Test mold of air-sensitive solid-state battery, interface micro-analysis and controllable pressure system and method

Abstract

The invention provides a test mold for an air-sensitive solid-state battery, and an interface micro-analysis and controllable pressure system and method, and the test mold comprises a support which comprises a top plate and a plurality of adjusting rods; the first ejector rod and the second ejector rod are oppositely arranged, and the adjusting rod sequentially penetrates through and is connected with the ejector plate, the first ejector rod and the second ejector rod; the sealing assembly comprises at least two sleeves, two openings are formed after the two sleeves are combined, the first ejector rod and the second ejector rod abut against the opening positions of the two opposite sides of the sealing assembly respectively to form a sealing cavity, the sealing cavity is used for containing the solid-state battery, and the multiple adjusting rods are used for driving the second ejector rod to move relative to the first ejector rod; and the pressure applied to the solid-state battery by the second ejector rod is adjusted. According to the application, the pressure applied to the solid-state battery can be accurately controlled, different pressure conditions are further simulated, and the air-sensitive solid-state electrolyte material is allowed to be subjected to atmospheric transfer and in-situ testing in an air-isolated environment.

Description

Technical Field

[0001] The present application relates to the technical field of solid-state battery testing, and in particular to a test mold, interface micro-analysis and controllable pressure system and method for air-sensitive solid-state batteries. Background Art

[0002] With the development of electric vehicles, solid-state batteries have become the preferred technology for the next generation of energy storage devices due to their higher energy density and power density, higher safety and electrochemical stability. The interface stability between electrode materials and solid electrolytes is a key factor affecting the performance and life of solid-state batteries.

[0003] At present, solid electrolyte materials such as sulfides and halides have attracted much attention due to their excellent ionic conductivity. These materials can provide high ionic conductivity at room temperature, which makes them have potential application advantages in solid-state batteries. However, these materials are extremely sensitive to air and easily react with moisture and oxygen, resulting in performance degradation and chemical instability. This sensitivity poses a challenge to the study of the interface stability between electrode materials and solid electrolytes.

[0004] Existing research equipment for the interface stability between electrode materials and solid electrolytes has a single function, making it difficult to achieve effective atmospheric transfer, electrochemical testing, and interface stability research on solid-state batteries using air-sensitive solid electrolytes. Summary of the invention In view of the above, it is necessary to provide a test mold, interface microanalysis and controllable pressure system and method for air-sensitive solid-state batteries to solve the technical problem that the existing research equipment for the interface stability between electrode materials and solid electrolytes has a single function and is difficult to achieve effective atmospheric transfer, electrochemical testing, and interface stability research on solid-state batteries using air-sensitive solid electrolytes.

[0005] The present application embodiment provides a test mold for an air-sensitive solid-state battery, the test mold comprising: A bracket, including a top plate and a plurality of adjustment rods; a first push rod and a second push rod, wherein the first push rod and the second push rod are arranged opposite to each other, and the adjusting rod passes through and connects the top plate, the first push rod and the second push rod in sequence; The sealing assembly includes at least two sleeves, which are combined to form two openings. The first push rod and the second push rod are respectively pressed against the opening positions on opposite sides of the sealing assembly to form a sealed cavity, which is used to accommodate the solid-state battery. The multiple adjustment rods are used to drive the second push rod to move relative to the first push rod to adjust the pressure applied by the second push rod to the solid-state battery.

[0006] The test mold of the air-sensitive solid-state battery of the present application can accurately control the pressure applied by the second push rod to the solid-state battery through the design of multiple adjustment rods, so that researchers can adjust the pressure according to different test requirements, and then simulate different pressure conditions to obtain more accurate test data. The sealed cavity formed by the sealing component can effectively isolate air and moisture, allowing air-sensitive solid electrolyte materials to be atmospherically transferred and in-situ tested in an air-isolated environment, which is crucial for observing the interface stability of solid-state batteries under actual working conditions. The combined design of the sealing component facilitates researchers to install and disassemble solid-state batteries. The design of the adjustment rod running through and connecting the top plate, the first push rod and the second push rod makes the operation of the test mold easier and improves the test efficiency. Since different pressure conditions can be simulated and the influence of the external environment on the solid-state battery can be isolated, the test mold provided by the present application can provide more accurate and reliable data for testing, which is helpful for in-depth analysis of the performance of the solid-state battery.

[0007] In some embodiments of the present application, the test mold further includes: A pressure sensor is disposed between the top plate and the first top rod, and is used to monitor the pressure borne by the solid-state battery in real time; A temperature sensor is disposed between the top plate and the first top rod, and the temperature sensor is used to monitor the temperature of the solid-state battery in real time.

