CN111943635A - Preparation method of solid electrolyte - Google Patents
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- CN111943635A CN111943635A CN202010778563.9A CN202010778563A CN111943635A CN 111943635 A CN111943635 A CN 111943635A CN 202010778563 A CN202010778563 A CN 202010778563A CN 111943635 A CN111943635 A CN 111943635A
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- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000003792 electrolyte Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 8
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000009736 wetting Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 12
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 3
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 3
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910010941 LiFSI Inorganic materials 0.000 claims description 2
- 239000002228 NASICON Substances 0.000 claims description 2
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 2
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 claims description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims 1
- 229910052808 lithium carbonate Inorganic materials 0.000 claims 1
- 239000002203 sulfidic glass Substances 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 12
- 229910052744 lithium Inorganic materials 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910009511 Li1.5Al0.5Ge1.5(PO4)3 Inorganic materials 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/90—Electrical properties
- C04B2111/94—Electrically conducting materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
- H01M2300/0071—Oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to the field of batteries, in particular to a preparation method of a solid electrolyte, which comprises the following steps: s1, adding a lithium salt solution with the concentration of 1-3 mol/L into electrolyte powder for wetting, and grinding until the particle size of electrolyte powder particles is 10 mu m; s2, heating the wet electrolyte ground in the step S1 to 140-160 ℃ at a heating rate of 8-15 ℃/min under the pressure of 450-600 MPa, and then preserving heat for 100-150 min; and S3, after the heat preservation in the step S2 is finished, cooling to room temperature to obtain the solid electrolyte. The invention has low sintering temperature, and effectively avoids the problem of element volatilization caused by the high-temperature sintering process; the process flow is simple, the operation is convenient, the cost is low, and the time consumption is short; by using the prepared solid electrolyte, the energy density of the battery can be significantly improved. The solid-state lithium ion battery prepared based on the method has good performance and is suitable for various energy storage devices.
Description
Technical Field
The invention relates to the field of batteries, in particular to a preparation method of a solid electrolyte.
Technical Field
Lithium ion batteries are widely used due to their advantages of high energy density, high operating voltage, long cycle life, low self-discharge rate, rapid charge and discharge, and environmental friendliness. However, the conventional lithium secondary battery contains a large amount of organic electrolyte, has the defects of easy volatilization, flammability, explosiveness and the like, and has serious potential safety hazard. Compared with the traditional liquid electrolyte lithium secondary battery, the solid electrolyte-based all-solid-state lithium battery has larger promotion space in the aspects of battery energy density, working temperature range, cycle life, safety and the like. Therefore, the development of a solid electrolyte with high ionic conductivity, high chemical stability and high cycle performance is one of the important development directions for lithium battery research.
In the conventional ceramic sintering technology, the sintering and heat preservation process usually requires tens of hours of processing time. For solid electrolytes, lithium and sodium are very volatile during sintering. Therefore, too long sintering and holding time and too high sintering temperature can cause loss of volatile elements, and further cause density reduction and performance reduction of the solid electrolyte ceramic, thereby limiting the application of the materials. To overcome these limitations, the conventional ceramic sintering method is continuously innovated and developed. The novel sintering techniques include microwave-assisted sintering, spark plasma sintering, flash sintering, and the like. These new ceramic sintering methods often require the use of vacuum or inert gas shielding during sintering, depending on the properties of the material itself, with limited applicability. In addition, these sintering methods typically require expensive Pt electrodes, complex process flows, and high costs.
Disclosure of Invention
The invention aims to overcome the technical problems that the preparation method of the solid electrolyte in the prior art needs high temperature, is responsible for process flow, has high cost and the like, and provides the preparation method of the solid electrolyte.
The purpose of the invention is realized by the following technical scheme:
a method of preparing a solid electrolyte comprising the steps of:
s1, adding a lithium salt solution with the concentration of 1-3 mol/L into electrolyte powder for wetting, and grinding until the particle size of electrolyte powder particles is 10 mu m; wherein the addition amount of the lithium salt solution is 1-10% of the weight of the solid electrolyte;
s2, filling the wet electrolyte ground in the step S1 into a heating mold, placing the mold under the pressure of 500-600 MPa, rapidly heating to 140-160 ℃ at the heating rate of 10-15 ℃/min, and then preserving heat for 100-150 min; the pressure is maintained in the whole heat preservation process, and the pressure fluctuation range is +/-20 MPa.
And S3, after the heat preservation in the step S2 is finished, cooling to room temperature, and demolding to obtain the solid electrolyte.
