Method for detecting conductivity of solid-state battery, solid-state battery and electric device

Abstract

The application relates to a solid-state battery compactness detection method, a solid-state battery and an electric equipment, a solid-state battery conductivity detection method, which comprises the following steps: filling a to-be-detected sample and metal powder in a filler tube, and arranging the to-be-detected sample with metal powder at both ends in a first direction, wherein the first direction is the axial direction of the filler tube; performing compaction treatment on the to-be-detected sample and the metal powder; electrically connecting the metal powder at both ends of the to-be-detected sample to a conductivity testing device respectively, and obtaining the conductivity of the to-be-detected sample through the conductivity testing device. A solid-state battery is prepared by using the above-mentioned solid-state battery conductivity testing method. An electric equipment comprises the above-mentioned solid-state battery. The above-mentioned solid-state battery compactness detection method, the solid-state battery and the electric equipment can make the material ion or electron transmission channel smooth, and reduce the probability that the conductivity test is inaccurate due to the excessively large gap between the to-be-detected sample and the metal powder.

Description

Technical Field

[0001] This application relates to the field of battery technology, and in particular to a method for detecting the conductivity of a solid-state battery, a solid-state battery, and an electrical device thereof. Background Technology

[0002] With the popularization and promotion of new energy vehicles, their charging and discharging performance and range have increasingly attracted people's attention and importance. As the power energy source for new energy vehicles, power batteries are widely used.

[0003] Solid-state batteries, as one of the future development trends of power batteries, have advantages such as high energy density and good safety. When testing the conductivity of solid-state batteries, destructive operations such as stamping are required before placing the stamped battery and metal sheets inside a filler tube. Metal sheets are placed at both ends of the stamped battery, and the conductivity of the stamped battery is obtained by energizing the metal sheets. Currently, in the conductivity testing process of solid-state batteries, voids easily remain inside the filler tube, leading to obstructed ion or electron transport channels and affecting the accuracy of the conductivity test results. Summary of the Invention

[0004] Therefore, it is necessary to provide a method for detecting the conductivity of solid-state batteries, as well as a solid-state battery and electrical equipment, to address the problem that residual voids in the filler tube can lead to inaccurate conductivity test results.

[0005] A method for detecting the conductivity of a solid-state battery includes the following steps: filling a test sample and metal powder into a filler tube, with metal powder at both ends of the test sample along a first direction, the first direction being the axial direction of the filler tube; compacting the test sample and metal powder; electrically connecting the metal powder at both ends of the test sample to a conductivity testing device; and obtaining the conductivity of the test sample through the conductivity testing device. This method for detecting the conductivity of a solid-state battery, by placing metal powder at both ends of the test sample along the first direction and compacting the test sample and metal powder before testing the conductivity, creates a dense solid-solid contact interface between the test sample and the metal powder. This facilitates smooth ion or electron transport channels in the material, reducing the probability of inaccurate conductivity testing due to excessive voids between the test sample and the metal powder, thus improving the accuracy of conductivity testing for solid-state batteries.

[0006] In some embodiments, the step of filling the packing tube with the test sample and metal powder includes: closing the first open end of the packing tube and opening the second open end of the packing tube, the second open end being positioned opposite to the first open end along a first direction; filling a portion of the metal powder into the end of the packing tube where the first open end is located; placing the test sample into the packing tube; filling another portion of the metal powder into the end of the packing tube where the second open end is located; and closing the second open end. In this way, the test sample and metal powder can be filled into the packing tube, and the test sample has metal powder at both ends along the first direction, resulting in high filling efficiency.

[0007] In some embodiments, after the step of sealing the second opening and before the step of compacting the sample and metal powder, the method further includes: sealing the second opening and the first opening, wherein the airtightness of the packing tube is in the range of 1E-9 Pa·m. 3 / s~1E-6 Pa·m 3 / s. This seals both the second and first opening ends of the packing tube, facilitating subsequent compaction operations on the packing tube.

[0008] In some embodiments, the airtightness of the packing tube is 0.55E-7 Pa·m. 3 / s. Thus, by optimizing the design of the airtightness and leakage rate of the packing tube, the leakage of metal powder at the second opening end and the first opening end during subsequent operations can be improved.

[0009] In some embodiments, the step of compacting the sample and metal powder includes: performing a first compaction operation on the packing tube; and performing a second compaction operation on the packing tube. Thus, by performing two compaction operations, the sample and metal powder can be further compacted, resulting in a denser solid-solid interface between them.

[0010] In some embodiments, the step of performing the first compaction operation includes: fixing the packing tube to the ultrasonic device; subjecting the packing tube to ultrasonic vibration to achieve one-time compaction of the sample and metal powder; and removing the packing tube from the ultrasonic device. Thus, by fixing the packing tube to the ultrasonic device, performing ultrasonic vibration, and then removing the packing tube from the ultrasonic device, the sample and metal powder can be compacted in one step through ultrasonic vibration, resulting in high compaction efficiency and no damage to the sample.

[0011] In some embodiments, when ultrasonically vibrating the packing tube, the ultrasonic frequency is 20kHz to 2000kHz, and the ultrasonic vibration time is 10s to 360s. Thus, by limiting the range of ultrasonic frequency and ultrasonic vibration time, the sample to be tested and the metal powder can be compacted while minimizing energy consumption.

