaped insulating cylinder 2 may be a T-shaped teflon insulating cylinder, and the lower insulating plate 12 is made of PEEK insulating material.
The driving structure comprises a rod piece, the upper end of the rod piece is connected with the upper electrode pressure head 3, the lower portion of the rod piece is sleeved with a lower supporting plate 14, and the height of the lower supporting plate 14 is adjusted based on the set stacking pressure.
Specifically, the rod is a pressing fixed screw rod 13, the pressing fixed screw rod 13 penetrates through the lower supporting plate 14, a fastening nut 15 is connected to the penetrating end, the position of the fastening nut 15 is adjusted based on a torque wrench, and the stacking pressure is adjusted.
When the application is used, the four pressing fixed screw rods 13 apply required pressure to the battery through the fastening nuts 15; the taper hole of the upper electrode pressure head 3 is sealed by polyimide adhesive tape, so that the whole battery is sealed in the PEEK insulating tabletting mold 8, and further air transfer can be isolated; when the absorption spectrum experiment station of the synchrotron radiation light source is tested, the fixed sample rack plug 6 is used for fixing the whole device to a sample rack of the experiment station cavity; the upper working electrode screw 4 and the lower working electrode screw 11 are connected with a charging and discharging power supply through a wire, so that the battery is in a working state, synchrotron radiation light irradiates the battery through a taper hole of the upper electrode pressure head 3, and a detector of an experiment station collects fluorescence/electronic signals emitted after the synchrotron radiation light excites battery materials.
Example 2
As shown in fig. 3, another driving structure is adopted on the basis of the above embodiment 1: the rod piece is a guide rod 19, the lower support plate 14 is sleeved on the surface of the guide rod 19 to move up and down, a driving source 18 is fixedly connected to the lower end face of the lower support plate 14, a moving sleeve 20 is connected to the driving end of the driving source 18, a moving screw rod 16 is connected to the moving sleeve 20 in a threaded mode, the moving screw rod 16 is fixedly connected with a connecting plate 17, the moving screw rod 16 is fixedly connected with the guide rod 19 through the connecting plate 17, the driving source 18 drives the moving sleeve 20 to rotate, and the moving sleeve 20 moves up and down on the surface of the moving screw rod 16.
It should be noted that, the driving source 18 may be a motor, which can meet the environment in embodiment 1, and the type of motor may be adopted, and the driving source 18 drives the moving sleeve 20 to rotate, so that the whole lower support plate 14 moves up and down, and provides corresponding pressure for the battery.
In the present embodiment, a control device may also be incorporated to control the drive source 18 while:
the up end of lower backup pad 14 is provided with pressure detection subassembly 21, pressure detection subassembly 21 includes the pressure post, the fixed surface of pressure post is connected with the pressure measurement board, the fixed surface of guide bar 19 is connected with the fixed plate, the surface of pressure measurement board is provided with pressure sensor, works as when lower electrode pressure head 10 cooperation battery pack contacts with upper electrode pressure head 3, pressure sensor on pressure measurement board surface with the fixed plate contact.
The external pressure detection assembly 21 is used for more conveniently helping the experimenter to determine the corresponding pressure, the model of the pressure sensor is not limited, the pressure sensor can be used in a vacuum environment, even if the pressure sensor cannot be used in a vacuum environment, the pressure sensor can be removed after the corresponding pressure is determined in an inert gas environment, and the pressure sensor can be independently used in the driving structure in the embodiment 1.
Example 3
As shown in fig. 4 to 6, the device can be applied to solid batteries and other types of batteries based on the above embodiments 1 and 2; specifically, the upper electrode pressing head 3 comprises a pressing head assembly 22, wherein the pressing head assembly 22 comprises a beryllium sheet and a protection sheet, and the protection sheet is arranged below the beryllium sheet; the lower electrode pressing head 10 comprises a calibration tube 24 capable of moving up and down, the upper end face of the calibration tube 24 is flush with the upper end face of the lower electrode pressing head 10, the lower movement limit distance of the calibration tube 24 is the thickness distance of the protection sheet, and the side wall of the lower electrode pressing head 10 is provided with an injection molding tube assembly 31.