[0008] In some embodiments of the present application, the test mold further includes: A manual pressure rod passes through and connects the top plate and the first push rod in sequence, and the manual pressure rod is used to drive the first push rod to move relative to the second push rod to adjust the pressure applied by the first push rod to the solid-state battery.

[0009] In some embodiments of the present application, the first push rod includes a first clamping plate and a first push block, the first clamping plate is integrally connected to the first push block and forms a "T" shape; the second push rod includes a second clamping plate and a second push block, the second clamping plate is integrally connected to the second push block and forms a "T" shape; the first push block and the second push block are arranged opposite to each other.

[0010] In some embodiments of the present application, a first groove is provided at one end of the first top block facing the second clamping plate, and a first sealing ring is provided in the first groove; a second groove is provided at one end of the second top block facing the first clamping plate, and a second sealing ring is provided in the second groove.

[0011] The embodiment of the present application also provides an interface microscopic analysis and controllable pressure system for a solid-state battery, the system comprising an electrochemical device, an observation device, and a test mold for an air-sensitive solid-state battery as described in any one of the above embodiments; The electrochemical device is electrically connected to the positive electrode material and the negative electrode material of the solid-state battery, and the electrochemical device is used to apply an electrochemical signal to the solid-state battery to perform an electrochemical test on the solid-state battery; The observation device is located above the solid-state battery, and is used to observe in real time the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery.

[0012] The interface micro-analysis and controllable pressure system of the air-sensitive solid-state battery of the present application applies electrochemical signals to the solid-state battery through an electrochemical device to perform electrochemical testing, which allows researchers to evaluate the performance of the solid-state battery under different chemical conditions. Real-time observation of the interface changes between the positive electrode material and the solid electrolyte by an observation device is crucial to understanding the interface stability and interface reaction of the solid-state battery during operation, and helps to reveal the mechanism of performance degradation and failure of the solid-state battery. By simulating different pressure conditions through the test mold, and is able to isolate the influence of the external environment on the solid-state battery, the real state of the solid-state battery is maintained and accurate testing is performed, which is especially important for air-sensitive solid electrolyte materials such as sulfides and halides, because they may exhibit different electrochemical properties under different pressure conditions. The interface micro-analysis and controllable pressure system of the air-sensitive solid-state battery of the present application realizes in-situ electrochemical testing of solid-state batteries under different conditions, transfer of sensitive solid-state batteries in the atmosphere, and atomic force microscopy observation, which can track and record the evolution of the interface structure of electrodes and electrolytes in the solid-state battery during charging and discharging online and visualize the study. This application can also perform tests without destroying the solid-state battery, reducing the complexity of sample preparation and avoiding possible safety risks during testing. It helps researchers better understand the working principles of solid-state batteries, thereby guiding the development of air-sensitive solid-state electrolyte materials and the optimization of solid-state battery design, and promoting the development of solid-state battery technology.

[0013] In some embodiments of the present application, the observation device includes: Atomic force microscope-infrared spectroscopy equipment, used to obtain images and infrared absorption spectrum data of the interface between the positive electrode material and the solid electrolyte in real time; A controller is communicatively connected to the atomic force microscope-infrared spectroscopy device, and the controller is used to determine interface change data between the positive electrode material and the solid electrolyte based on the image and the infrared absorption spectrum data.

[0014] In some embodiments of the present application, the system further comprises: The thermal evaporation device is used to evaporate a metal film at the interface between the positive electrode material and the solid electrolyte, which serves as an infrared transparent window of the atomic force microscope-infrared spectrometer.

[0015] The present application also provides an interface microscopic analysis and controllable pressure method for an air-sensitive solid-state battery, using the interface microscopic analysis and controllable pressure system for an air-sensitive solid-state battery as described in any of the above embodiments, the method comprising: Placing the solid-state battery in the sealed cavity of the sealing assembly, and adjusting the interface between the positive electrode material and the solid electrolyte of the solid-state battery to face the opening close to the first push rod; The pressure applied by the first push rod to the solid-state battery is adjusted by a manual pressure rod, and the pressure applied by the second push rod to the solid-state battery is adjusted by an adjustment rod, so as to adjust the pressure on the solid-state battery to a preset pressure value; The pressure of the solid-state battery is monitored in real time by a pressure sensor, and the temperature of the solid-state battery is monitored in real time by a temperature sensor; Connecting the positive electrode material and the negative electrode material of the solid-state battery to an electrochemical device respectively, and performing an electrochemical test on the solid-state battery through the electrochemical device; The interface changes between the positive electrode material and the solid electrolyte of the solid-state battery are observed in real time by an observation device.

