Preparation method, preparation device and use method of solid electrolyte with high ionic conductivity

Abstract

The invention discloses a preparation method, a preparation device and a use method of a solid electrolyte with high ionic conductivity, and relates to the technical field of electrolyte preparation, and the preparation method comprises the following steps: crushing raw materials of the solid electrolyte, carrying out heat preservation, and cooling to room temperature to obtain micron-sized solid electrolyte powder; spraying a nano-scale organic solvent into the micron-scale solid electrolyte powder while stirring, then carrying out high-temperature stirring, and cooling to room temperature to obtain the solid electrolyte with high ionic conductivity, under the dissolving action of nanoscale organic solvent spray, nanoscale particles on the surface of the micron-sized solid electrolyte powder are dissolved in a nanoscale organic solvent; the nanoscale solid electrolyte particles formed by recrystallization of the nanoscale particles in the evaporation process of the nanoscale organic solution can be filled in the pores among the larger solid electrolyte particles to form a more compact solid electrolyte film, so that the obtained solid electrolyte has higher ionic conductivity.

Description

Technical Field

[0001] The present invention relates to the technical field of solid electrolytes, and in particular to a preparation method, a preparation device and a use method of a solid electrolyte with high ionic conductivity. Background Art

[0002] Since the development and commercialization of the 18650 lithium-ion battery, featuring a carbon anode and a lithium-containing compound as the cathode, it has seen rapid growth in consumer electronics, new energy vehicles, and energy storage, owing to its advantages such as high energy density, stable performance, no memory effect, high output voltage, low self-discharge, environmental friendliness, and a wide operating range. Most current lithium-ion batteries are liquid, with the electrolyte serving as the solvation and transport mechanism for lithium ions, effectively acting as the battery's "blood."

[0003] The electrolyte primarily consists of organic solvents such as ethylene carbonate and propylene carbonate, lithium salts, and additives. However, its low flash point, flammability, and interaction with the positive and negative electrodes at high temperatures and voltages can lead to electrolyte decomposition and the release of flammable gases, which can cause severe thermal runaway. The resulting safety issues have long been a source of concern. Although industry and academia have made significant improvements to the structure, components, production processes, and battery management systems of lithium-ion batteries, the recurring safety incidents continue to hinder their further development.

[0004] Solid-state lithium-ion batteries use solid electrolytes to replace the separators and liquid electrolytes, which will fundamentally solve the above problems. Since its proposal, it has received widespread attention and great anticipation. Compared with liquid lithium-ion batteries, solid-state batteries use non-flammable oxides, sulfides, chlorides or polymers as electrolytes to further improve battery characteristics such as energy density, safety, cycle life, rapid charge and discharge capabilities, and temperature operating range. It is one of the hot topics of concern in countries around the world, and all countries have invested a lot of manpower and material resources in the research and development of solid-state batteries. Among various types of solid electrolytes, sulfide solid electrolytes have advantages such as good machinability, high energy density, low cost, long cycle life, and especially high ionic conductivity. They have high commercial prospects, and major companies have laid out the research and development and mass production of sulfide-based solid-state lithium-ion batteries.

[0005] There are two methods for synthesizing solid electrolytes: solid-phase method and liquid-phase method. The former mainly uses the method of high-energy ball milling followed by heat treatment, which can achieve higher ionic conductivity. However, the high-energy ball milling itself has high equipment requirements, long grinding time, and low yield, and still needs to be improved to be suitable for large-scale production. The latter puts the material into a polar organic solvent and stirs it, and then evaporates the solvent and heat treats it to obtain a solid electrolyte, which can reduce production costs and facilitate large-scale preparation. However, during the heat treatment process, the solvent evaporates and the crystallized solvent molecules decompose and escape, which will produce a porous structure inside the electrolyte particles, thereby reducing the ionic conductivity. Summary of the Invention

[0006] One of the objectives of the present invention is to provide a method for preparing a solid electrolyte with high ionic conductivity, so as to improve the yield and ionic conductivity of the solid electrolyte.

[0007] A second object of the present invention is to provide a preparation device for implementing the above preparation method.

[0008] A third object of the present invention is to provide a method for using the above-mentioned preparation device, for implementing the above-mentioned preparation device.

[0009] Solve the following technical problems: How to improve the yield and ionic conductivity of solid-state electrolytes.

