CN108832174B - Preparation process of solid-state lithium ion battery - Google Patents
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
The invention discloses a preparation process of a solid lithium ion battery, which comprises the following steps: the method comprises the following steps: the inorganic ceramic electrolyte powder, the binder and the lithium salt are uniformly mixed in the organic solvent to obtain coating slurry, the coating slurry is respectively coated on the surfaces of the positive plate and the negative plate, and the inorganic ceramic electrolyte coated integrated electrode material with the coating thickness of 10-100 mu m is prepared by drying, and has the advantages that: the all-solid-state lithium ion battery has the advantages that the electrolyte with the structure has high ionic conductivity and excellent interface contact, the all-solid-state lithium ion battery has high specific capacity and excellent cycling stability, the preparation method is simple, the cost is low, the electrochemical performance is excellent, and the all-solid-state lithium ion battery has wide application prospect and advantages.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, and relates to a preparation process of a solid-state lithium ion battery.
Background
Since the first commercialized lithium ion battery in the 90 s of the 20 th century, lithium ion batteries have been widely used in the fields of mobile electronic devices, electric tools, small-sized energy storage devices, and the like, due to their advantages of high energy density, large output power, no memory effect, and the like. With the application of lithium ion batteries to power automobiles, lithium ion batteries with high safety and high safety become a research hotspot at home and abroad. Different from the traditional liquid lithium ion battery, the all-solid lithium ion battery does not contain a liquid organic solvent, so that the safety problem of the battery can be fundamentally solved.
Inorganic ceramic electrolytes are concerned by researchers with ultrahigh conductivity and wider electrochemical window, but the preparation process of the thin ceramic sheet is too difficult and complex, and the prepared ceramic sheet has very poor contact with the positive and negative electrode interfaces, so that the application of the inorganic ceramic electrolyte in practical production is greatly limited. Polymer electrolytes have been widely studied because of their good flexibility, which allows good interfacial contact between the electrolyte and the electrode, but their ionic conductivity is low, which limits their further development. Therefore, it is a great challenge to prepare an all-solid-state lithium ion battery having both high ion conductivity and good interface contact.
Disclosure of Invention
The purpose of the invention is: aiming at the defects, a preparation process of the solid-state lithium ion battery is provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation process of a solid-state lithium ion battery comprises the following steps: the method comprises the following steps: uniformly mixing inorganic ceramic electrolyte powder, a binder and lithium salt in an organic solvent to obtain coating slurry, respectively coating the coating slurry on the surfaces of a positive plate and a negative plate, and drying to obtain an inorganic ceramic electrolyte coated integrated electrode material with the coating thickness of 10-100 mu m;
step two: uniformly stirring and mixing the polymer electrolyte, lithium salt and additive to obtain polymer solid electrolytes, and respectively coating the polymer solid electrolytes on the surfaces of electrodes coated with inorganic ceramic electrolytes to obtain electrodes of double solid electrolytes with the thickness of a polymer solid electrolyte layer of 1-10 mu m;
step three: the composite electrodes coated with the double solid electrolytes are attached together, an aluminum plastic film is used as a packaging material, and then vacuumizing and heat sealing are carried out; carrying out hot-pressing treatment on the sealed battery core, and then carrying out cold pressing to obtain the solid-state lithium ion battery, wherein the heat-sealing temperature is 180-; the hot pressing temperature is 50-100 deg.C, hot pressing pressure is 0.1-0.5MPa, and hot pressing time is 1-10 min; the cold pressing temperature is 20-35 deg.C, the cold pressing pressure is 0.1-0.5MPa, and the cold pressing time is 1-10 min.
The inorganic ceramic electrolyte is one or more of lithium lanthanum titanium oxide, lithium lanthanum zirconium oxide and tantalum-doped lithium lanthanum zirconium oxide, and the mass percentage of the inorganic ceramic electrolyte is 10-80 wt%.
The binder is one or more of polymethyl methacrylate, polytetrafluoroethylene emulsion, polyvinylidene fluoride emulsion, polyimide and polyether silane, and the mass percentage of the binder is 1-10 wt%.