The protective sheet can be in the form of an aluminum film and a polyimide film, or can be made of other high-molecular polymer materials, and the material with certain electric conductivity is optimally selected; further, an inner groove 28 is formed in the lower electrode pressing head 10, the inner groove 28 is divided into an upper section and a lower section, the diameter of the upper section groove is larger than that of the lower section groove, the calibration tube 24 slides in the upper section groove, an inner sliding groove 25 is formed in the lower electrode pressing head 10 above the lower section groove, an inner sliding wedge 26 is arranged in the inner sliding groove 25, one end of the inner sliding wedge 26 is connected with a pull rope assembly 30, a wedge surface is also arranged at the edge position of the lower end face of the calibration tube 24, one end of the pull rope assembly 30 penetrates through the outer part of the lower electrode pressing head 10, and the end is fixedly connected with a fixing block 29; the calibration tube 24 is a hollow annular tube, a rod inserting piece 23 is arranged in the middle of the calibration tube 24, the lower end of the calibration tube 24 is connected with an internal pulling spring 27, and the internal pulling spring 27 is arranged in the lower section of the internal groove 28.
In practical use, when the corresponding loss corrosion occurs on the protective sheet, the lower electrode pressing head 10 is moved to a position contacting with the upper electrode pressing head 3, so that the fixed block 29 and the whole lower electrode pressing head 10 are correspondingly displaced, the inner sliding wedge 26 is pulled to move in the inner sliding groove 25, the calibration tube 24 is pulled to move downwards by the inner pulling spring 27, the calibration tube 24 moves downwards, in the process, the whole lower electrode pressing head 10 moves upwards to a limit position, the pressing head assembly 22 of the upper electrode pressing head 3 is matched, the thickness space of the corresponding protective sheet is reserved, and an experimenter can inject injection molding liquid of the protective sheet into the space through the injection molding tube assembly 31, so that the thickness of the protective sheet is complemented, and the problem of inaccurate pressure caused by the corrosion loss of the protective sheet is solved.
It should be further added that the fixed block 29 may be fixedly connected to the inner wall of the insulating pressing mold 8, or may be slidably connected to the lower electrode pressing head 10, and if a sliding connection mode is adopted, a corresponding blocking member is disposed in the insulating pressing mold 8, and when the whole lower electrode pressing head 10 moves upwards, the fixed block 29 will be blocked by the blocking member, so that the relative displacement between the fixed block 29 and the lower electrode pressing head 10 occurs; the pull rope assembly 30 comprises a spring element arranged in the inner chute 25 and a pull rope element connecting the fixed block 29 and the inner slide wedge 26; the syringe assembly 31 may be disposed in the calibration tube 24 or the insert rod member 23, and the optimum outlet is the upper end surface thereof when disposed in the calibration tube 24.
Further, the surface of the lower electrode pressing head 10 is also fixedly connected with an upper dynamic sealing assembly 32 and a lower dynamic sealing assembly 33.
When this embodiment is used in combination with embodiment 2 described above, it is necessary to provide the fixing plate in a rotatable manner to prevent it from obstructing the upward movement of the lower electrode indenter 10.
Example 4
A method for testing the absorption spectrum of cell transfer and in-situ synchrotron radiation comprises,
installing the device described in each embodiment above in an inert gas environment;
extruding the cell assembly at a set stack pressure;
closing the taper hole on the surface of the upper electrode pressure head 3, and transferring the device to a sample frame of the experimental station cavity;
vacuumizing the experimental station cavity, and simultaneously opening a taper hole on the surface of the closed upper electrode pressure head 3;
the battery is in a working state through the electrode screw, the synchronous radiation light irradiates the battery through the taper hole on the surface of the upper electrode pressure head 3, and the detector of the experimental station collects fluorescent/electronic signals emitted after the synchronous radiation light excites the battery material.
The basic implementation method of not exposing the air transfer battery and realizing the in-situ test can be briefly described as follows, the solid-state Li-S battery applies required pressure values to the battery by using torque wrenches (the pressures corresponding to different torques are calibrated through pressure sensors) to four pressure-applying screws of the device in a glove box filled with inert gas, and then a polyimide adhesive tape is adopted to seal a test taper hole of the device; then, the device is taken out of the glove and transferred to a synchronous radiation absorption spectrum experiment station of a light source, and the synchronous radiation absorption spectrum experiment station is placed on a sample frame of a vacuum cavity of the experiment station; electrode columns on the flange plate of the vacuum cavity are connected to two electrode screws of the device through wires so as to realize the connection of the battery device and a charge and discharge power supply outside the vacuum cavity; after the steps are finished, vacuumizing the cavity of the experimental station, and tearing off the polyimide adhesive tape covering the taper hole of the in-situ testing device by using a mechanical handle in the vacuumizing process.