[0012] In some embodiments, the ultrasonic frequency is 50 kHz and the ultrasonic vibration time is 30 s. This optimal design of ultrasonic frequency and vibration time maximizes the compaction effect of the sample and metal powder while minimizing energy consumption.

[0013] In some embodiments, the step of performing the second compaction operation includes: placing the packing tube inside an isostatic container; filling the isostatic container with an isostatic medium; applying pressure to the outer periphery of the isostatic container and transmitting the pressure to the packing tube through the isostatic medium, thereby achieving secondary compaction of the sample and metal powder. Thus, performing isostatic compaction on the packing tube to achieve secondary compaction of the sample and metal powder results in a denser solid-solid interface between the sample and the metal powder.

[0014] In some embodiments, when pressure is applied to the outer periphery of the isostatic pressure vessel, the isostatic pressure is 2 MPa to 1000 MPa, the isostatic temperature is 25°C to 300°C, and the isostatic time is 10 s to 300 s. This allows for secondary compaction of the sample and metal powder, further reducing the voids between them.

[0015] In some embodiments, the isostatic pressure is 500 MPa, the isostatic temperature is 85°C, and the isostatic time is 120 s. This optimizes the isostatic pressure, temperature, and time, further reducing the voids between the sample and the metal powder.

[0016] In some embodiments, the isostatic medium is any one of esters, water, or inert gases. This allows for flexible selection of the isostatic medium material based on specific circumstances.

[0017] In some embodiments, the packing tube is configured to shrink axially at a preset temperature and / or preset pressure. This allows the packing tube to shrink to fit the dimensions of the sample and metal powder before and after compaction.

[0018] In some embodiments, the axial shrinkage rate of the packing tube is 3% to 60%. Thus, by limiting the axial shrinkage rate of the packing tube, the same packing tube can be used for both the test sample and the metal powder before and after compaction.

[0019] In some embodiments, the packing tube is made of any one of polyimide, polyetheretherketone, polytetrafluoroethylene, polypropylene, polyethylene, and polyvinyl chloride. This allows for flexible selection of the packing tube material according to actual needs.

[0020] In some embodiments, in the step of filling the packing tube with the test sample and metal powder, and providing metal powder at both ends of the test sample along a first direction: the height ratio of the metal powder at either end of the test sample to the height of the test sample in the first direction is 1 / 10 to 1 / 2. Thus, by limiting the range of the height ratio between the metal powder and the test sample, a dense solid-solid contact interface can be achieved between the test sample and the metal powder, and the amount of metal powder can meet the usage requirements.

[0021] In some embodiments, the metal powder is one or more of aluminum powder, copper powder, nickel powder, aluminum alloy powder, and copper alloy powder. This allows for flexible selection of the type of metal powder according to actual needs.

[0022] In some embodiments, the sample to be tested is one or at least two of the following: sulfide electrolyte, oxide electrolyte, chloride electrolyte, lithium iron phosphate, ternary lithium electrolyte, silicon-carbon electrolyte, and silver-carbon electrolyte. This allows for flexible selection of the solid electrolyte material according to actual needs.

[0023] A solid-state battery is prepared using the aforementioned solid-state battery conductivity detection method. In this solid-state battery, metal powder is placed at both ends of the sample along a first direction, and the sample and metal powder are compacted before conductivity testing. This results in a dense solid-solid interface between the sample and the metal powder, facilitating smooth ion or electron transport channels and reducing the probability of inaccurate conductivity testing due to excessive voids between the sample and the metal powder. This improves the accuracy of solid-state battery conductivity testing.

[0024] An electrical device includes the aforementioned solid-state battery. This device reduces the probability of inaccurate conductivity testing due to excessively large gaps between the sample and the metal powder, thus improving the accuracy of conductivity testing for solid-state batteries. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the electrical equipment in some embodiments of this application.

[0026] Figure 2 This is a schematic diagram of the sample to be tested in some embodiments of this application.

[0027] Figure 3 This is a schematic diagram of the packing tube in some embodiments of this application.

[0028] Figure 4 This is a schematic diagram of a packing tube placed inside an isostatic pressure vessel in some embodiments of this application.

[0029] Figure 5 This is a schematic diagram of the electrical connection of metal powder in some embodiments of this application.

[0030] Figure 6 This is a flowchart illustrating the conductivity detection method for solid-state batteries in some embodiments of this application.

[0031] Figure 7 This is a flowchart illustrating step S100 in the conductivity detection method for solid-state batteries in some embodiments of this application.

[0032] Figure 8 This is a flowchart illustrating step S200 in the conductivity detection method for solid-state batteries in some embodiments of this application.

[0033] Figure 9 This is a flowchart illustrating step S210 in the conductivity detection method for solid-state batteries in some embodiments of this application.

[0034] Figure 10 This is a flowchart illustrating step S220 in the conductivity detection method for solid-state batteries in some embodiments of this application.

[0035] Figure label:

[0036] 10. Vehicle; 11. Controller; 12. Motor; 20. Solid-state battery; 30. Filler tube; 31. First open end; 32. Second open end; 40. Sample to be tested; 50. Metal powder; 60. Conductivity testing device; 80. Isostatic pressure vessel; 91. Sealing component; 92. Sealing gasket. Detailed Implementation

[0037] The embodiments of the technical solution of this application will now be described in detail with reference to the accompanying drawings. These embodiments are only used to more clearly illustrate the technical solution of this application and are therefore merely examples, and should not be used to limit the scope of protection of this application.

