A method of making, a device for making, and a method of using a solid state electrolyte having high ionic conductivity

Abstract

The application discloses a preparation method and a preparation device of a solid-state electrolyte with high ionic conductivity and a use method thereof, relates to the technical field of electrolyte preparation, and comprises the following steps: crushing raw materials of the solid-state electrolyte, keeping warm, and then cooling to room temperature to obtain micron-grade solid-state electrolyte powder; spraying nanometer-grade organic solvents into the micron-grade solid-state electrolyte powder while stirring, then high-temperature stirring, and cooling to room temperature to obtain the solid-state electrolyte with high ionic conductivity; through the dissolving effect of the nanometer-grade organic solvent spraying, nanometer-grade particulate matters on the surface of the micron-grade solid-state electrolyte powder are dissolved in the nanometer-grade organic solvents; and the nanometer-grade particulate matters formed by recrystallization during the evaporation of the nanometer-grade organic solvents will fill in the pores between larger solid-state electrolyte particles, form a more compact solid-state electrolyte film, and thus the obtained solid-state electrolyte has higher ionic conductivity.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of solid-state electrolyte, and in particular to a preparation method and device of a solid-state electrolyte with high ionic conductivity and a use method thereof. BACKGROUND

[0002] Since the 18650 type lithium ion battery with carbon material as the negative electrode and lithium-containing compound as the positive electrode was developed and first commercialized, lithium ion batteries have rapidly developed in the fields of 3C consumer electronics, new energy vehicles, energy storage, etc. due to their high energy density, stable performance, no memory effect, high output voltage, small self-discharge, environmental protection, wide working range, etc. Today, most lithium ion batteries are of liquid structure, and the electrolyte therein plays the functions of solvating lithium ions and transporting lithium ions, which is the "blood" of lithium ion batteries.

[0003] The electrolyte is mainly composed of organic solvents such as ethylene carbonate and propylene carbonate, lithium salts, additives, etc. However, its low ignition point, flammable characteristics, electrolyte decomposition and flammable gas emission between the positive and negative electrodes at high temperature and high voltage, etc. will cause serious battery thermal runaway, and the safety problems caused thereby have been criticized by people. Although the industry and academia have made a lot of optimization on the structure, composition, production process, battery management system, etc. of lithium ion batteries, the safety accidents of lithium ion batteries that occur from time to time still limit the further development of lithium ion batteries.

[0004] Solid-state lithium ion batteries use solid-state electrolytes to replace the separator and liquid electrolyte therein, which will fundamentally solve the above problems and has been widely concerned and deeply expected since it was proposed. Compared with liquid lithium ion batteries, solid-state batteries use non-flammable oxides, sulfides, chlorides or polymers as electrolytes, which further improves the energy density, safety, cycle life, rapid charging and discharging capacity and temperature working range of the battery, etc. Battery characteristics, which is one of the hotspots of attention in the world, and countries have invested a lot of manpower and material resources in the research and development of solid-state batteries. Among various types of solid-state electrolytes, sulfide solid-state electrolytes have good mechanical processability, high energy density, low cost, long cycle life, especially high ionic conductivity, and have high commercialization prospects, and major enterprises have laid out the research and production of sulfide-based solid-state lithium ion batteries.

[0005] The synthesis method of the solid-state electrolyte has two kinds of solid phase method or liquid phase method, the former is mainly high-energy ball milling and heat treatment method, which can realize high ionic conductivity, but the high-energy ball milling itself requires high equipment, long grinding time and low yield, which still needs to be improved to be suitable for large-scale production; the latter is to put the material into a polar organic solvent and stir, then evaporate the solvent and heat treatment to obtain the solid-state electrolyte, which can reduce the production cost and be convenient for large-scale preparation, but in the heat treatment process, the solvent volatilization and the decomposition of the crystallization solvent molecules will produce a porous structure in the electrolyte particles, thereby reducing the ionic conductivity. SUMMARY

[0006] One of the purposes of the present application is to provide a preparation method of a solid-state electrolyte with high ionic conductivity, for improving the yield and ionic conductivity of the solid-state electrolyte.

[0007] The second purpose of the present application is to provide a preparation device for implementing the above preparation method.

[0008] The third purpose of the present application is to provide a use method of the above preparation device for implementing the above preparation device.

[0009] The following technical problems are solved:

[0010] How to improve the yield and ionic conductivity of the solid-state electrolyte.