The lithium salt in the inorganic ceramic electrolyte is one or more of lithium hexafluorophosphate, lithium bistrifluoromethanesulfonylimide, lithium tetrafluoroborate and lithium dioxalate borate, and the mass percentage of the lithium salt is 10-50 wt%.
The polymer electrolyte is one or more of polymethyl methacrylate, polyether silane, epichlorohydrin rubber and perfluoropolyether, and the mass percentage of the polymer electrolyte is 10-80 wt%.
The lithium salt in the polymer solid electrolyte is one or more of lithium hexafluorophosphate, lithium bistrifluoromethanesulfonimide, lithium tetrafluoroborate and lithium dioxalate borate, and the mass percentage of the lithium salt is 10-50 wt%.
The additive is one or more of ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate, and the mass percentage of the additive is 5-15 wt%.
Compared with the prior art, the invention achieves the technical effects that: the all-solid-state lithium ion battery has the advantages that the electrolyte with the structure has high ionic conductivity and excellent interface contact, the all-solid-state lithium ion battery has high specific capacity and excellent cycling stability, the preparation method is simple, the cost is low, the electrochemical performance is excellent, and the all-solid-state lithium ion battery has wide application prospect and advantages.
Drawings
Fig. 1 is a first charge-discharge curve diagram.
Detailed Description
The invention is further described with reference to the following figures and examples:
the first embodiment is as follows:
as shown in fig. 1: the invention relates to a preparation process of a solid lithium ion battery, which comprises the following steps: the method comprises the following steps: uniformly mixing 35 wt% of tantalum-doped lithium lanthanum zirconium oxide, 5 wt% of polytetrafluoroethylene emulsion and 10 wt% of lithium bis (trifluoromethanesulfonyl) imide in 50 wt% of azomethidone solvent to obtain coating slurry, respectively coating the coating slurry on the surfaces of a positive plate and a negative plate, and drying to obtain an inorganic ceramic electrolyte coated integrated electrode material with the coating thickness of 10 microns;
step two: stirring and mixing 50 wt% of polyether silane, 40 wt% of lithium bistrifluoromethanesulfonimide and 10 wt% of ethylene carbonate uniformly to obtain polymer solid electrolytes, and respectively coating the polymer solid electrolytes on the surfaces of electrodes coated with inorganic ceramic electrolytes to obtain electrodes of the bi-solid electrolytes with polymer solid electrolyte layers of which the thicknesses are 1 mu m;
step three: the composite electrodes coated with the double solid electrolytes are attached together, an aluminum plastic film is used as a packaging material, and then vacuumizing and heat sealing are carried out; carrying out hot-pressing treatment on the sealed battery core, and then carrying out cold pressing to obtain the solid-state lithium ion battery, wherein the heat-sealing temperature is 185 ℃, the heat-sealing time is 5s, and the heat-sealing pressure is 0.2 MPa; the hot-pressing temperature is 80 ℃, the hot-pressing pressure is 0.12MPa, and the hot-pressing time is 10 min; the cold pressing temperature is 25 ℃, the cold pressing pressure is 0.2MPa, and the cold pressing time is 2 min.
Compared with the prior art, the invention achieves the technical effects that: the all-solid-state lithium ion battery has the advantages that the electrolyte with the structure has high ionic conductivity and excellent interface contact, the all-solid-state lithium ion battery has high specific capacity and excellent cycling stability, the preparation method is simple, the cost is low, the electrochemical performance is excellent, and the all-solid-state lithium ion battery has wide application prospect and advantages.