[0016] The interface microscopic analysis and controllable pressure method of the air-sensitive solid-state battery of the present application applies electrochemical signals to the solid-state battery through an electrochemical device to perform electrochemical testing, which allows researchers to evaluate the performance of the solid-state battery under different chemical conditions. Real-time observation of the interface changes between the positive electrode material and the solid electrolyte by an observation device is crucial to understanding the interface stability and interface reaction of the solid-state battery during operation, and helps to reveal the mechanism of performance degradation and failure of the solid-state battery. By simulating different pressure conditions through the test mold, and is able to isolate the influence of the external environment on the solid-state battery, the real state of the solid-state battery is maintained and accurate testing is performed, which is especially important for air-sensitive solid electrolyte materials such as sulfides and halides, because they may exhibit different electrochemical properties under different pressure conditions. The interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery of the present application realizes in-situ electrochemical testing of solid-state batteries under different conditions, transfer of sensitive solid-state batteries in the atmosphere, and atomic force microscopy observation, which can track and record the evolution of the interface structure of electrodes and electrolytes in the solid-state battery during charging and discharging online and visualize the study. This application can also perform tests without destroying the solid-state battery, reducing the complexity of sample preparation and avoiding possible safety risks during testing. It helps researchers better understand the working principles of solid-state batteries, thereby guiding the development of air-sensitive solid-state electrolyte materials and the optimization of solid-state battery design, and promoting the development of solid-state battery technology.

[0017] In some embodiments of the present application, the real-time observation of the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery by an observation device includes: The solid-state battery in the test mold is transferred to a thermal evaporation device, and a metal film is evaporated at the interface between the positive electrode material and the solid electrolyte by the thermal evaporation device; Scanning the interface between the positive electrode material and the solid electrolyte for generating the metal film at a micrometer scale by using an atomic force microscope-infrared spectroscopy device to collect images and infrared absorption spectrum data; Analyzing the image and the infrared absorption spectrum data by a controller to determine interface change data between the positive electrode material and the solid electrolyte, wherein the interface change data includes chemical decomposition products of the solid-state battery during the charge and discharge process and the distribution of the chemical decomposition products at the interface between the positive electrode material and the solid electrolyte; The influence of the chemical decomposition product on the stability of the interface between the positive electrode material and the solid electrolyte of the solid-state battery is evaluated based on the interface change data. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0019] Figure 1 It is a structural schematic diagram of a test mold for an air-sensitive solid-state battery provided in one embodiment of the present application.

[0020] Figure 2 It is a structural schematic diagram of the interface micro-analysis and controllable pressure system of an air-sensitive solid-state battery provided in another embodiment of the present application.

[0021] Figure 3 This is a schematic diagram of the steps of the interface microanalysis and controllable pressure method of air-sensitive solid-state batteries provided in another embodiment of the present application.

[0022] Figure 4 It is a structural schematic diagram of an interface microscopic analysis and controllable pressure method for an air-sensitive solid-state battery provided in yet another embodiment of the present application.

[0023] Main component symbols Test mold 100 Brackets 101 Top Plate 1011 Adjustment rod 1012 The first push rod 102 The first clamping plate 1021 The first top block 1022 First sealing ring 1023 Second ejector 103 The second clamping plate 1031 The second top block 1032 Manual pressure lever 104 Insulation sleeve 105 Connecting screw 106 Seal assembly 107 Sleeve 1071 Fixing 1072 Electrochemical device 200 Electrochemical workstation 201 Electronic Circuit 202 Observation device 300 Atomic Force Microscope-Infrared Spectroscopy Equipment 301 Controller 302 Integrated circuit device 400 Rectifier circuit module 401 Signal conversion module 402 Communication module 403 Cloud Server 500 User terminal 600 The following specific implementation methods will further illustrate the present application in conjunction with the above-mentioned drawings. DETAILED DESCRIPTION

[0024] The embodiments of the present application are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present application, and cannot be understood as limiting the present application.

[0025] In the embodiments of the present application, it should be noted that, unless otherwise clearly specified and limited, words such as "exemplary" or "for example" are used to indicate examples, illustrations or descriptions. Any embodiment or design described as "exemplary" or "for example" in the embodiments of the present application should not be interpreted as being more preferred or more advantageous than other embodiments or designs. Specifically, the use of words such as "exemplary" or "for example" is intended to present related concepts in a concrete way. In the absence of conflict, the following embodiments and features in the embodiments may be combined with each other.

[0026] In the description of this application, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, an electrical connection, or mutual communication; it can be a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to the specific situation.