[0011] The purposes of the present application can be realized by the following technical solutions:

[0012] In a first aspect, the present application discloses a preparation method of a solid-state electrolyte with high ionic conductivity, comprising the following steps:

[0013] S1, crushing the raw material of the solid-state electrolyte to obtain micron-level mixture;

[0014] S2, heat treating the micron-level mixture at 400-600 DEG C for 10-30h, and cooling to room temperature to obtain micron-level solid-state electrolyte powder;

[0015] S3, spraying nano-level organic solvent into the micron-level solid-state electrolyte powder while stirring, the spraying time is 10-108min; then continue to stir at 70-300 DEG C for 3-8h, and cool to room temperature to obtain the solid-state electrolyte with high ionic conductivity.

[0016] It should be noted that in step S3, the stirring temperature should be higher than the recrystallization temperature of the micron-level solid-state electrolyte powder surface nano-particle material and the evaporation temperature of the nano-level organic solvent.

[0017] In a further aspect of the present application, in step S1, the method for crushing the raw material of the solid-state electrolyte is as follows: stirring at a speed of 20000-60000 rpm for 30-60 s, stopping, cooling for 30-120 s, and repeating the operation for 4-10 times.

[0018] Preferably, the stirring is performed at a speed of 20000 rpm for 30 s, stopping, cooling for 60 s, and repeating the operation for 8 times.

[0019] In a further aspect of the present application, in step S3, the spraying amount of the nanoscale organic solvent is 0.01-5% of the weight of the micrometer-scale solid-state electrolyte powder.

[0020] In a further aspect of the present application, in step S3, the nanoscale organic solvent is any one of acetonitrile, carbon tetrachloride, 1,2-ethanediamine, N,N-dimethylacetamide, 1,2-ethanedithiol, ethanethiol, dibromomethane, n-hexane, and n-heptane; the nanoscale organic solvent is selected according to the type of the raw material of the solid-state electrolyte, and the stirring temperature should be higher than the recrystallization temperature of the nanometer particles on the surface of the micrometer-scale solid-state electrolyte powder and the evaporation temperature of the nanoscale organic solvent.

[0021] In a further aspect of the present application, in step S3, the droplet diameter of the nanoscale organic solvent is 50-500 nm.

[0022] In a further aspect of the present application, in step S3, the stirring speed during the spraying of the nanoscale organic solvent into the micrometer-scale solid-state electrolyte powder is 500-3000 rpm.

[0023] In a further aspect of the present application, in step S3, the stirring speed during the continuous stirring at 70-300 ℃ for 3-8 h is 100-1000 rpm.

[0024] In a second aspect, the present application discloses a preparation device for implementing the preparation method of the solid-state electrolyte with high ionic conductivity, which comprises a tank body, a heating device arranged on the side wall of the tank body, a dispersion tank arranged in the tank body, and a stirring device arranged in the dispersion tank; a nanometer spraying head is arranged in the tank body to spray the nanoscale organic solvent into the dispersion tank; an air inlet, an air outlet, and a feeding port are arranged on the tank body, and a recovery device is further arranged on the top of the tank body to recover the nanometer organic solvent.

[0025] In a further aspect of the present application, a condensing mechanism is arranged in the recovery device to reduce the recovered gaseous nanometer organic solvent into liquid.

[0026] In a third aspect, the present application further discloses a use method of the preparation device, which comprises the following steps:

[0027] Step one, through the gas outlet tank vacuum, the internal pressure in 500-2000Pa, 3-5 times after the cycle, through the air inlet into inert gas, control the water vapor content in the tank <0.1ppm, oxygen content <1ppm;

[0028] Step two, through the feed port into the raw material powder into the dispersion tank, the volume of raw material powder accounts for 0.3-0.7 times the volume of dispersion tank;

[0029] Step three, the speed of the stirring device is adjusted to 20000-60000rpm, the duration is 30-60 seconds, stop and heat dissipation 30-120 seconds; repeat the above operation 4-10 times;

[0030] Step four, start heating device temperature setting is 400-600℃, holding time is 10-30 hours, cooling to room temperature, get the size of uniform micron solid electrolyte powder;

[0031] Step five, the speed of the stirring device is adjusted to 500-3000rpm, the size of the gaseous spray is adjusted to 50-500nm and the nano-level organic solvent is sprayed into the dispersion tank, the duration is 10-180min; adjust the speed of the stirring device to 100-1000rpm, the temperature of the heating device is 70-300℃, the duration is 3-8h, and the nano-level organic solvent is recycled and reused by using the recycling device;

[0032] Step six, after cooling to room temperature, seal the dispersion tank and stop the inert gas, finally obtain the solid electrolyte with high ionic conductivity.