[0010] The purpose of the present invention can be achieved through the following technical solutions: In a first aspect, the present invention discloses a method for preparing a solid electrolyte with high ionic conductivity, comprising the following steps: S1. Crushing the raw materials of the solid electrolyte to obtain a micron-sized mixture; S2, keeping the micron-sized mixture at 400-600° C. for 10-30 hours, and cooling it to room temperature to obtain a micron-sized solid electrolyte powder; S3. Spraying a nanometer-sized organic solvent into the micrometer-sized solid electrolyte powder while stirring for 10-108 minutes; then continuing to stir at 70-300° C. for 3-8 hours, and cooling to room temperature to obtain a solid electrolyte with high ionic conductivity.

[0011] It should be noted that in step S3, the stirring temperature should be higher than the recrystallization temperature of the nanoparticles on the surface of the micron-sized solid electrolyte powder and the evaporation temperature of the nano-sized organic solvent.

[0012] In a further embodiment of the present invention, in step S1, the solid electrolyte raw material is crushed by stirring at a speed of 20,000-60,000 rpm for 30-60 seconds, stopping, dissipating heat for 30-120 seconds, and repeating the operation 4-10 times. Preferably, stirring is performed at a speed of 20,000 rpm for 30 seconds, then stopped, heat is dissipated for 60 seconds, and the operation is repeated 8 times.

[0013] In a further embodiment of the present invention: in step S3, the spraying amount of the nano-scale organic solvent is 0.01-5% of the weight of the micron-scale solid electrolyte powder.

[0014] In a further embodiment of the present invention: in step S3, the nanoscale organic solvent is any one of acetonitrile, carbon tetrachloride, 1,2-ethylenediamine, N,N-dimethylacetamide, 1,2-ethanedithiol, ethanethiol, dibromomethane, n-hexane, and n-heptane; the nanoscale organic solvent is selected according to the type of raw materials of the solid electrolyte, and the stirring temperature should be higher than the recrystallization temperature of the nanoparticles on the surface of the micron-sized solid electrolyte powder and the evaporation temperature of the nanoscale organic solvent.

[0015] In a further embodiment of the present invention: in step S3, the diameter of the droplets of the nano-scale organic solvent is 50-500 nm.

[0016] In a further embodiment of the present invention: in step S3, the stirring rate when spraying the nano-sized organic solvent into the micron-sized solid electrolyte powder while stirring is 500-3000 rpm.

[0017] In a further embodiment of the present invention: in step S3, the stirring rate is 100-1000 rpm when stirring is continued at 70-300°C for 3-8 hours.

[0018] In a second aspect, the present invention discloses a preparation device for implementing the preparation method of a solid electrolyte with high ionic conductivity as described above, the device comprising a tank body, a heating device being provided on the side wall of the tank body, and a dispersion tank being provided inside the tank body, wherein a stirring device is provided inside the dispersion tank; a nano-nozzle is also provided inside the tank body for spraying nano-scale organic solvent into the dispersion tank; an air inlet, an air outlet and a feed port are provided on the tank body, and a recovery device is also provided on the top of the tank body for recovering the nano-organic solvent.

[0019] In a further embodiment of the present invention, the recovery device is provided with a condensing mechanism for reducing the recovered gaseous nano-organic solvent to a liquid state.

[0020] In a third aspect, the present invention further discloses a method for using the preparation device as described above, comprising the following steps:

[0021] Step 1: Evacuate the tank through the air outlet to make the internal pressure between 500-2000Pa. After 3-5 cycles, introduce inert gas through the air inlet to control the water vapor content in the tank to less than 0.1ppm and the oxygen content to less than 1ppm. Step 2: Add the raw material powder into the dispersion tank through the feed port. The volume of the raw material powder accounts for 0.3-0.7 times the volume of the dispersion tank. Step 3: Adjust the speed of the stirring device to 20,000-60,000 rpm for 30-60 seconds, stop and dissipate heat for 30-120 seconds; repeat the above operation 4-10 times; Step 4: Start the heating device and set the temperature to 400-600°C for 10-30 hours. After cooling to room temperature, a micron-sized solid electrolyte powder with uniform size is obtained. Step 5: Adjust the speed of the stirring device to 500-3000 rpm, adjust the gaseous spray size of the nano nozzle to 50-500 nanometers, and spray the nano-scale organic solvent into the dispersion tank for 10-180 minutes; then adjust the speed of the stirring device to 100-1000 rpm, the temperature of the heating device to 70-300°C, the duration is 3-8 hours, and use the recovery device to recover and reuse the nano-scale organic solvent; Step 6: After cooling to room temperature, the dispersion tank is sealed with a cover and the introduction of inert gas is stopped, thereby finally obtaining a solid electrolyte with high ionic conductivity.