[0038] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the application; the terms “comprising” and “having”, and any variations thereof, in the specification, claims, and foregoing description of the drawings are intended to cover non-exclusive inclusion.

[0039] In the description of the embodiments of this application, technical terms such as "first" and "second" are used only to distinguish different objects and should not be construed as indicating or implying relative importance or implicitly specifying the number, specific order, or primary and secondary relationship of the indicated technical features. In the description of the embodiments of this application, "multiple" means two or more, unless otherwise explicitly defined.

[0040] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0041] In the description of the embodiments in this application, the term "and / or" is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, and B existing alone. Additionally, the character " / " in this document generally indicates that the preceding and following related objects have an "or" relationship.

[0042] In the description of the embodiments of this application, the term "multiple" refers to two or more (including two), similarly, "multiple sets" refers to two or more (including two sets), and "multiple pieces" refers to two or more (including two pieces).

[0043] In the description of the embodiments of this application, the technical terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of this application and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this application.

[0044] In the description of the embodiments of this application, unless otherwise expressly specified and limited, technical terms such as "installation," "connection," "joining," and "fixing" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. For those skilled in the art, the specific meaning of the above terms in the embodiments of this application can be understood according to the specific circumstances.

[0045] With the popularization and promotion of new energy vehicles, their charging and discharging performance and range have increasingly attracted people's attention and importance. As the power energy source for new energy vehicles, power batteries are widely used.

[0046] Solid-state batteries, as one of the future development trends of power batteries, have advantages such as high energy density and good safety. When testing the conductivity of solid-state batteries, destructive operations such as stamping are required before placing the stamped battery and metal sheets inside a filler tube. Metal sheets are placed at both ends of the stamped battery, and the conductivity of the stamped battery is obtained by energizing the metal sheets. Currently, in the conductivity testing process of solid-state batteries, voids easily remain inside the filler tube, leading to obstructed ion or electron transport channels and affecting the accuracy of the conductivity test results.

[0047] Based on the above considerations, and after in-depth research, this application designs a method for detecting the conductivity of solid-state batteries, a solid-state battery, and an electrical device. In the method for detecting the conductivity of solid-state batteries, metal powder is placed at both ends of the sample to be tested along a first direction, and the sample to be tested and the metal powder are compacted before the conductivity is tested. This results in a dense solid-solid contact interface between the sample to be tested and the metal powder, which enables smooth ion or electron transport channels in the material and reduces the probability of inaccurate conductivity testing due to excessive gaps between the sample to be tested and the metal powder, thereby improving the accuracy of conductivity testing of solid-state batteries.

[0048] The solid-state battery of this application embodiment typically includes: a negative electrode, a solid electrolyte, and a positive electrode. The negative electrode includes a negative electrode current collector and a negative electrode active material layer, the negative electrode active material layer being coated on the surface of the negative electrode current collector.

[0049] The negative electrode current collector can be pure lithium, a lithium alloy, or a lithium metal composite oxide. Lithium alloys are alloy materials, including lithium metal and other metals (such as any one or more of aluminum, magnesium, potassium, sodium, and calcium); lithium metal composite oxides are oxides composed of lithium and other metals (such as silicon, tin, zinc, magnesium, cadmium, cerium, and nickel). The negative electrode current collector may also have a protective layer, which can include any material as long as it has lithium-ion conductivity, does not interfere with battery operation, and does not react with lithium. For example, a ceramic protective layer or a lithium-ion polyacrylic acid protective layer can be provided. Any protective layer can be used for the negative electrode current collector in this application embodiment, as long as the protective layer improves the safety of the negative electrode current collector. The negative electrode active material includes at least one of lithium titanate, silicon anode, silicon-carbon anode, lithium metal anode material, tin-based anode material, and tin oxide anode material.

[0050] In this embodiment of the application, the solid electrolyte may include at least one of sulfide solid electrolyte, oxide solid electrolyte and organic solid electrolyte.

[0051] Sulfide-based solid electrolytes possess high lithium-ion conductivity, readily forming a contact interface between the electrode and the electrolyte, and exhibit high mechanical strength and flexibility. In this application, there are no particular limitations on the type of sulfide-based solid electrolyte, and all known sulfide materials used in the battery field are acceptable.

[0052] Oxide-based solid electrolytes exhibit high safety in air and possess lithium-ion conductivity that is lower than, but relatively higher than, that of sulfide-based solid electrolytes. Furthermore, oxide-based solid electrolytes exhibit high electrochemical safety and mechanical strength, and also have high oxidation voltage. However, solid electrolytes have high grain boundary resistance, making it difficult to form a contact interface between the electrode and the electrolyte, requiring high-temperature heat treatment processes of 1000°C or higher, and these processes are difficult to scale up. In the embodiments of this application, the oxide-based solid electrolyte can be any known oxide material used in the field of lithium batteries.

[0053] Organic solid electrolytes (OSEs) are a type of solid electrolyte. OSEs can readily form electrode interfaces and minimize dendrite growth, thus ensuring stable reactions between OSEs and lithium metal. The disadvantages of OSEs are their relatively low lithium-ion conductivity and the fact that they typically require high-temperature operation. In this embodiment, the OSE comprises polyethylene oxide.

[0054] The positive electrode in this application typically includes a positive current collector and a positive active material layer, with the positive active material layer coated on the surface of the positive current collector.