[0033] In further schemes of the present application: in step one, the inert gas is argon or nitrogen.

[0034] The beneficial effects of the present application are:

[0035] (1) The preparation method of the solid-state electrolyte with high ionic conductivity of the present application is different from the existing mainstream high-energy ball milling and heat treatment solid phase method and liquid phase method. The preparation method of the present application can crush and disperse the solid-state electrolyte raw materials in a very short time, obtain micron-sized primary products with uniform particle size distribution, and the method is fast, simple, time-saving, efficient and easy to mass produce. Through the dissolving effect of the nano-sized organic solvent spray, the nano-sized particles on the surface of the micron-sized solid-state electrolyte powder are dissolved in the nano-sized organic solvent, so that the micron-sized solid-state electrolyte powder particles are separated from the surface. The size distribution of the micron-sized solid-state electrolyte powder can be adjusted and optimized. Especially, the nano-sized solid-state electrolyte particles formed by recrystallization of the nano-sized particles during the evaporation of the nano-sized organic solvent will fill the pores between the larger solid-state electrolyte particles, forming a more dense solid-state electrolyte film, so that the obtained solid-state electrolyte has higher ionic conductivity.

[0036] (2) The preparation device for preparing the solid-state electrolyte with high ionic conductivity of the present application has strong comprehensive performance. The raw material powder is added into the dispersion tank of the device through the feeding port, avoiding contact pollution with the external environment. The reserved gas inlet and gas outlet can provide inert protective atmosphere of vacuum or ultra-low water and oxygen environment, avoiding the performance reduction caused by the contact of raw material powder or product with water vapor or oxygen. The organic solvent recovery device is more environmentally friendly and reduces production cost. The matched heating device meets the different temperature requirements of different types of solid-state electrolyte preparation processes, and can evaporate organic solvents, suitable for the preparation of sulfides, halides, oxides, polymers and other solid-state electrolytes. BRIEF DESCRIPTION OF DRAWINGS

[0037] The present application will be further described below with reference to the accompanying drawings.

[0038] Figure 1 is a part of the flow chart of the preparation method of the solid-state electrolyte with high ionic conductivity of the present application;

[0039] Figure 2 is a structure schematic diagram of the preparation device of the present application;

[0040] Figure 3 is the electrochemical impedance curve of the solid-state electrolyte with high ionic conductivity prepared in example 9 as the battery pole piece;

[0041] Figure 4 is the voltammetry cycle curve of the solid-state electrolyte with high ionic conductivity prepared in example 9 as the battery pole piece;

[0042] Figure 5 is the voltage-current relationship curve of the solid-state electrolyte with high ionic conductivity prepared in example 9 as the battery pole piece.

[0043] 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

[0044] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0045] The specific embodiments of the present application will be described in detail below, but it should be understood that the scope of protection of the present application is not limited by the specific embodiments.

[0046] The terms used in the embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to limit the present application. The singular forms "a", "an" and "the" used in the embodiments of the present application and the appended claims are also intended to include the plural forms, unless the context clearly indicates otherwise.

[0047] It should be understood that in various embodiments of the present application, the magnitude of the sequence number of each process does not mean the order of execution, and part or all of the steps can be executed in parallel or in sequence, and the execution order of each process should be determined according to its function and inherent logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.

[0048] The weight of the related components mentioned in the embodiments of the present application can not only refer to the specific content of each component, but also represent the weight ratio relationship between each component, therefore, as long as the content of the related components in the embodiments of the present application is enlarged or reduced in proportion, it is within the scope disclosed in the embodiments of the present application. Specifically, the mass mentioned in the embodiments of the present application can be μg, mg, g, kg and other mass units commonly known in the chemical field.

[0049] Unless otherwise defined, all professional terms used below have the same meaning as generally understood by those skilled in the art. The professional terms used in this paper are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present application.

[0050] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present application can be purchased from the market or can be prepared by existing methods.

[0051] The experimental methods in the following examples are all conventional methods, and are carried out according to the techniques or conditions described in the literature in the art or according to the product instructions, unless otherwise specified. The materials, reagents, etc. used in the following examples can be obtained commercially, unless otherwise specified.