[0022] In a further embodiment of the present invention: in step 1, the inert gas is argon or nitrogen.

[0023] Beneficial effects of the present invention: (1) The preparation method of the solid electrolyte with high ionic conductivity of the present invention is different from the existing mainstream solid-phase method and liquid-phase method of high-energy ball milling followed by heat treatment. The preparation method of the present invention can crush and disperse the solid electrolyte raw materials in a very short time to obtain a micron-sized primary product with uniform particle size distribution. The method is fast and simple, short in time, highly efficient, and easy to prepare in batches. Through the dissolving effect of the nano-sized organic solvent spray, the nano-sized particles on the surface of the micron-sized solid electrolyte powder are dissolved in the nano-sized organic solvent, thereby detaching from the surface of the micron-sized solid electrolyte powder particles. The size distribution of the micron-sized solid electrolyte powder can be controlled and optimized. In particular, the nano-sized solid electrolyte particles formed by the recrystallization of the nano-sized particles during the evaporation of the nano-sized organic solvent will fill the pores between the larger solid electrolyte particles to form a denser solid electrolyte film, so that the obtained solid electrolyte has a higher ionic conductivity.

[0024] (2) The comprehensive performance of the preparation device for preparing solid electrolytes with high ionic conductivity of the present invention is strong. The raw material powder is added to the dispersion tank of the equipment through the feed port, avoiding contact and pollution with the external environment; the reserved air inlet and air outlet can provide an inert protective atmosphere of a vacuum or ultra-low water and oxygen environment, avoiding the performance degradation caused by contact between the raw material powder or product and water vapor or oxygen; the organic solvent recovery device is more environmentally friendly and reduces production costs; the matching heating device meets the different temperatures required for the preparation process of different types of solid electrolytes, and can evaporate the organic solvent at the same time, and is suitable for the preparation of various solid electrolytes such as sulfides, halides, oxides, polymers, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The present invention will be further described below with reference to the accompanying drawings.

[0026] Figure 1 is a partial flow chart of a method for preparing a solid electrolyte with high ionic conductivity according to Example 1 of the present invention; Figure 2 Schematic diagram of the structure of the preparation device of Example 8 of the present invention; Figure 3 This is an electrochemical AC impedance curve diagram of the solid electrolyte with high ionic conductivity prepared in Example 9 of the present invention when used as a battery electrode; Figure 4 This is the volt-ampere cycle curve when the solid electrolyte with high ionic conductivity prepared in Example 9 of the present invention is used as a battery electrode; Figure 5 This is a voltage-current relationship curve when the solid electrolyte with high ionic conductivity prepared in Example 9 of the present invention is used as a battery electrode.

[0027] In the figure: 1. Tank body; 2. Heating device; 3. Dispersion tank; 4. Stirring device; 5. Nano nozzle; 6. Air inlet; 7. Air outlet; 8. Feed inlet; 9. Recovery device; 10. Raw material powder; 11. Gaseous spray. DETAILED DESCRIPTION

[0028] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0029] The specific embodiments of the present invention are described in detail below, but it should be understood that the protection scope of the present invention is not limited by the specific embodiments.

[0030] The terms used in the examples of this application are for the purpose of describing specific implementation rules only and are not intended to limit this application. The singular forms "a", "an", "the" and "the" used in the implementation rules of this application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.

[0031] It should be understood that in the various embodiments of the present application, the size of the serial number of each process does not mean the order of execution. Some or all steps can be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the implementation regulations of this application.

[0032] The weights of the relevant components mentioned in the examples of this application may not only refer to the specific content of each component, but also represent the weight ratio between the components. Therefore, as long as the content of the relevant components is proportionally enlarged or reduced according to the examples of this application, it is within the scope disclosed in the examples of this application. Specifically, the mass described in the examples of this application may be a mass unit known in the chemical industry, such as μg, mg, g, kg, etc.