[0027] In the description of this application, it should be noted that the terms "first", "second", etc. (if any) in the description and claims of this application are used to distinguish similar objects, rather than to describe a specific order or sequence. In the description of this application, "plurality" means two or more, unless otherwise clearly and specifically defined.

[0028] In order to more clearly understand the above-mentioned purposes, features and advantages of the present application, the present application is described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.

[0029] See also Figure 1, which is a structural schematic diagram of a test mold 100 for an air-sensitive solid-state battery provided in one embodiment of the present application.

[0030] Specifically, the test mold 100 includes a bracket 101, a first push rod 102, a second push rod 103, and a sealing assembly 107. The bracket 101 includes a top plate 1011 and a plurality of adjustment rods 1012. The first push rod 102 and the second push rod 103 are arranged opposite to each other. The adjustment rod 1012 passes through and connects the top plate 1011, the first push rod 102, and the second push rod 103 in sequence. The sealing assembly 107 includes two sleeves 1071, which are combined to form two openings (not shown in the figure). The first push rod 102 and the second push rod 103 are respectively pressed against the opening positions on the opposite sides of the sealing assembly 107 to form a sealed cavity (not shown in the figure). The sealed cavity is used to accommodate the solid-state battery. The plurality of adjustment rods 1012 are used to drive the second push rod 103 to move relative to the first push rod 102 to adjust the pressure applied by the second push rod 103 to the solid-state battery.

[0031] In the above embodiment, through the design of multiple adjustment rods 1012, the pressure applied by the second push rod 103 to the solid-state battery can be accurately controlled, so that researchers can adjust the pressure according to different test requirements, and then simulate different pressure conditions to obtain more accurate test data. The sealed cavity formed by the sealing component 107 can effectively isolate air and moisture, allowing air-sensitive solid electrolyte materials to perform atmospheric transfer and in-situ testing in an environment isolated from air, which is very important for observing the interface stability of solid-state batteries under actual working conditions. The combined design of the sealing component 107 is convenient for researchers to install and disassemble solid-state batteries. The design of the adjustment rod 1012 running through and connecting the top plate 1011, the first push rod 102 and the second push rod 103 makes the operation of the test mold 100 easier and improves the test efficiency. Because different pressure conditions can be simulated and the influence of the external environment on the solid-state battery can be isolated, therefore, testing using the test mold 100 provided by the present application can provide more accurate and reliable data, which is helpful for in-depth analysis of the performance of the solid-state battery.

[0032] In some embodiments of the present application, the sealing assembly 107 further includes a plurality of fixing members 1072, and the plurality of fixing members 1072 are used to seal and fix the two sleeves 1071, which facilitates disassembly and installation and is easy to operate.

[0033] In some embodiments of the present application, the fixing member 1072 may be a screw, which is screwed and fixed to form a stable sealing structure to ensure the safe transfer of the solid-state battery in different atmospheric environments.

[0034] In some embodiments of the present application, the two sleeves 1071 are in a "7" shape and are made of high-performance polymer materials, have good corrosion resistance and wear resistance, and can still maintain stable electrical properties under high temperature, high frequency and high pressure environments.

[0035] In some embodiments of the present application, the adjustment rod 1012, the first top rod 102, and the second top rod 103 are made of stainless steel, which can ensure the stability of the solid-state battery interface and the reliability of the test.

[0036] In some embodiments of the present application, an insulating sleeve 105 is provided at the connection between the adjustment rod 1012 and the first top rod 102 to prevent the positive and negative electrodes of the solid-state battery from being short-circuited, thereby ensuring safe operation of the solid-state battery.

[0037] In some embodiments of the present application, the test mold 100 further includes two connecting screws 106 , which are respectively disposed on the first push rod 102 and the second push rod 103 . The two connecting screws 106 are used to connect the electrochemical device 200 , thereby ensuring the smooth progress of the electrochemical reaction.

[0038] In some embodiments of the present application, the test mold 100 also includes a pressure sensor (not shown) and a temperature sensor (not shown). The pressure sensor is disposed between the top plate 1011 and the first top rod 102, and the pressure sensor is used to monitor the pressure borne by the solid-state battery in real time. The temperature sensor is disposed between the top plate 1011 and the first top rod 102, and the temperature sensor is used to monitor the temperature of the solid-state battery in real time. By arranging the pressure sensor and the temperature sensor at appropriate positions of the test mold 100, the pressure changes and temperature changes of the solid-state battery during the test process can be recorded in real time, thereby realizing real-time observation of the changes in interface pressure and interface temperature during the test process of the solid-state battery.