Example two:
as shown in fig. 1: the invention relates to a preparation process of a solid lithium ion battery, which comprises the following steps: the method comprises the following steps: uniformly mixing 45 wt% of lithium lanthanum titanium oxide, 5 wt% of polymethyl methacrylate and 20 wt% of lithium hexafluorophosphate in 30 wt% of azomethyl pyrrolidone solvent to obtain coating slurry, respectively coating the coating slurry on the surfaces of a positive plate and a negative plate, and drying to obtain an inorganic ceramic electrolyte coated integrated electrode material with the coating thickness of 50 microns;
step two: uniformly stirring and mixing 40 wt% of polymethyl methacrylate, 55 wt% of lithium tetrafluoroborate and 15 wt% of dimethyl carbonate to obtain polymer solid electrolytes, and respectively coating the polymer solid electrolytes on the surfaces of electrodes coated with inorganic ceramic electrolytes to obtain electrodes of double solid electrolytes with polymer solid electrolyte layers of which the thicknesses are 5 microns;
step three: the composite electrodes coated with the double solid electrolytes are attached together, an aluminum plastic film is used as a packaging material, and then vacuumizing and heat sealing are carried out; carrying out hot-pressing treatment on the sealed battery core, and then carrying out cold pressing to obtain the solid-state lithium ion battery, wherein the heat-sealing temperature is 200 ℃, the heat-sealing time is 7s, and the heat-sealing pressure is 0.5 MPa; the hot pressing temperature is 70 ℃, the hot pressing pressure is 0.3MPa, and the hot pressing time is 7 min; the cold pressing temperature is 30 ℃, the cold pressing pressure is 0.3MPa, and the cold pressing time is 7 min.
Compared with the prior art, the invention achieves the technical effects that: the all-solid-state lithium ion battery has the advantages that the electrolyte with the structure has high ionic conductivity and excellent interface contact, the all-solid-state lithium ion battery has high specific capacity and excellent cycling stability, the preparation method is simple, the cost is low, the electrochemical performance is excellent, and the all-solid-state lithium ion battery has wide application prospect and advantages.
Example three:
as shown in fig. 1: the invention relates to a preparation process of a solid lithium ion battery, which comprises the following steps: the method comprises the following steps: uniformly mixing lithium lanthanum zirconium oxide with the mass percentage of 20 wt%, polyvinylidene fluoride emulsion with the mass percentage of 10 wt% and lithium tetrafluoroborate in a nitrogen methyl pyrrolidone solvent with the mass percentage of 10 wt% to obtain coating slurry, respectively coating the coating slurry on the surfaces of a positive plate and a negative plate, and drying to obtain an inorganic ceramic electrolyte coated integrated electrode material with the coating thickness of 100 mu m;
step two: stirring and mixing 60 wt% of perfluoropolyether, 35 wt% of lithium dioxalate borate and 5 wt% of ethyl methyl carbonate uniformly to obtain polymer solid electrolytes, and respectively coating the polymer solid electrolytes on the surfaces of electrodes coated with inorganic ceramic electrolytes to obtain electrodes of double solid electrolytes with the thickness of a polymer solid electrolyte layer of 10 mu m;
step three: the composite electrodes coated with the double solid electrolytes are attached together, an aluminum plastic film is used as a packaging material, and then vacuumizing and heat sealing are carried out; carrying out hot-pressing treatment on the sealed battery core, and then carrying out cold pressing to obtain the solid-state lithium ion battery, wherein the heat-sealing temperature is 220 ℃, the heat-sealing time is 10s, and the heat-sealing pressure is 1 MPa; the hot pressing temperature is 100 ℃, the hot pressing pressure is 0.5MPa, and the hot pressing time is 10 min; the cold pressing temperature is 35 ℃, the cold pressing pressure is 0.5MPa, and the cold pressing time is 10 min.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (5)
1. A preparation process of a solid-state lithium ion battery is characterized by comprising the following steps: the method comprises the following steps: the method comprises the following steps: uniformly mixing inorganic ceramic electrolyte powder, a binder and lithium salt in an organic solvent to obtain coating slurry, respectively coating the coating slurry on the surfaces of a positive plate and a negative plate, and drying to obtain an inorganic ceramic electrolyte coated integrated electrode material with the coating thickness of 10-100 mu m;
step two: uniformly stirring and mixing the polymer electrolyte, lithium salt and additive to obtain polymer solid electrolytes, and respectively coating the polymer solid electrolytes on the surfaces of electrodes coated with inorganic ceramic electrolytes to obtain electrodes of double solid electrolytes with the thickness of a polymer solid electrolyte layer of 1-10 mu m;
step three: the composite electrodes coated with the double solid electrolytes are attached together, an aluminum plastic film is used as a packaging material, and then vacuumizing and heat sealing are carried out; carrying out hot-pressing treatment on the sealed battery core, and then carrying out cold pressing to obtain the solid-state lithium ion battery, wherein the heat-sealing temperature is 180-; the hot pressing temperature is 50-100 deg.C, hot pressing pressure is 0.1-0.5MPa, and hot pressing time is 1-10 min; the cold pressing temperature is 20-35 ℃, the cold pressing pressure is 0.1-0.5MPa, and the cold pressing time is 1-10 min;
the polymer electrolyte is one or more of polymethyl methacrylate, polyether silane, epichlorohydrin rubber and perfluoropolyether, and the mass percentage of the polymer electrolyte is 10-80 wt%;
the additive is one or more of ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate, and the mass percentage of the additive is 5-15 wt%.