[0033] Unless otherwise defined, all technical terms used hereinafter have the same meanings as those generally understood by those skilled in the art. The technical terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.

[0034] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this application can be purchased from the market or prepared by existing methods.

[0035] Unless otherwise specified, the experimental methods in the following examples are conventional methods and were performed according to the techniques or conditions described in the literature in the field or according to the product instructions. The materials and reagents used in the following examples, unless otherwise specified, were all commercially available.

[0036] Example 1

[0037] See also Figure 1 This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity, comprising the following steps: S1. Crushing 500 g of Li2S, P2S5, and LiCl powders with a molar ratio of 4:1:3, stirring at 20,000 rpm for 30 seconds, stopping, dissipating heat for 60 seconds, and repeating the operation 8 times to obtain a micron-sized mixture; S2, keeping the micron-sized mixture at 500° C. for 15 hours, and cooling it to room temperature to obtain a micron-sized solid electrolyte powder; S3. Spray N,N-dimethylacetamide with a droplet size of 50 nm into the micron-sized solid electrolyte powder while stirring at a speed of 900 rpm. The spraying amount is 1% of the weight of the micron-sized solid electrolyte powder. The spraying time is 30 minutes. During this process, the nano-sized particles on the surface of the micron-sized solid electrolyte powder are dissolved in the nano-sized organic solvent, thereby detaching from the surface of the micron-sized solid electrolyte powder particles. Then continue stirring at a speed of 300 rpm at 200°C for 8 hours. During this process, N,N-dimethylacetamide is evaporated and removed due to the high temperature. At the same time, the nano-sized particles are recrystallized to form a nano-sized solid electrolyte, which fills the pores between the larger solid electrolyte particles. After cooling to room temperature, a solid electrolyte with high ionic conductivity is obtained.

[0038] Example 2

[0039] This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that "keeping at 500°C for 15 hours" in step S2 is replaced by "keeping at 400°C for 30 hours", and the other steps and conditions remain the same, and a solid electrolyte with high ionic conductivity is finally obtained.

[0040] Example 3

[0041] This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that "keeping at 500°C for 15 hours" in step S2 is replaced by "keeping at 600°C for 10 hours", and the other steps and conditions remain the same, and a solid electrolyte with high ionic conductivity is finally obtained.

[0042] Example 4

[0043] This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that the spraying amount of N,N-dimethylacetamide in step S3 is replaced with "a spraying amount of 0.01% of the weight of the micron-sized solid electrolyte powder". The other steps and conditions remain the same, and a solid electrolyte with high ionic conductivity is finally obtained.

[0044] Example 5

[0045] This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that the spraying amount of N,N-dimethylacetamide in step S3 is replaced with "a spraying amount of 5% of the weight of the micron-sized solid electrolyte powder". The other steps and conditions remain the same, and a solid electrolyte with high ionic conductivity is finally obtained.

[0046] Example 6

[0047] This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that "then continue stirring at a speed of 300 rpm at 200°C for 8 hours" in step S3 is replaced by "then continue stirring at a speed of 300 rpm at 70°C for 5 hours". The other steps and conditions remain the same, and a solid electrolyte with high ionic conductivity is finally obtained.

[0048] Example 7

[0049] This embodiment discloses a method for preparing a solid electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that "then continue stirring at a speed of 300 rpm at 200°C for 8 hours" in step S3 is replaced by "then continue stirring at a speed of 300 rpm at 70°C for 3 hours". The other steps and conditions remain the same, and a solid electrolyte with high ionic conductivity is finally obtained.

[0050] Example 8

[0051] See also Figure 2 This embodiment discloses a preparation method and a preparation device for a solid electrolyte with high ionic conductivity, which is used for the preparation method of the solid electrolyte with high ionic conductivity in Example 1.

[0052] The preparation device includes a tank body 1 for accommodating raw material powder 10; a heating device 2 is provided on the side wall of the tank body 1, and a dispersion tank 3 is provided inside the tank body 1, and a stirring device 4 is provided inside the dispersion tank 3; a nano nozzle 5 is also provided inside the tank body 1 for spraying a gaseous spray 11 formed by a nano-scale organic solvent into the dispersion tank 3; an air inlet 6, an air outlet 7 and a feed port 8 are provided on the tank body 1, and a recovery device 9 is also provided on the top of the tank body 1 for recovering the nano-organic solvent; a condensing mechanism is provided in the recovery device 9 for reducing the recovered gaseous nano-organic solvent to a liquid state.