[0039] In some embodiments of the present application, the test mold 100 further includes a manual pressure rod 104. The manual pressure rod 104 sequentially penetrates and connects the top plate 1011 and the first top rod 102. The manual pressure rod 104 is used to drive the first top rod 102 to move relative to the second top rod 103 to adjust the pressure applied by the first top rod 102 to the solid-state battery, thereby achieving different pressure conditions.

[0040] In some embodiments of the present application, the top plate 1011 is in an "I" shape, the manual pressure rod 104 is installed in the middle position of the top plate 1011, and the pressure sensor and the temperature sensor are arranged between the manual pressure rod 104 and the first top rod 102, ensuring that the pressure sensor and the temperature sensor can accurately measure the pressure on the solid-state battery.

[0041] In some embodiments of the present application, the first push rod 102 includes a first clamping plate 1021 and a first top block 1022, and the first clamping plate 1021 is integrally connected with the first top block 1022 to form a "T" shape. The second push rod 103 includes a second clamping plate 1031 and a second top block 1032, and the second clamping plate 1031 is integrally connected with the second top block 1032 to form a "T" shape. The first top block 1022 and the second top block 1032 are arranged opposite to each other. The "T"-shaped design ensures that uniform pressure is provided to the solid-state battery during the pressure application process.

[0042] In some embodiments of the present application, both ends of the adjustment rod 1012 are threaded structures, and both the top plate 1011 and the second clamping plate 1031 are provided with threaded holes, and the adjustment rod 1012 is connected to the top plate 1011 and the second clamping plate 1031 through the cooperation of the thread and the threaded hole. The middle part of the adjustment rod 1012 is movably connected to the first clamping plate 1021, so that the manual pressure rod 104 can push the first clamping plate 1021 to move relative to the second clamping plate 1031.

[0043] In some embodiments of the present application, a first groove (not shown) is provided at one end of the first top block 1022 facing the second clamping plate 1031, and a first sealing ring 1023 is provided in the first groove. A second groove (not shown) is provided at one end of the second top block 1032 facing the first clamping plate 1021, and a second sealing ring (not shown) is provided in the second groove, which enhances the sealing performance of the sealing assembly 107 during the pressure application process.

[0044] In some embodiments of the present application, the first sealing ring 1023 and the second sealing ring are made of chemically resistant materials to prevent chemical reactions between the solid-state battery and the test mold 100 .

[0045] See also Figure 2 , which is a structural schematic diagram of the interface micro-analysis and controllable pressure system of the air-sensitive solid-state battery provided in one embodiment of the present application.

[0046] Specifically, the interface microanalysis and controllable pressure system of air-sensitive solid-state batteries include Figure 1 Shown are a test mold 100 , an electrochemical device 200 , and an observation device 300 .

[0047] The electrochemical device 200 is electrically connected to the positive electrode material and the negative electrode material of the solid-state battery, and is used to apply an electrochemical signal to the solid-state battery to perform an electrochemical test on the solid-state battery. The observation device 300 is located above the solid-state battery, and is used to observe the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery in real time.

[0048] In some embodiments of the present application, the observation device 300 includes an atomic force microscope-infrared spectrometer 301 and a controller 302. The atomic force microscope-infrared spectrometer 301 is used to obtain images and infrared absorption spectrum data of the interface between the positive electrode material and the solid electrolyte in real time. The controller 302 is communicatively connected to the atomic force microscope-infrared spectrometer 301, and the controller 302 is used to determine the interface change data between the positive electrode material and the solid electrolyte based on the image and infrared absorption spectrum data.

[0049] In some embodiments of the present application, the image collected by the atomic force microscope-infrared spectrometer 301 is an image generated by an atomic force microscope (Atomic Force Microscope, AFM).

[0050] In some embodiments of the present application, the interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery further includes a thermal evaporation device (not shown). The thermal evaporation device is used to evaporate a layer of metal film at the interface between the positive electrode material and the solid electrolyte, which serves as an infrared transparent window of the atomic force microscope-infrared spectrometer 301 to ensure accurate acquisition of the infrared spectrum during the observation process. At the same time, the metal film also protects the air-sensitive solid electrolyte from air erosion.

[0051] In some embodiments of the present application, the metal film is formed by heating the film material in a vacuum environment using resistance, electron beam, laser heating, etc., so that the film material evaporates or sublimates, and the gaseous particles are deposited on the surface of the positive electrode material of the solid-state battery to form a thin film.