Further, before the apparatus described in each of the above embodiments is installed in an inert gas atmosphere;
and measuring the thickness of the protective sheet in the pressure head assembly 22, and when the thickness of the protective sheet is lower than a preset threshold value, adding the protective sheet with corresponding thickness to be attached to the surface of the protective sheet of the pressure head assembly 22.
In the foregoing embodiment 3, a supplementary injection molding method is provided, but in practical use, an experimenter may further determine the corresponding thickness of the pressure head assembly 22 by increasing the number of layers of the protective sheet, specifically, may use a double-layer aluminum film form, and when the protective sheet is damaged, may reapply the corresponding film body to maintain the corresponding thickness of the pressure head assembly 22, so as to prevent the occurrence of inaccurate battery compression caused by thickness variation of the pressure head assembly 22.
The embodiment has been described above with reference to the embodiment, but the embodiment is not limited to the above-described specific implementation, which is only illustrative and not restrictive, and many forms can be made by those of ordinary skill in the art, given the benefit of this disclosure, are within the scope of this embodiment.

Claims (6)

1. The device is characterized by comprising a fixed sample holder plug (6), wherein the surface of the fixed sample holder plug (6) is connected with an upper electrode press head (3), a taper hole is formed in the surface of the upper electrode press head (3), the lower end face of the upper electrode press head (3) is connected with an insulating press sheet die (8), a battery component to be tested is placed in the insulating press sheet die (8), a lower electrode press head (10) capable of being inserted from below is further arranged in the insulating press sheet die (8), the upper electrode press head (3) is connected with an upper working electrode screw (4), the lower electrode press head (10) is connected with a lower working electrode screw (11), the lower electrode press head (10) is also connected with a lower support plate (14), the lower support plate (14) is connected with a driving structure capable of moving up and down, and the upper electrode press head (3) and the lower electrode press head (10) squeeze the electrode of the battery component with set stack pressure based on the position of the lower support plate (14); the fixed sample holder plug (6) comprises a flat plate with screw holes formed in the surface, the screw holes on the surface of the flat plate are connected with fastening screws (1), a T-shaped insulating cylinder (2) is sleeved on the surface of the fastening screws (1), the fastening screws (1) are matched with the T-shaped insulating cylinder (2) to connect the upper electrode pressing head (3) and the flat plate, and an upper insulating plate (5) is further arranged between the upper electrode pressing head (3) and the flat plate; an upper sealing ring (7) and a lower sealing ring (9) are respectively arranged at the upper end face and the lower end of the insulating tabletting mold (8); a lower insulating plate (12) is arranged between the lower electrode pressing head (10) and the lower supporting plate (14); the driving structure comprises a rod piece, the upper end of the rod piece is connected with the upper electrode pressure head (3), the lower part of the rod piece is sleeved with a lower supporting plate (14), and the height of the lower supporting plate (14) is adjusted based on the set stacking pressure; the upper electrode pressure head (3) comprises a pressure head assembly (22), wherein the pressure head assembly (22) comprises a beryllium sheet and a protection sheet, and the protection sheet is arranged below the beryllium sheet; the lower electrode pressure head (10) comprises a calibration tube (24) capable of moving up and down, the upper end face of the calibration tube (24) is flush with the upper end face of the lower electrode pressure head (10), the lower limit distance of the calibration tube (24) is the thickness distance of a protection sheet, and an injection molding tube assembly (31) is arranged on the side wall of the lower electrode pressure head (10); an inner groove (28) is formed in the lower electrode pressing head (10), the inner groove (28) is divided into an upper section and a lower section, the diameter of the upper section groove body is larger than that of the lower section groove body, the calibration pipe (24) slides in the upper section groove body, an inner sliding groove (25) is formed in the lower electrode pressing head (10) above the lower section groove body, an inner sliding wedge (26) is arranged in the inner sliding groove (25), one end of the inner sliding wedge (26) is connected with a pull rope assembly (30), a wedge surface is also arranged at the edge position of the lower end