[0052] Example 1

[0053] See Figure 1 The present example discloses a method for preparing a solid-state electrolyte with high ionic conductivity, comprising the following steps:

[0054] S1, 500g of Li2S, P2S5 and LiCl powders with a molar ratio of 4:1:3 were crushed, stirred at a speed of 20000 rpm for 30s, stopped, cooled for 60s, and then repeated the operation for 8 times to obtain micron-sized mixed powders;

[0055] S2, the micron-sized mixed powders were kept at 500℃ for 15h, and then cooled to room temperature to obtain micron-sized solid-state electrolyte powders;

[0056] S3, while stirring at a speed of 900 rpm, N,N-dimethylacetamide with a droplet size of 50nm was sprayed into the micron-sized solid-state electrolyte powders, the spraying amount was 1% of the weight of the micron-sized solid-state electrolyte powders, and the spraying time was 30min. During this process, the nano-sized particles on the surface of the micron-sized solid-state electrolyte powders were dissolved in the nano-sized organic solvent, thereby separating from the surface of the micron-sized solid-state electrolyte powders. Then, the stirring was continued at a speed of 300 rpm at 200℃ for 8h. During this process, the N,N-dimethylacetamide was removed by evaporation due to high temperature, and at the same time, the nano-sized particles recrystallized to form nano-sized solid-state electrolyte, which filled the pores between the larger solid-state electrolyte particles. After cooling to room temperature, a solid-state electrolyte with high ionic conductivity was obtained.

[0057] Example 2

[0058] The present example discloses a method for preparing a solid-state electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that "keeping at 500℃ for 15h" in step S2 is replaced by "keeping at 400℃ for 30h", and other steps and conditions remain the same. Finally, a solid-state electrolyte with high ionic conductivity is prepared.

[0059] Example 3

[0060] The present example discloses a method for preparing a solid-state electrolyte with high ionic conductivity. Compared with Example 1, the only difference is that "keeping at 500℃ for 15h" in step S2 is replaced by "keeping at 600℃ for 10h", and other steps and conditions remain the same. Finally, a solid-state electrolyte with high ionic conductivity is prepared.

[0061] Example 4

[0062] The present example discloses a preparation method of a solid-state electrolyte with high ionic conductivity, which is different from Example 1 only in that the spraying amount of N,N-dimethylacetamide in step S3 is replaced by “spraying amount is 0.01% of the weight of micron-level solid-state electrolyte powder”. Other steps and conditions remain the same, and finally a solid-state electrolyte with high ionic conductivity is prepared.

[0063] Example 5

[0064] The present example discloses a preparation method of a solid-state electrolyte with high ionic conductivity, which is different from Example 1 only in that the spraying amount of N,N-dimethylacetamide in step S3 is replaced by “spraying amount is 5% of the weight of micron-level solid-state electrolyte powder”. Other steps and conditions remain the same, and finally a solid-state electrolyte with high ionic conductivity is prepared.

[0065] Example 6

[0066] The present example discloses a preparation method of a solid-state electrolyte with high ionic conductivity, which is different from Example 1 only in that the “then continue stirring at 300 rpm for 8 h at 200°C” in step S3 is replaced by “then continue stirring at 300 rpm for 5 h at 70°C”. Other steps and conditions remain the same, and finally a solid-state electrolyte with high ionic conductivity is prepared.

[0067] Example 7

[0068] The present example discloses a preparation method of a solid-state electrolyte with high ionic conductivity, which is different from Example 1 only in that the “then continue stirring at 300 rpm for 8 h at 200°C” in step S3 is replaced by “then continue stirring at 300 rpm for 3 h at 70°C”. Other steps and conditions remain the same, and finally a solid-state electrolyte with high ionic conductivity is prepared.

[0069] Example 8

[0070] Please refer to Figure 2 , the present example discloses a preparation device for a preparation method of a solid-state electrolyte with high ionic conductivity, which is used for the preparation method of a solid-state electrolyte with high ionic conductivity in Example 1.

[0071] The preparation device comprises a tank body 1 for containing raw material powder 10; a heating device 2 is arranged on the side wall of the tank body 1, and a dispersion tank 3 is arranged in the tank body 1, and the dispersion tank 3 is internally provided with a stirring device 4; a nano nozzle 5 is further arranged in the tank body 1 to spray gaseous spray 11 of nano-level organic solvent to the dispersion tank 3; an air inlet 6, an air outlet 7 and a feeding port 8 are arranged on the tank body 1, and a recovery device 9 is further arranged on the top of the tank body 1 to recover nano organic solvent; and the recovery device 9 is provided with a condensing mechanism to reduce the recovered gaseous nano organic solvent into liquid state.

[0072] The above heating device 2, stirring device 4 and recovery device 9 with condensing mechanism are all mature prior art, and thus will not be described here.