[0055] The positive electrode current collector can be made of aluminum or stainless steel with a surface treated with carbon, nickel, titanium, or silver, or it can be any of the following: membrane, sheet, foil, mesh, porous body, foam, or nonwoven fabric. The positive electrode active material can be lithium cobalt oxide, lithium iron phosphate, ternary lithium, or lithium manganese oxide, etc.

[0056] This application provides an electrical device that uses a solid-state battery as a power source. The electrical device can be, but is not limited to, vehicles, mobile phones, portable devices, laptops, ships, spacecraft, electric toys, and power tools. Vehicles can be gasoline-powered cars, natural gas-powered cars, or new energy vehicles; new energy vehicles can be pure electric vehicles, hybrid electric vehicles, or range-extended electric vehicles, etc.; spacecraft include airplanes, rockets, space shuttles, and spacecraft, etc.; electric toys include stationary or mobile electric toys, such as game consoles, electric car toys, electric ship toys, and electric airplane toys, etc.; power tools include metal cutting power tools, grinding power tools, assembly power tools, and railway power tools, such as electric drills, electric grinders, electric wrenches, electric screwdrivers, electric hammers, impact drills, concrete vibrators, and electric planers, etc.

[0057] For ease of explanation, the following embodiments will be described using a vehicle 10 as an example of an electrical device according to an embodiment of this application.

[0058] Please refer to Figure 1 Vehicle 10 can be a gasoline-powered vehicle, a natural gas-powered vehicle, or a new energy vehicle. New energy vehicles can be pure electric vehicles, hybrid electric vehicles, or range-extended electric vehicles, etc. A solid-state battery 20 is installed inside vehicle 10, and the solid-state battery 20 can be located at the bottom, front, or rear of vehicle 10. The solid-state battery 20 can be used to power vehicle 10; for example, it can serve as the operating power source for vehicle 10. Vehicle 10 may also include a controller 11 and a motor 12. The controller 11 controls the solid-state battery 20 to supply power to the motor 12, for example, to meet the power needs of vehicle 10 during startup, navigation, and driving.

[0059] In some embodiments of this application, the solid-state battery 20 can not only serve as the operating power source for the vehicle 10, but also as the driving power source for the vehicle 10, replacing or partially replacing fuel or natural gas to provide driving force for the vehicle 10.

[0060] Please refer to Figures 2 to 6 The conductivity detection method of the solid-state battery 20 in one embodiment includes the following steps:

[0061] S100. The sample to be tested 40 and metal powder 50 are filled into the packing tube 30, and the sample to be tested 40 is provided with metal powder 50 at both ends along the first direction, the first direction being the axial direction of the packing tube 30.

[0062] S200, the sample to be tested 40 and the metal powder 50 are compacted;

[0063] S300, the metal powder 50 located at both ends of the sample 40 to be tested is electrically connected to the conductivity testing device 60, and the conductivity of the sample 40 to be tested is obtained through the conductivity testing device 60.

[0064] It should be noted that the first direction is the axial direction of the stuffing tube 30, that is... Figure 3 The Z direction is shown.

[0065] In the embodiments of this application, the sample to be tested 40 is a solid electrolyte powder, and the metal powder 50 has conductive properties, so that there is electrical conductivity between the metal powder 50 and the sample to be tested 40, which facilitates subsequent testing to obtain the conductivity of the sample to be tested 40. The conductivity is either ionic conductivity or electronic conductivity.

[0066] In the embodiments of this application, the packing tube 30 is a hollow cylindrical structure, which includes cylindrical, elliptical, or other forms of cylindrical structure. The shape of the packing tube 30 is not specifically limited here. The packing tube 30 is constructed to be able to shrink along its own axis at a preset temperature so that the size of the packing tube 30 can be adapted to the test sample 40 and the metal powder 50 before and after compaction.

[0067] In the embodiments of this application, the purpose of compacting the sample 40 and the metal powder 50 in step S200 is to reduce the gap between them. By compacting the sample 40 and the metal powder 50, the gap between them can be reduced, allowing for more thorough contact and minimizing the impact on the accuracy of subsequent conductivity testing. The compaction process can be achieved in various ways, such as ultrasonic vibration or isostatic compaction.

[0068] In the embodiments of this application, in step S300, the metal powder 50 located at both ends of the sample 40 to be tested is connected to the positive and negative terminals of the conductivity testing device 60, respectively. When the conductivity testing device 60 is in a conductive state, the conductivity of the sample 40 to be tested can be obtained through the conductivity testing device 60.

[0069] The above-described method for detecting the conductivity of solid-state battery 20 involves placing metal powder 50 at both ends of the sample 40 to be tested along the first direction, and then compacting the sample 40 and the metal powder 50 before testing the conductivity. This results in a dense solid-solid contact interface between the sample 40 and the metal powder 50, which facilitates the smooth transport of ions or electrons in the material. This reduces the probability of inaccurate conductivity testing due to excessively large gaps between the sample 40 and the metal powder 50, thereby improving the accuracy of conductivity testing for solid-state battery 20.

[0070] Please refer to some embodiments in this application. Figure 3 and Figure 7 The step S100 of filling the test sample 40 and metal powder 50 into the packing tube 30 includes:

[0071] S110, the first open end 31 of the packing tube 30 is closed and the second open end 32 of the packing tube 30 is opened, with the second open end 32 and the first open end 31 being arranged opposite to each other in the first direction.