[0052] In some embodiments of the present application, the interface micro-analysis and controllable pressure system of the air-sensitive solid-state battery further includes an integrated circuit device 400. The integrated circuit device 400 includes a rectifier circuit module 401, a signal conversion module 402, and a communication module 403. The rectifier circuit module 401 is used to rectify the pressure data and the temperature data. The signal conversion module 402 is used to convert the pressure data and the temperature data into digital signals, and transmit the digital signals to the cloud server 500 and / or the user terminal 600 through the communication module 403.

[0053] In some embodiments of the present application, the electrochemical device 200 includes an electrochemical workstation 201 and an electronic circuit 202. The electrochemical workstation 201 is used to perform an electrochemical test on the solid-state battery by applying an electrochemical signal to the solid-state battery. The electronic circuit 202 is used to monitor and record the electrochemical information of the solid-state battery during the electrochemical test.

[0054] In some embodiments of the present application, the design and manufacture of the test mold 100, the electrochemical device 200, the observation device 300, and the integrated circuit device 400 meet the standards of precision engineering, ensuring the stability and reliability of the interface microanalysis and controllable pressure system of the air-sensitive solid-state battery.

[0055] The interface micro-analysis and controllable pressure system of the air-sensitive solid-state battery of the present application applies electrochemical signals to the solid-state battery through the electrochemical device 200 to perform electrochemical testing, which allows researchers to evaluate the performance of the solid-state battery under different chemical conditions. Real-time observation of the interface changes between the positive electrode material and the solid electrolyte by the observation device 300 is crucial for understanding the interface stability and interface reaction of the solid-state battery during operation, and helps to reveal the mechanism of performance degradation and failure of the solid-state battery. The test mold 100 simulates different pressure conditions and can isolate the influence of the external environment on the solid-state battery, thereby maintaining the true state of the solid-state battery and performing accurate testing, which is particularly important for air-sensitive solid electrolyte materials such as sulfides and halides, because they may exhibit different electrochemical properties under different pressure conditions. The interface micro-analysis and controllable pressure system of the air-sensitive solid-state battery of the present application realizes in-situ electrochemical testing of solid-state batteries under different conditions, transfer of sensitive solid-state batteries in the atmosphere, and atomic force microscopy observation, which can track and record the evolution of the interface structure of electrodes and electrolytes in the process of charging and discharging of solid-state batteries online and visualize the research. This application can also perform tests without destroying the solid-state battery, reducing the complexity of sample preparation and avoiding possible safety risks during testing. It helps researchers better understand the working principles of solid-state batteries, thereby guiding the development of air-sensitive solid-state electrolyte materials and the optimization of solid-state battery design, and promoting the development of solid-state battery technology.

[0056] See also Figure 3 , which is a schematic diagram of the steps of the interface microanalysis and controllable pressure method of an air-sensitive solid-state battery provided in one embodiment of the present application.

[0057] The interface microscopic analysis and controllable pressure method of the air-sensitive solid-state battery provided in the embodiment of the present application is applied to the interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery in any of the above embodiments. Specifically, the interface microscopic analysis and controllable pressure method of the air-sensitive solid-state battery includes: Step S10 , placing the solid-state battery in the sealed cavity of the sealing assembly 107 , and adjusting the interface between the positive electrode material and the solid electrolyte of the solid-state battery to face the opening close to the first push rod 102 .

[0058] Step S11, adjusting the pressure applied by the first push rod 102 to the solid-state battery through the manual pressure rod 104, and adjusting the pressure applied by the second push rod 103 to the solid-state battery through the adjustment rod 1012, so as to adjust the pressure on the solid-state battery to a preset pressure value.

[0059] Step S12, monitoring the pressure on the solid-state battery in real time through a pressure sensor, and monitoring the temperature of the solid-state battery in real time through a temperature sensor.

[0060] Step S13, connecting the positive electrode material and the negative electrode material of the solid-state battery to the electrochemical device 200 respectively, and performing an electrochemical test on the solid-state battery through the electrochemical device 200.

[0061] Step S14, observing the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery in real time through the observation device 300.

[0062] The interface microscopic analysis and controllable pressure method of the air-sensitive solid-state battery of the present application applies electrochemical signals to the solid-state battery through the electrochemical device 200 to perform electrochemical testing, which allows researchers to evaluate the performance of the solid-state battery under different chemical conditions. Real-time observation of the interface changes between the positive electrode material and the solid electrolyte by the observation device 300 is crucial to understanding the interface stability and interface reaction of the solid-state battery during operation, and helps to reveal the mechanism of performance degradation and failure of the solid-state battery. The test mold 100 simulates different pressure conditions and can isolate the influence of the external environment on the solid-state battery, thereby maintaining the true state of the solid-state battery and performing accurate testing, which is particularly important for air-sensitive solid electrolyte materials such as sulfides and halides, because they may exhibit different electrochemical properties under different pressure conditions. The interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery of the present application realizes in-situ electrochemical testing of solid-state batteries under different conditions, transfer of sensitive solid-state batteries in the atmosphere, and atomic force microscopy observation, which can track and record the evolution of the interface structure of electrodes and electrolytes in the solid-state battery during charging and discharging online and visualize the study. This application can also perform tests without destroying the solid-state battery, reducing the complexity of sample preparation and avoiding possible safety risks during testing. It helps researchers better understand the working principles of solid-state batteries, thereby guiding the development of air-sensitive solid-state electrolyte materials and the optimization of solid-state battery design, and promoting the development of solid-state battery technology.