The invention provides an ultralow temperature cold sintering process for preparing a solid electrolyte ceramic material by a hot pressing process at 140-160 ℃. The ceramic particles are wetted and then filled into a hot-pressing mold. The liquid phase lubricates the particle surface and facilitates particle rearrangement, so that the sharp edge part of the particles is dissolved into the liquid phase, more gap spaces are generated, and particle sliding is facilitated. With the help of the applied external pressure, the liquid phase tends to redistribute itself and fill into the particle interstices, creating an initial particle compaction at an early stage of sintering. The ceramic-based solid electrolyte can be rapidly prepared through short-time heat preservation and pressure maintaining processes. The invention realizes the rapid preparation of the solid electrolyte at ultralow temperature and effectively solves the problems caused by high-temperature sintering. The invention has simple process flow, low energy consumption, high yield and low preparation cost. The solid-state secondary battery constructed by the solid electrolyte sintered by the method shows excellent electrochemical performance
Preferably, the electrolyte powder in step S1 includes: garnet-type solid electrolyte, NASICON solid electrolyte or sulfide, LiPF6One or more of solid electrolytes such as LiTFSI and LiFSI.
Preferably, the lithium salt solution in step S1 includes a lithium perchlorate solution.
The grinding operation in step S1 described above was performed in an agate mortar. The perchloric acid solution is prepared by perchloric acid with purity of more than 99.9 percent.
Preferably, the grinding time in the step S1 is 180 min.
And step S2, the wet electrolyte powder is placed into a tungsten steel heating die, and the wet electrolyte powder is compacted under the pressure of 10-15 MPa. Then heating to 140-160 ℃ and pressing, sintering and forming. The whole process of the sintering heat preservation process needs pressure maintaining, and preferably, the pressure fluctuation range is +/-20 MPa.
Preferably, the pressure maintaining time in step S2 is 10 min.
The solid electrolyte is prepared by the preparation method of the solid electrolyte.
The solid electrolyte is applied to the preparation of a solid battery.
The prepared solid electrolyte is sequentially polished by 500 meshes, 1000 meshes, 2000 meshes and 3000 meshes of sand paper to obtain the solid electrolyte ceramic. And (2) adopting lithium iron phosphate, lithium cobaltate and NCM ternary positive electrode materials and/or lithium manganate as positive electrode materials of the battery, adopting metal lithium or lithium magnesium alloy as negative electrode materials of the battery, activating the interface, finally packaging in a button battery, and pressurizing and sealing to obtain the solid-state battery.
Compared with the prior art, the invention has the following technical effects:
the preparation method of the solid electrolyte provided by the invention has the advantages that the sintering temperature is low, and the problem of element volatilization caused by a high-temperature sintering process is effectively avoided; the process flow is simple, the operation is convenient, the cost is low, and the time consumption is short; the solid-state battery prepared on the basis has high energy density, can use the metal lithium as a negative electrode, and can obviously improve the energy density of the battery. The solid electrolyte solid lithium ion battery prepared based on the method has good performance, and is suitable for various energy storage devices, such as portable energy storage devices, electric automobiles and electric tools, backup power supplies, reserve power supplies and the like.
Drawings
FIG. 1X-ray diffraction pattern of LAGP prepared in example 1;
FIG. 2 is a topographical view of a LAGP prepared in example 1 under a scanning transmission electron microscope;
FIG. 3 EIS test chart of LAGP prepared in example 1;
FIG. 4 is a graph of lithium stability testing of LAGP prepared in example 1;
fig. 5 charge and discharge curves of the solid-state battery obtained in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail with reference to specific embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Unless otherwise specified, the devices used in this example are all conventional experimental devices, the materials and reagents used are commercially available, and the experimental method without specific description is also a conventional experimental method.
Example 1
A method of preparing a solid electrolyte comprising the steps of:
s1, preparing a lithium salt solution with the concentration of 2mol/L for later use. Taking a proper amount of electrolyte Li1.5Al0.5Ge1.5(PO4)3Adding (LAGP) ceramic powder into an agate mortar, adding 1-10 wt% of lithium perchlorate solution, and fully grinding until the particle size of electrolyte particles is 20 mu m to obtain wet ceramic powder for later use;
s2, placing the wet LAGP powder freshly prepared in the step S1 in a heating mould, compacting, applying pressure of 10MPa, and maintaining the pressure for 10 min. And then placing the heating mold in a hot press, and starting to heat to 140-160 ℃. The heating rate was 10 ℃/min. While raising the temperature, a uniaxial pressure of 600MPa was applied. Pressure maintaining is required in the whole heating process, and the pressure fluctuation range is +/-20 MPa;
and S3, after hot pressing is finished, naturally cooling the heated mold to room temperature, and demolding to obtain the cold-fired solid electrolyte.