[0072] S120. A portion of the metal powder 50 is loaded into one end of the first opening 31 of the packing tube 30.

[0073] S130. Place the sample to be tested 40 inside the packing tube 30;

[0074] S140. Another portion of metal powder 50 is loaded into one end of the packing tube 30 where the second opening end 32 is located.

[0075] S150, Close the second opening end 32.

[0076] It should be noted that the packing tube 30 has a packing cavity inside, and the packing cavity is open at both ends along the first direction (i.e., the first open end 31 and the second open end 32). The sample to be tested 40 and the metal powder 50 are both contained in the packing cavity. The packing cavity is a hollow cylindrical cavity, which may be cylindrical, elliptical, or other shapes. The shape of the packing cavity is not specifically limited here.

[0077] In the embodiments of this application, in step S110, the first open end 31 of the packing tube 30 can be closed in the following way: for example, by covering or inserting the sealing member 91 onto the first open end 31, the first open end 31 can be closed.

[0078] In the embodiments of this application, in step S120, a portion of metal powder 50 is filled into one end of the first open end 31 of the packing tube 30, which can be achieved in the following way: for example, first weigh a preset weight of metal powder 50, and then manually fill the weighed metal powder 50 into one end of the first open end 31 of the packing tube 30.

[0079] In the embodiments of this application, in step S130, the sample to be tested 40 is placed inside the packing tube 30. At this time, the sample to be tested 40 is located on the side of a portion of the metal powder 50 away from the first opening end 31. The sample to be tested 40 and the side of the portion of the metal powder 50 away from the first opening end 31 can be attached tightly or not.

[0080] In the embodiments of this application, in step S140, another portion of metal powder 50 is filled into one end of the second opening end 32 of the packing tube 30, which can be achieved in the following way: for example, first weigh a preset weight of metal powder 50, and then manually fill the weighed metal powder 50 into one end of the second opening end 32 of the packing tube 30.

[0081] In the embodiments of this application, in step S150, closing the second opening end 32 can be achieved in the following way: for example, by covering or inserting the sealing member 91 onto the second opening end 32, the second opening end 32 can be closed.

[0082] With the above settings, the sample to be tested 40 and the metal powder 50 can be filled into the filler tube 30, and the sample to be tested 40 is provided with metal powder 50 at both ends along the first direction, resulting in high filling efficiency.

[0083] Please refer to some embodiments in this application. Figure 4 The procedure following the step of sealing the second opening end 32 and before the step of compacting the sample 40 and the metal powder 50 includes:

[0084] The second opening end 32 and the first opening end 31 are sealed, and the airtightness leakage rate of the packing tube 30 is in the range of 1E-9 Pa·m. 3 / s~1E-6Pa·m 3 / s.

[0085] It should be noted that the airtightness leakage rate is defined as the amount of gas flowing through the leak per unit time when the pressure difference across the leak is known.

[0086] In the embodiments of this application, the sealing treatment of the second opening end 32 and the first opening end 31 can be achieved by the following method: sealing gaskets 92 are respectively covered or inserted on the second opening end 32 and the first opening end 31, and sealant is applied at the connection between the sealing gaskets 92 and each opening end, so as to make the connection between the sealing gaskets 92 and each opening end more sealed.

[0087] The above settings seal the second opening end 32 and the first opening end 31 of the packing tube 30, facilitating subsequent compaction operations on the packing tube 30.

[0088] Please refer to some embodiments in this application. Figure 4 The airtightness leakage rate of the packing tube 30 is 0.55E-7 Pa·m. 3 / s.

[0089] By optimizing the design of the airtightness and leakage rate of the packing tube 30, the leakage of metal powder 50 at the second opening end 32 and the first opening end 31 during subsequent operations can be improved.

[0090] Please refer to some embodiments in this application. Figure 4 and Figure 8 The compaction process for the test sample 40 and the metal powder 50 includes:

[0091] S210, Perform the first compaction operation on the packing tube 30;

[0092] S220, Perform the second compaction operation on the packing tube 30.

[0093] In the embodiments of this application, the first compaction operation and the second compaction operation are performed sequentially.

[0094] With the above settings, by performing two compaction operations, the sample 40 and the metal powder 50 can be further compacted, resulting in a denser solid-solid contact interface between the sample 40 and the metal powder 50.

[0095] Please refer to some embodiments in this application. Figure 4 and Figure 9 Step S210, which involves performing the first compaction operation, includes:

[0096] S211. Fix the packing tube 30 to the ultrasonic device;

[0097] S212. The packing tube 30 is subjected to ultrasonic vibration to compact the sample 40 and the metal powder 50 in one step.

[0098] S213. Remove the packing tube 30 from the ultrasonic device.

[0099] It should be noted that fixing the packing tube 30 to the ultrasonic device before performing ultrasonic vibration can improve the situation where the packing tube 30 falls off or gets detached during ultrasonic vibration.

[0100] In the embodiments of this application, in step S212, ultrasonic vibration of the packing tube 30 can be achieved as follows: the packing tube 30 is fixed by a limiting structure, an ultrasonic generator generates ultrasonic waves, and the generated ultrasonic waves are used to ultrasonically vibrate the packing tube 30. The limiting structure and the ultrasonic generator can be separate structures or an integrated structure.