[0063] See also Figure 4 , which is a structural schematic diagram of the interface microanalysis and controllable pressure method of air-sensitive solid-state batteries provided in another embodiment of the present application.

[0064] In some embodiments of the present application, step S14, the specific steps of real-time observation of the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery by the observation device 300 include: Step S141, transferring the solid-state battery in the test mold 100 to a thermal evaporation device, and using the thermal evaporation device to evaporate a layer of metal film on the interface between the positive electrode material and the solid electrolyte.

[0065] Step S142, using the atomic force microscope-infrared spectrometer 301 to scan the interface between the positive electrode material and the solid electrolyte for generating the metal film at a micrometer scale, and collect images and infrared absorption spectrum data.

[0066] Step S143, analyzing the image and infrared absorption spectrum data through the controller 302 to determine the interface change data between the positive electrode material and the solid electrolyte, wherein the interface change data includes the chemical decomposition products of the solid-state battery during the charge and discharge process and the distribution of the chemical decomposition products at the interface between the positive electrode material and the solid electrolyte.

[0067] Step S144, evaluating the influence of the chemical decomposition products on the stability of the interface between the positive electrode material and the solid electrolyte of the solid-state battery according to the interface change data.

[0068] The interface micro-analysis and controllable pressure method of the air-sensitive solid-state battery of the present application realizes infrared spectral micro-area detection of the interface of the air-sensitive solid-state battery by evaporating a metal film as an infrared transparent window at the interface of the positive electrode material and the solid electrolyte of the solid-state battery. At the same time, the air-sensitive electrolyte material is protected from atmospheric pollution. The interface can be scanned at the nanoscale through atomic force microscopy-infrared spectroscopy technology. The collected infrared absorption spectrum data can be used to analyze the chemical composition of the interface. Detailed chemical analysis can be performed on the tiny area of ​​the interface, revealing the distribution of chemical decomposition products at the interface between the positive electrode material and the solid electrolyte, including the precise position and concentration of the chemical decomposition products, and then accurately analyzing the changes in the interface composition of the solid-state battery under different charging and discharging states, so that researchers can better understand the chemical stability of the positive electrode material and its evolution during the long-term use of the battery, providing an important scientific basis for the development of solid-state battery technology, thereby optimizing battery design, improving battery performance, and increasing the battery charging and discharging efficiency and cycle life, thereby promoting the development of solid-state battery technology.

[0069] Therefore, no matter from which point of view, the embodiments should be regarded as illustrative and non-restrictive, and the scope of the present application is limited by the appended claims rather than the above description, so it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims are included in the present application. Any attached figure mark in the claims should not be regarded as limiting the claims involved.

[0070] In addition, it is obvious that the word "comprising" does not exclude other submodules or steps, and the singular does not exclude the plural. The multiple submodules or devices stated in this application can also be implemented by one submodule or device through software or hardware.

[0071] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present application and are not intended to limit it. Although the present application has been described in detail with reference to the preferred embodiments, a person of ordinary skill in the art should understand that the technical solution of the present application may be modified or replaced by equivalents without departing from the spirit and scope of the technical solution of the present application.

Claims

1. A test mold for an air-sensitive solid-state battery, characterized in that: The test mold comprises: A bracket, including a top plate and a plurality of adjustment rods; a first push rod and a second push rod, wherein the first push rod and the second push rod are arranged opposite to each other, and the adjusting rod passes through and connects the top plate, the first push rod and the second push rod in sequence; The sealing assembly includes at least two sleeves, which are combined to form two openings. The first push rod and the second push rod are respectively pressed against the opening positions on opposite sides of the sealing assembly to form a sealed cavity, which is used to accommodate a solid-state battery. The multiple adjustment rods are used to drive the second push rod to move relative to the first push rod to adjust the pressure applied by the second push rod to the solid-state battery.