[0053] The above-mentioned heating device 2, stirring device 4 and recovery device 9 with condensation mechanism are all mature existing technologies, so they are not described in detail here.

[0054] Example 9

[0055] This embodiment discloses a method for using the preparation device of Example 8 in the method for preparing a solid electrolyte with high ionic conductivity of Example 1, comprising the following steps: Step 1: Evacuate the tank body 1 through the air outlet 7 to maintain the internal pressure at 1000 Pa. After three cycles, introduce nitrogen through the air inlet 6 to control the water vapor content in the tank body 1 to less than 0.1 ppm and the oxygen content to less than 1 ppm. Step 2: Add 500 g of Li2S, P2S5, and LiCl powders with a molar ratio of 4:1:3 into the dispersion tank 3 through the feed port 8. The volume of the raw material powders accounts for 0.3 times the volume of the dispersion tank 3, and cover it; Step 3: Adjust the speed of the stirring device 4 to 20,000 rpm for 30 seconds, stop and dissipate heat for 60 seconds; repeat the above operation 8 times to ensure that the powder is fully mixed; Step 4: Start the heating device 2 and set the temperature to 500° C., keep the temperature for 15 hours, and cool to room temperature to obtain micron-sized solid electrolyte powder; Step 5: Adjust the speed of the stirring device 4 to 900 rpm, adjust the spray size of the nano nozzle 5 to 50 nm, and spray nano-grade N, N-dimethylacetamide into the dispersion tank 3, with a spraying amount of 5 g and a duration of 30 min; then adjust the speed of the stirring device 4 to 300 rpm, the temperature of the heating device 2 to 200 ° C, and the duration for 8 h, and use the recovery device 9 to recycle and reuse the nano-grade N, N-dimethylacetamide; in this process, the nano-grade N, N-dimethylacetamide will optimize the size of the micron-sized solid electrolyte powder in the product, recrystallize to form a nano-scale solid electrolyte, fill the pores between the larger particles, and facilitate the formation of a denser solid electrolyte film in the later stage; Step 6: After cooling to room temperature, the dispersion tank 3 is sealed with a cover and the introduction of nitrogen is stopped, thereby finally obtaining a solid electrolyte with high ionic conductivity.

[0056] The solid electrolyte with high ionic conductivity finally obtained in step 6 is taken as a sample for charge and discharge performance testing. The test method is as follows: (1) Weigh about 180 mg of the sample in the glove box, then pour it into a battery mold with a diameter of 1 cm, press it into a sheet under a pressure of 7 tons and hold the pressure for 5 minutes. Use stainless steel electrodes to measure the electrochemical impedance spectroscopy (EIS) of the battery. The frequency range is 1 Hz-1 MHz and the bias voltage is 10 mV. The test results are as follows: Figure 3 As shown, after calculation, it can be seen that the ionic conductivity of the product is about 2.2mS / cm; (2) Weigh about 180 mg of the sample in the glove box, then pour it into a battery mold with a diameter of 1 cm, press it into a sheet under a pressure of 7 tons and hold the pressure for 5 minutes. Use stainless steel and lithium metal electrodes to measure the battery's voltammetric cycle curve (CV), where the measurement range is 0-5V and the step size is 1mV / s. The results are as follows Figure 4 As shown, it can be seen that except for the redox peak of lithium ions near 0V, there is no obvious peak position, indicating that the material has good electrochemical stability.

[0057] (3) Weigh about 180 mg of the sample in the glove box, then pour it into a battery mold with a diameter of 1 cm, press it into a sheet under a pressure of 7 tons and hold the pressure for 5 minutes. Use lithium metal and stainless steel electrodes to measure the electronic conductivity of the battery. The applied voltage is 1 V. The results are as follows: Figure 5 As shown, the calculated electronic conductivity is 8.5×10-10S / cm, indicating that the prepared material has good electronic insulation.

[0058] The above describes in detail several embodiments of the present invention. However, the above contents are only preferred embodiments of the present invention and should not be considered as limiting the scope of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the present invention.