[0101] With the above setup, after the packing tube 30 is fixed on the ultrasonic device, ultrasonic vibration is performed, and then the packing tube 30 is removed from the ultrasonic device. The ultrasonic vibration can compact the sample 40 and the metal powder 50 in one step, which has high compaction efficiency and does not damage the sample 40.

[0102] Please refer to some embodiments in this application. Figure 4 When the packing tube 30 is subjected to ultrasonic vibration, the ultrasonic frequency is 20kHz~2000kHz and the ultrasonic vibration time is 10s~360s.

[0103] It should be noted that during ultrasonic vibration, both the ultrasonic frequency and the ultrasonic vibration time will affect the compaction effect of the sample 40 and the metal powder 50.

[0104] By setting the ultrasonic frequency and ultrasonic vibration time within a certain range, the sample 40 and the metal powder 50 can be compacted while minimizing energy consumption.

[0105] Please refer to some embodiments in this application. Figure 4 The ultrasonic frequency is 50kHz and the ultrasonic vibration time is 30s.

[0106] With the above settings, the ultrasonic frequency and ultrasonic vibration time are optimally designed, which can optimize the compaction effect of the sample 40 and the metal powder 50, while minimizing energy consumption.

[0107] Please refer to some embodiments in this application. Figure 4 and Figure 10 Step S220, which involves performing the second compaction operation, includes:

[0108] S221. Place the stuffing tube 30 inside the isostatic pressure vessel 80;

[0109] S222. Fill the isostatic pressure vessel 80 with an isostatic medium;

[0110] S223. Apply pressure to the outer periphery of the isostatic pressure vessel 80 and transmit the pressure to the packing tube 30 through the isostatic medium so that the sample 40 to be tested and the metal powder 50 are compacted a second time.

[0111] It is understandable that the packing tube 30 is placed inside the isostatic pressure vessel 80, and the isostatic pressure vessel 80 is filled with an isostatic medium. The uniform isostatic pressure is applied to the outer surface of the isostatic pressure vessel 80, and the pressure is transmitted to the inside of the packing tube 30 through the isostatic medium, so that the sample 40 to be tested and the metal powder 50 are compacted twice.

[0112] In the embodiments of this application, steps S221 and S222 can be performed in a specific order, that is, step S221 can be performed first and then step S222, or step S221 can be performed first and then step S222.

[0113] In the embodiments of this application, when the second compaction operation is performed, pressure is applied to the outer periphery of the isostatic pressure vessel 80, that is, the isostatic pressure vessel 80 will be compressed in all directions, and the sample 40 to be tested and the metal powder 50 in the packing tube 30 will shrink significantly in the axial direction of the packing tube 30.

[0114] With the above settings, isostatic pressing is performed on the packing tube 30 to achieve secondary compaction of the test sample 40 and the metal powder 50, so that the test sample 40 and the metal powder 50 have a denser solid-solid contact interface.

[0115] Please refer to some embodiments in this application. Figure 4 When pressure is applied to the outer periphery of the isostatic pressure vessel 80, the isostatic pressure is 2 MPa to 1000 MPa, the isostatic temperature is 25℃ to 300℃, and the isostatic time is 10s to 300s.

[0116] It should be noted that when pressure is applied to the outer periphery of the isostatic pressure vessel 80, the packing tube 30 is placed inside the isostatic pressure vessel 80. Under the preset isostatic pressure ambient temperature, the packing tube 30 is subjected to isostatic pressure treatment using preset isostatic pressure and isostatic pressure time, so that the sample 40 to be tested and the metal powder 50 can be compacted twice.

[0117] The above settings enable secondary compaction of the test sample 40 and the metal powder 50, further reducing the gap between the test sample 40 and the metal powder 50.

[0118] Please refer to some embodiments in this application. Figure 4 The isostatic pressure is 500 MPa, the isostatic temperature is 85℃, and the isostatic time is 120 s.

[0119] The above settings optimize the isostatic pressure, temperature, and time, further reducing the gap between the test sample 40 and the metal powder 50.

[0120] Please refer to some embodiments in this application. Figure 4 The isostatic medium can be any one of esters, water, or inert gases.

[0121] In the embodiments of this application, the isostatic medium is a medium used to transmit pressure and is a material that does not react with the positive and negative electrodes or the solid electrolyte.

[0122] The above settings allow for flexible selection of materials for isostatic media based on actual conditions.

[0123] Please refer to some embodiments in this application. Figure 4 The stuffing tube 30 is configured to contract along its own axial direction at a preset temperature and / or preset pressure.

[0124] In the embodiments of this application, when the second compaction operation is performed, pressure is applied to the outer periphery of the isostatic pressure vessel 80, that is, the isostatic pressure vessel 80 will be compressed in all directions, and the sample 40 to be tested and the metal powder 50 in the packing tube 30 will shrink significantly in the axial direction of the packing tube 30.

[0125] The above settings allow the packing tube 30 to shrink so that it can fit the dimensions of the sample 40 and the metal powder 50 before and after compaction.

[0126] Please refer to some embodiments in this application. Figure 4 The axial shrinkage rate of the packing tube 30 is 3%~60%.

[0127] It should be noted that axial shrinkage rate is defined as the ratio of the change in longitudinal geometry that occurs at a certain temperature and time to the original geometry.

[0128] By setting the above parameters and limiting the axial shrinkage rate of the packing tube 30, the same packing tube 30 can be used for both the test sample 40 and the metal powder 50 before and after compaction.