2. The test mold for air-sensitive solid-state batteries according to claim 1, characterized in that: The test mold also includes: A pressure sensor is disposed between the top plate and the first top rod, and is used to monitor the pressure borne by the solid-state battery in real time; A temperature sensor is disposed between the top plate and the first top rod, and the temperature sensor is used to monitor the temperature of the solid-state battery in real time.

3. The test mold for air-sensitive solid-state batteries according to claim 1, characterized in that: The test mold also includes: A manual pressure rod passes through and connects the top plate and the first push rod in sequence, and the manual pressure rod is used to drive the first push rod to move relative to the second push rod to adjust the pressure applied by the first push rod to the solid-state battery.

4. The test mold for air-sensitive solid-state batteries according to claim 1, characterized in that: The first push rod includes a first clamping plate and a first push block, the first clamping plate is integrally connected to the first push block and forms a "T" shape; the second push rod includes a second clamping plate and a second push block, the second clamping plate is integrally connected to the second push block and forms a "T" shape; the first push block and the second push block are arranged opposite to each other.

5. The test mold for air-sensitive solid-state batteries according to claim 4, characterized in that: A first groove is provided at one end of the first top block facing the second clamping plate, and a first sealing ring is provided in the first groove; a second groove is provided at one end of the second top block facing the first clamping plate, and a second sealing ring is provided in the second groove.

6. An interface microanalysis and controllable pressure system for air-sensitive solid-state batteries, characterized in that: The system comprises an electrochemical device, an observation device, and a test mold for an air-sensitive solid-state battery as described in any one of claims 1 to 5; The electrochemical device is electrically connected to the positive electrode material and the negative electrode material of the solid-state battery, and the electrochemical device is used to apply an electrochemical signal to the solid-state battery to perform an electrochemical test on the solid-state battery; The observation device is located above the solid-state battery, and is used to observe in real time the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery.

7. The interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery according to claim 6, characterized in that: The observation device comprises: Atomic force microscope-infrared spectroscopy equipment, used to obtain images and infrared absorption spectrum data of the interface between the positive electrode material and the solid electrolyte in real time; A controller is communicatively connected to the atomic force microscope-infrared spectroscopy device, and the controller is used to determine interface change data between the positive electrode material and the solid electrolyte based on the image and the infrared absorption spectrum data.

8. The interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery according to claim 7, characterized in that: The system further comprises: The thermal evaporation device is used to evaporate a metal film at the interface between the positive electrode material and the solid electrolyte, which serves as an infrared transparent window of the atomic force microscope-infrared spectrometer.

9. An interface microscopic analysis and controllable pressure method for air-sensitive solid-state batteries, characterized in that: Using the interface microscopic analysis and controllable pressure system of the air-sensitive solid-state battery as described in any one of claims 6 to 8, the method comprises: Placing the solid-state battery in the sealed cavity of the sealing assembly, and adjusting the interface between the positive electrode material and the solid electrolyte of the solid-state battery to face the opening close to the first push rod; The pressure applied by the first push rod to the solid-state battery is adjusted by a manual pressure rod, and the pressure applied by the second push rod to the solid-state battery is adjusted by an adjustment rod, so as to adjust the pressure on the solid-state battery to a preset pressure value; The pressure of the solid-state battery is monitored in real time by a pressure sensor, and the temperature of the solid-state battery is monitored in real time by a temperature sensor; Connecting the positive electrode material and the negative electrode material of the solid-state battery to an electrochemical device respectively, and performing an electrochemical test on the solid-state battery through the electrochemical device; The interface changes between the positive electrode material and the solid electrolyte of the solid-state battery are observed in real time by an observation device.

10. The interface microscopic analysis and controllable pressure method of the air-sensitive solid-state battery according to claim 9, characterized in that: The real-time observation of the interface changes between the positive electrode material and the solid electrolyte of the solid-state battery by an observation device comprises: The solid-state battery in the test mold is transferred to a thermal evaporation device, and a metal film is evaporated at the interface between the positive electrode material and the solid electrolyte by the thermal evaporation device; Scanning the interface between the positive electrode material and the solid electrolyte for generating the metal film at a micrometer scale by using an atomic force microscope-infrared spectroscopy device to collect images and infrared absorption spectrum data; Analyzing the image and the infrared absorption spectrum data by a controller to determine interface change data between the positive electrode material and the solid electrolyte, wherein the interface change data includes chemical decomposition products of the solid-state battery during the charge and discharge process and the distribution of the chemical decomposition products at the interface between the positive electrode material and the solid electrolyte; The influence of the chemical decomposition product on the stability of the interface between the positive electrode material and the solid electrolyte of the solid-state battery is evaluated based on the interface change data.

Images