surface of the calibration pipe (24), one end of the pull rope assembly (30) penetrates through the outer part of the lower electrode pressing head (10), and the end is fixedly connected with a fixing block (29); the calibration tube (24) is a hollow annular tube, the middle part of the calibration tube (24) is provided with an insertion rod piece (23), the lower end of the calibration tube (24) is connected with an inward-pulling spring (27), and the inward-pulling spring (27) is arranged in the lower section of the inner groove (28); when the corresponding loss corrosion occurs to the protective sheet, the lower electrode pressing head (10) is moved to a position contacted with the upper electrode pressing head (3), so that the fixed block (29) and the whole lower electrode pressing head (10) are correspondingly displaced, the sliding wedge block (26) is pulled to move in the sliding groove (25), the calibration tube (24) is pulled to move downwards by the inward-pulling spring (27), the calibration tube (24) moves downwards, and in the process, the whole lower electrode pressing head (10) moves upwards to a limit position and is matched with the pressing head assembly (22) of the upper electrode pressing head (3), so that the thickness space of the corresponding protective sheet is reserved; injection liquid of the protective sheet is injected into the space through an injection pipe assembly (31), so that the thickness of the protective sheet is complemented.
2. The device for testing the battery transfer and in-situ synchrotron radiation absorption spectrum according to claim 1, wherein the rod is a pressing fixed screw (13), the pressing fixed screw (13) penetrates through the lower supporting plate (14), a fastening nut (15) is connected to the penetrating end, and the position of the fastening nut (15) is adjusted based on a torque wrench to adjust the stack pressure.
3. The battery transfer and in-situ synchrotron radiation absorption spectrum testing device according to claim 1, wherein the rod is a guide rod (19), the lower support plate (14) is sleeved on the surface of the guide rod (19) to move up and down, a driving source (18) is fixedly connected to the lower end face of the lower support plate (14), a moving sleeve (20) is connected to the driving end of the driving source (18), a moving screw (16) is connected to the moving sleeve (20) in a threaded manner, a connecting plate (17) is fixedly connected to the moving screw (16), the moving screw (16) is fixedly connected with the guide rod (19) through the connecting plate (17), the driving source (18) drives the moving sleeve (20) to rotate, and the moving sleeve (20) moves up and down on the surface of the moving screw (16).
4. A battery transfer and in-situ synchrotron radiation absorption spectrum testing device according to claim 3, wherein the upper end surface of the lower support plate (14) is provided with a pressure detection assembly (21), the pressure detection assembly (21) comprises a pressure column, the surface of the pressure column is fixedly connected with a pressure measuring plate, the surface of the guide rod (19) is fixedly connected with a fixing plate, the surface of the pressure measuring plate is provided with a pressure sensor, and when the lower electrode pressure head (10) is matched with the battery assembly to contact with the upper electrode pressure head (3), the pressure sensor on the surface of the pressure measuring plate contacts with the fixing plate.
5. A method for testing the absorption spectrum of cell transfer and in-situ synchrotron radiation is characterized in that the method comprises the following steps,
installing the apparatus of claim 1 in an inert gas environment;
extruding the cell assembly at a set stack pressure;
closing the taper hole on the surface of the upper electrode pressure head (3), and transferring the device to a sample frame of the experimental station cavity;
vacuumizing the experimental station cavity, and simultaneously opening a taper hole on the surface of a closed upper electrode pressure head (3);
the battery is in a working state through the electrode screw, the synchronous radiation light irradiates the battery through a taper hole on the surface of the upper electrode pressure head (3), and a detector of the experimental station collects fluorescent/electronic signals emitted after the synchronous radiation light excites the battery material.
6. A method of testing the absorption spectrum of synchrotron radiation in-situ and cell transfer as claimed in claim 5, wherein, before installing the apparatus as claimed in claim 1 in an inert atmosphere:
and measuring the thickness of the protective sheet in the pressure head assembly (22), and when the thickness of the protective sheet is lower than a preset threshold value, adding the protective sheet with corresponding thickness to be attached to the surface of the protective sheet of the pressure head assembly (22).
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