[0129] Please refer to some embodiments in this application. Figure 2 The filler tube 30 is made of any one of polyimide, polyetheretherketone, polytetrafluoroethylene, polypropylene, polyethylene, or polyvinyl chloride.

[0130] With the above settings, the material of the packing tube 30 can be flexibly selected according to actual needs.

[0131] Please refer to some embodiments in this application. Figure 5 In the step of filling the test sample 40 and metal powder 50 into the packing tube 30, and providing metal powder 50 at both ends of the test sample 40 along the first direction: in the first direction, the height ratio of the metal powder 50 located at either end of the test sample 40 to the height of the test sample 40 is 1 / 10 to 1 / 2.

[0132] In the embodiments of this application, after the test sample 40 and metal powder 50 are filled into the packing tube 30, the design of the height ratio of metal powder 50 to packing tube 30 needs to take into account that after subsequent processing, there is a dense solid-solid contact interface between the test sample 40 and metal powder 50, and the amount of metal powder 50 can meet the usage requirements.

[0133] By setting the above parameters and limiting the height ratio range between the metal powder 50 and the sample 40 to be tested, a dense solid-solid contact interface can be formed between the sample 40 to be tested and the metal powder 50, and the amount of metal powder 50 can meet the usage requirements.

[0134] Please refer to some embodiments in this application. Figure 5 The metal powder 50 is one or at least two of aluminum powder, copper powder, nickel powder, aluminum alloy powder, and copper alloy powder.

[0135] In the embodiments of this application, the metal powder 50 has conductive properties so that the metal powder 50 and the sample 40 to be tested can be electrically connected, which facilitates subsequent testing to obtain the conductivity of the sample 40 to be tested.

[0136] With the above settings, the type of metal powder 50 can be flexibly selected according to actual needs.

[0137] Please refer to some embodiments in this application. Figure 5 The 40 samples to be tested are one or more of the following: sulfide electrolyte, oxide electrolyte, chloride, lithium iron phosphate, ternary lithium, silicon-carbon, and silver-carbon.

[0138] The above settings allow for flexible selection of the solid electrolyte material based on actual needs.

[0139] Please refer to Figure 1 and Figure 2 In one embodiment, the solid-state battery 20 is prepared using the above-described conductivity detection method for solid-state battery 20.

[0140] It should be noted that the solid-state battery 20 includes not only the negative electrode, solid electrolyte and positive electrode, but also other components such as the casing and terminals.

[0141] The solid-state battery 20 described above, by placing metal powder 50 at both ends of the sample 40 to be tested along the first direction, and then compacting the sample 40 and the metal powder 50 before testing the conductivity, creates a dense solid-solid contact interface between the sample 40 and the metal powder 50. This allows for smooth ion or electron transport channels in the material, reducing the probability of inaccurate conductivity testing due to excessive gaps between the sample 40 and the metal powder 50, and thus improving the accuracy of conductivity testing for the solid-state battery 20.

[0142] Please refer to Figure 1 In one embodiment, the electrical device includes the solid-state battery 20 described above.

[0143] The aforementioned electrical equipment reduces the probability of inaccurate conductivity testing due to excessive gaps between the sample 40 and the metal powder 50, thus improving the accuracy of conductivity testing for the solid-state battery 20.

[0144] According to some embodiments in this application, see Figures 2 to 10 This application provides a method for detecting the conductivity of a solid-state battery 20, comprising the following steps: sealing the first open end 31 of a filler tube 30 and opening the second open end 32 of the filler tube 30; filling a portion of metal powder 50 into one end of the filler tube 30 where the first open end 31 is located; placing the sample to be tested 40 inside the filler tube 30; filling another portion of metal powder 50 into one end of the filler tube 30 where the second open end 32 is located, wherein the height ratio of the metal powder 50 at either end of the sample to be tested 40 to the height of the sample to be tested 40 is 1 / 10 to 1 / 2; sealing the second open end 32 and the first open end 31, wherein the airtightness leakage rate of the filler tube 30 is 0.55E. - 7 Pa·m 3 / s; Fix the packing tube 30 to the ultrasonic device; Perform ultrasonic vibration on the packing tube 30 to achieve primary compaction of the sample 40 and metal powder 50; Remove the packing tube 30 from the ultrasonic device; Place the packing tube 30 into the isostatic pressure vessel 80; Fill the isostatic pressure vessel 80 with isostatic medium; Apply pressure to the outer periphery of the isostatic pressure vessel 80 and transmit the pressure to the packing tube 30 through the isostatic medium to achieve secondary compaction of the sample 40 and metal powder 50. The shrinkage rate of the packing tube 30 is 3%~60%.

[0145] According to some embodiments in this application, see Figure 2 and Figure 1 This application provides a solid-state battery 20, which is prepared using the above-described conductivity detection method for solid-state batteries 20.

[0146] According to some embodiments in this application, see Figure 1 This application provides an electrical device, which includes the solid-state battery 20 described above.

[0147] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and not to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. These modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application, and they should all be covered within the scope of the claims and specification of this application. In particular, as long as there is no structural conflict, the various technical features mentioned in the embodiments can be combined in any way. This application is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A method for detecting the conductivity of a solid-state battery (20), characterized in that, Includes the following steps: The sample to be tested (40) and metal powder (50) are filled in the packing tube (30), and the metal powder (50) is provided at both ends of the sample to be tested (40) along the first direction, the first direction being the axial direction of the packing tube (30); The sample to be tested (40) and the metal powder (50) are compacted. The metal powder (50) located at both ends of the sample (40) to be tested is electrically connected to the conductivity testing device (60), and the conductivity of the sample (40) to be tested is obtained through the conductivity testing device (60).