Claims

1. A method for preparing a solid electrolyte with high ionic conductivity, characterized in that: The steps include: S1. Crushing the raw materials of the solid electrolyte to obtain a micron-sized mixture; S2, keeping the micron-sized mixture at 400-600° C. for 10-30 hours, and cooling it to room temperature to obtain a micron-sized solid electrolyte powder; S3. Spraying a nanometer-sized organic solvent into the micrometer-sized solid electrolyte powder while stirring for 10-108 minutes; then continuing to stir at 70-300° C. for 3-8 hours, and cooling to room temperature to obtain a solid electrolyte with high ionic conductivity.

2. The method for preparing a solid electrolyte with high ionic conductivity according to claim 1, wherein: In step S1, the operation method for crushing the raw material of the solid electrolyte is: stirring at a rotation speed of 20,000-60,000 rpm for 30-60 seconds, then stopping, dissipating heat for 30-120 seconds, and repeating the operation 4-10 times.

3. The method for preparing a solid electrolyte with high ionic conductivity according to claim 1, wherein: In step S3, the nanoscale organic solvent is any one of acetonitrile, carbon tetrachloride, 1,2-ethylenediamine, N,N-dimethylacetamide, 1,2-ethanedithiol, ethanethiol, dibromomethane, n-hexane, and n-heptane.

4. The method for preparing a solid electrolyte with high ionic conductivity according to claim 1, wherein: In step S3, the diameter of the nano-scale organic solvent droplets is 50-500 nm.

5. The method for preparing a solid electrolyte with high ionic conductivity according to claim 1, wherein: In step S3, the stirring rate when spraying the nano-sized organic solvent into the micron-sized solid electrolyte powder while stirring is 500-3000 rpm.

6. The method for preparing a solid electrolyte with high ionic conductivity according to claim 1, wherein: In step S3, the stirring rate is 100-1000 rpm when the stirring is continued at 70-300°C for 3-8 hours.

7. A preparation device, characterized in that: The device is used to implement the method for preparing a solid electrolyte with high ionic conductivity as claimed in claim 1, comprising a tank body (1), a heating device (2) being provided on the side wall of the tank body (1), a dispersion tank (3) being provided inside the tank body (1), and a stirring device (4) being provided inside the dispersion tank (3); a nano nozzle (5) being provided inside the tank body (1) for spraying a nano-scale organic solvent into the dispersion tank (3); an air inlet (6), an air outlet (7) and a feed port (8) being provided on the tank body (1), and a recovery device (9) being provided on the top of the tank body (1) for recovering the nano-scale organic solvent.

8. The preparation device according to claim 7, characterized in that: The recovery device (9) is provided with a condensing mechanism for reducing the recovered gaseous nano-organic solvent to a liquid state.

9. A method for using the preparation device according to any one of claims 7 to 8, characterized in that: The process includes the following steps: Step 1: Vacuum the tank (1) through the gas outlet (7) to make the internal pressure between 500-2000 Pa. After 3-5 cycles, introduce inert gas through the gas inlet (6) to control the water vapor content in the tank (1) to less than 0.1 ppm and the oxygen content to less than 1 ppm. Step 2: adding the raw material powder into the dispersion tank (3) through the feed port (8), wherein the volume of the raw material powder accounts for 0.3-0.7 times the volume of the dispersion tank (3); Step 3: Adjust the speed of the stirring device (4) to 20,000-60,000 rpm for 30-60 seconds, stop and dissipate heat for 30-120 seconds; repeat the above operation 4-10 times; Step 4: Start the heating device (2) and set the temperature to 400-600°C, keep the temperature for 10-30 hours, and cool to room temperature to obtain micron-sized solid electrolyte powder; Step 5: Adjust the rotation speed of the stirring device (4) to 500-3000 rpm, adjust the gaseous spray size of the nano nozzle (5) to 50-500 nanometers, and spray the nano-scale organic solvent into the dispersion tank (3) for a duration of 10-180 minutes; then adjust the rotation speed of the stirring device (4) to 100-1000 rpm, the temperature of the heating device (2) to 70-300° C., the duration of 3-8 hours, and use the recovery device (9) to recycle and reuse the nano-scale organic solvent; Step 6: After cooling to room temperature, the dispersion tank (3) is sealed with a cover and the introduction of inert gas is stopped, thereby finally obtaining a solid electrolyte with high ionic conductivity.

10. The method for using the preparation device according to claim 9, characterized in that: In step 1, the inert gas is argon or nitrogen.

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