[0073] Example 9

[0074] The embodiment discloses a use method of the preparation device of Example 8 in the preparation method of the solid-state electrolyte with high ionic conductivity of Example 1, comprising the following steps:

[0075] Step one, vacuumize the tank body 1 through the air outlet 7, and maintain the internal pressure at 1000 Pa; after 3 cycles, introduce nitrogen through the air inlet 6, and control the water vapor content in the tank body 1 to be less than 0.1 ppm and the oxygen content to be less than 1 ppm;

[0076] Step two, add 500 g of Li2S, P2S5 and LiCl powders with a molar ratio of 4:1:3 into the dispersion tank 3 through the feeding port 8, and the volume of the raw material powder accounts for 0.3 times of the volume of the dispersion tank 3, and cover it;

[0077] Step three, adjust the rotating speed of the stirring device 4 to 20000 rpm, and the duration is 30 seconds, stop and cool for 60 seconds; repeat the above operation for 8 times to fully mix and uniformly distribute the powders;

[0078] Step four, start the heating device 2 and set the temperature to 500℃, and the holding time is 15 hours; after cooling to room temperature, micron-level solid-state electrolyte powder with uniform size is obtained;

[0079] Step five, the rotation speed of the stirring device 4 is adjusted to 900 rpm, the spray size of the nano-atomizer 5 is adjusted to 50 nm, and the nano-sized N,N-dimethylacetamide is sprayed into the dispersion tank 3, the spraying amount is 5 g, and the duration is 30 min; then the rotation speed of the stirring device 4 is adjusted to 300 rpm, the temperature of the heating device 2 is adjusted to 200℃, and the duration is 8 h, and the nano-sized N,N-dimethylacetamide is recycled and reused by using the recycling device 9; during the process, the nano-sized N,N-dimethylacetamide optimizes the size of the micron-sized solid electrolyte powder in the product, recrystallizes to form a nano-sized solid electrolyte, and fills the pores between the larger particles, which is beneficial to the formation of a more dense solid electrolyte film in the later stage;

[0080] Step six, after cooling to room temperature, the dispersion tank 3 is sealed and the nitrogen gas is stopped, and finally the solid electrolyte with high ionic conductivity is obtained.

[0081] The solid electrolyte with high ionic conductivity obtained in step six is taken as a sample for charge and discharge performance test, and the test method is as follows:

[0082] (1) The sample is weighed in the glove box, about 180 mg, then poured into a battery mold with a diameter of 1 cm, pressed into a sheet under a pressure of 7 t and kept for 5 min, and the electrochemical impedance spectroscopy (EIS) of the battery is measured using a stainless steel electrode, the frequency range is 1 Hz-1 MHz, and the bias voltage is 10 mV, the test result is shown in Figure 3 , and after calculation, it is known that the ionic conductivity of the product is about 2.2 mS / cm;

[0083] (2) The sample is weighed in the glove box, about 180 mg, then poured into a battery mold with a diameter of 1 cm, pressed into a sheet under a pressure of 7 t and kept for 5 min, and the voltammetry cycle curve (CV) of the battery is measured using a stainless steel and lithium metal electrode, and the measurement range is 0-5 V, and the step is 1 mV / s. The results are shown in Figure 4 , from which it can be seen that there is no obvious peak position except for the redox peak of lithium ions near 0 V, indicating that the material has good electrochemical stability.

[0084] (3) The sample is weighed in the glove box, about 180 mg, then poured into a battery mold with a diameter of 1 cm, pressed into a sheet under a pressure of 7 t and kept for 5 min, and the electronic conductivity of the battery is measured using a lithium metal and stainless steel electrode, and the applied voltage is 1 V, the result is shown in Figure 5 , and the calculation shows that the electronic conductivity is 8.5×10-10 S / cm, indicating that the prepared material has good electronic insulation.

[0085] The above detailed description of the present application is only a preferred embodiment of the present application, and should not be considered as limiting the scope of the present application. Any equivalent changes and improvements made according to the scope of the present application should still belong to the patent coverage of the present application.

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 nano-scale organic solvent into the micron-scale 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; 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; and the droplet diameter of the nanoscale organic solvent is 50-500 nm.

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 stirring rate when spraying the nano-sized organic solvent into the micron-sized solid electrolyte powder while stirring is 500-3000 rpm.

4. 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.

5. 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.

6. The preparation device according to claim 5, 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.

7. A method for using the preparation device according to any one of claims 5 to 6, 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.

8. The method for using the preparation device according to claim 7, characterized in that: In step 1, the inert gas is argon or nitrogen.

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