2. The conductivity detection method for a solid-state battery (20) according to claim 1, characterized in that, The steps of filling the test sample (40) and metal powder (50) into the packing tube (30) include: The first opening end (31) of the packing tube (30) is closed and the second opening end (32) of the packing tube (30) is opened, the second opening end (32) and the first opening end (31) are arranged opposite to each other in the first direction; A portion of the metal powder (50) is filled into one end of the packing tube (30) where the first opening end (31) is located; The sample to be tested (40) is placed inside the packing tube (30); Another portion of the metal powder (50) is filled into one end of the packing tube (30) where the second opening end (32) is located; Close the second opening end (32).

3. The conductivity detection method for a solid-state battery (20) according to claim 2, characterized in that, The procedure following the step of sealing the second opening end (32) and before the step of compacting the sample to be tested (40) and the metal powder (50) further includes: The second opening end (32) and the first opening end (31) are sealed, and the airtightness leakage rate of the packing tube (30) is in the range of 1E-9 Pa·m. 3 / s~1E-6 Pa·m 3 / s.

4. The conductivity detection method for a solid-state battery (20) according to claim 3, characterized in that, The airtightness leakage rate of the packing tube (30) is 0.55E-7 Pa·m. 3 / s.

5. The conductivity detection method for a solid-state battery (20) according to claim 1, characterized in that, The steps of compacting the test sample (40) and the metal powder (50) include: The first compaction operation is performed on the packing tube (30); A second compaction operation is performed on the packing tube (30).

6. The conductivity detection method for a solid-state battery (20) according to claim 5, characterized in that, The steps for performing the first compaction operation include: The packing tube (30) is fixed to the ultrasonic device; The packing tube (30) is subjected to ultrasonic vibration so that the sample to be tested (40) and the metal powder (50) are compacted in one step; Remove the packing tube (30) from the ultrasonic device.

7. The conductivity detection method for a solid-state battery (20) according to claim 6, characterized in that, When the packing tube (30) is subjected to ultrasonic vibration, the ultrasonic frequency is 20kHz~2000kHz and the ultrasonic vibration time is 10s~360s.

8. The conductivity detection method for a solid-state battery (20) according to claim 7, characterized in that, The ultrasonic frequency is 50 kHz, and the ultrasonic vibration time is 30 s.

9. The conductivity detection method for a solid-state battery (20) according to claim 5, characterized in that, The steps for performing the second compaction operation include: The packing tube (30) is placed inside the isostatic pressure vessel (80); The isostatic pressure vessel (80) is filled with an isostatic medium; Pressure is applied to the outer periphery of the isostatic pressure vessel (80) and the pressure is transmitted to the packing tube (30) through the isostatic pressure medium so that the sample to be tested (40) and the metal powder (50) are compacted a second time.

10. The conductivity detection method for a solid-state battery (20) according to claim 9, characterized in that, When pressure is applied to the outer periphery of the isostatic pressure vessel (80), the isostatic pressure is 2 MPa to 1000 MPa, the isostatic temperature is 25°C to 300°C, and the isostatic time is 10 s to 300 s.

11. The conductivity detection method for a solid-state battery (20) according to claim 10, characterized in that, The isostatic pressure is 500 MPa, the isostatic temperature is 85°C, and the isostatic time is 120 s.

12. The conductivity detection method for a solid-state battery (20) according to claim 9, characterized in that, The isostatic medium is any one of esters, water, or inert gases.

13. The conductivity detection method for a solid-state battery (20) according to claim 9, characterized in that, The packing tube (30) is configured to contract along its own axial direction at a preset temperature and / or preset pressure.

14. The conductivity detection method for a solid-state battery (20) according to claim 13, characterized in that, The axial shrinkage rate of the packing tube (30) is 3%~60%.

15. The conductivity detection method for a solid-state battery (20) according to claim 14, characterized in that, The packing tube (30) is made of any one of polyimide, polyether ether ketone, polytetrafluoroethylene, polypropylene, polyethylene, and polyvinyl chloride.

16. The conductivity detection method for a solid-state battery (20) according to claim 1, characterized in that, In the step of filling the test sample (40) and metal powder (50) into the packing tube (30), and providing the metal powder (50) at both ends of the test sample (40) along the first direction: In the first direction, the height ratio of the metal powder (50) located at either end of the test sample (40) to the height of the test sample (40) is 1 / 10 to 1 / 2.

17. The conductivity testing method for the solid-state battery (20) according to claim 1, characterized in that, The metal powder (50) is one or at least two of aluminum powder, copper powder, nickel powder, aluminum alloy powder, and copper alloy powder.

18. The conductivity testing method for the solid-state battery (20) according to claim 1, characterized in that, The sample to be tested (40) is one or at least two of the following: sulfide electrolyte, oxide electrolyte, chloride, lithium iron phosphate, ternary lithium, silicon-carbon, and silver-carbon.

19. A solid-state battery (20), characterized in that, The solid-state battery (20) was prepared using the conductivity testing method described in any one of claims 1-18.

20. An electrical appliance, characterized in that, Including the solid-state battery (20) as described in claim 19.

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