The X-ray diffraction pattern of the LAGP solid electrolyte obtained in example 1 was measured, and as shown in fig. 1, it can be seen from fig. 1 that the prepared LAGP solid electrolyte was a pure phase, and the pure phase structure of the electrolyte ensured high ionic conductivity. The appearance of the LAGP solid electrolyte material obtained by cold sintering is shown by observation under a scanning electron microscope. As shown in fig. 2, the obtained LAGP solid electrolyte had a uniform particle size distribution and was dense as a whole.
And polishing the surface of the obtained LAGP solid electrolyte material, and testing the ionic conductivity of the silver-plated electrode. Fig. 3 is an ac impedance spectrum of the LAGP solid electrolyte material. The experimental results show that the ionic conductivity of the prepared LAGP is 2.4x10- 5S/cm。
Example 2
And (3) taking the prepared LAGP ceramic as an electrolyte in the solid-state battery, taking LFP as a positive electrode and metal lithium as a negative electrode, activating the interface, packaging in a button battery, and pressurizing and sealing to obtain the solid-state battery. The assembled solid-state battery described above was subjected to a lithium stability test. The test is carried out at room temperature, and the current density is 0.1mA/cm2. FIG. 4 shows the results of Li-LAGP (CSP) -Li tests. The results show that the cold-fired LAGP solid electrolyte is good in lithium stability.
And carrying out constant-current charge-discharge cycle test on the assembled solid-state battery. The test is carried out at room temperature, the voltage range is 3-4.2V, and charging and discharging are carried out at 0.1C multiplying power. Fig. 5 is a charge and discharge curve of a solid-state lithium ion battery using the prepared LAGP as an electrolyte.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (5)
1. A method of preparing a solid electrolyte, comprising the steps of:
s1, adding a lithium salt solution with the concentration of 1-3 mol/L into electrolyte powder for wetting, and fully grinding until the particle size of electrolyte powder particles is 10 mu m; wherein the addition amount of the lithium salt solution is 1-10% of the weight of the solid electrolyte;
s2, putting the wet electrolyte ground in the step S1 into a heating mold, heating the mold to 140-160 ℃ at a heating rate of 8-15 ℃/min under the pressure of 450-600 MPa, and then preserving heat for 100-150 min; the whole process of heat preservation needs pressure maintaining, and the pressure fluctuation range is +/-20 MPa.
And S3, after the heat preservation in the step S2 is finished, naturally cooling to room temperature, and demoulding to obtain the solid electrolyte.
2. The method for producing a solid electrolyte according to claim 1, wherein the electrolyte powder in step S1 includes: garnet-type solid electrolyte, LiPF6One or more of LiTFSI, LiFSI, NASICON solid electrolyte or sulfide solid electrolyte.
3. The method of claim 1, wherein the lithium salt solution in step S1 includes: lithium carbonate solution, lithium hydroxide solution, LiPF6Solution, lithium perchlorate solution.
4. A solid electrolyte obtained by the method for producing a solid electrolyte according to any one of claims 1 to 3.
5. Use of the solid-state electrolyte according to claim 4 for the preparation of a solid-state battery.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113363562A (en) * | 2021-05-19 | 2021-09-07 | 万向一二三股份公司 | Preparation method of low-resistivity garnet-type modified LLZO solid electrolyte |
| CN114552129A (en) * | 2021-07-13 | 2022-05-27 | 万向一二三股份公司 | Two-sided differentiation lithium cell diaphragm and contain lithium cell of this diaphragm |
| CN114725493A (en) * | 2022-04-11 | 2022-07-08 | 哈尔滨工业大学 | High-performance sulfide solid electrolyte sheet and preparation method and application thereof |
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| CN113363562A (en) * | 2021-05-19 | 2021-09-07 | 万向一二三股份公司 | Preparation method of low-resistivity garnet-type modified LLZO solid electrolyte |
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| CN114552129A (en) * | 2021-07-13 | 2022-05-27 | 万向一二三股份公司 | Two-sided differentiation lithium cell diaphragm and contain lithium cell of this diaphragm |
| CN114552129B (en) * | 2021-07-13 | 2023-10-03 | 万向一二三股份公司 | Double-sided differential lithium battery diaphragm and lithium battery comprising same |
| CN114725493A (en) * | 2022-04-11 | 2022-07-08 | 哈尔滨工业大学 | High-performance sulfide solid electrolyte sheet and preparation method and application thereof |
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