2. The process according to claim 1, wherein the process comprises the following steps: the inorganic ceramic electrolyte is one or more of lithium lanthanum titanium oxide, lithium lanthanum zirconium oxide and tantalum-doped lithium lanthanum zirconium oxide, and the mass percentage of the inorganic ceramic electrolyte is 10-80 wt%.
3. The process according to claim 1, wherein the process comprises the following steps: the binder is one or more of polymethyl methacrylate, polytetrafluoroethylene emulsion, polyvinylidene fluoride emulsion, polyimide and polyether silane, and the mass percentage of the binder is 1-10 wt%.
4. The process according to claim 1, wherein the process comprises the following steps: the lithium salt in the inorganic ceramic electrolyte is one or more of lithium hexafluorophosphate, lithium bistrifluoromethanesulfonylimide, lithium tetrafluoroborate and lithium dioxalate borate, and the mass percentage of the lithium salt is 10-50 wt%.
5. The process according to claim 1, wherein the process comprises the following steps: the lithium salt in the polymer solid electrolyte is one or more of lithium hexafluorophosphate, lithium bistrifluoromethanesulfonimide, lithium tetrafluoroborate and lithium dioxalate borate, and the mass percentage of the lithium salt is 10-50 wt%.
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| CN109768330B (en) * | 2019-01-07 | 2020-12-08 | 东莞赣锋电子有限公司 | A kind of preparation method of solid electrolyte lithium ion battery and battery |
| CN109761598A (en) * | 2019-01-12 | 2019-05-17 | 杨忠华 | A kind of preparation method of ceramic electrolyte |
| CN111697262A (en) * | 2019-03-14 | 2020-09-22 | 深圳格林德能源集团有限公司 | Composite solid electrolyte, all-solid-state lithium ion battery and preparation method thereof |
| CN113054259A (en) * | 2019-12-29 | 2021-06-29 | 江西格林德能源有限公司 | Preparation process of solid-state lithium ion battery |
| CN112038644A (en) * | 2020-08-24 | 2020-12-04 | 江苏塔菲尔新能源科技股份有限公司 | Functional coating, electrode plate and electrochemical device |
| CN111834662B (en) * | 2020-08-31 | 2022-07-08 | 珠海冠宇电池股份有限公司 | Interface functional layer, preparation method thereof and lithium ion battery |
| CN112599847B (en) * | 2020-12-25 | 2021-12-28 | 哈尔滨工业大学 | A kind of double-layer solid electrolyte film for lithium battery and preparation method thereof |
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| CN106299471A (en) * | 2016-09-19 | 2017-01-04 | 哈尔滨工业大学 | A kind of hybrid solid-state polymer dielectric and preparation method and application |
| CN106537676A (en) * | 2014-07-01 | 2017-03-22 | I-Ten公司 | All-solid-state battery with solid electrolyte and polymer material layer |
| CN106654362A (en) * | 2016-12-07 | 2017-05-10 | 珠海光宇电池有限公司 | Composite solid electrolyte membrane, preparation method and lithium-ion battery |
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| CN106537676A (en) * | 2014-07-01 | 2017-03-22 | I-Ten公司 | All-solid-state battery with solid electrolyte and polymer material layer |
| CN106299471A (en) * | 2016-09-19 | 2017-01-04 | 哈尔滨工业大学 | A kind of hybrid solid-state polymer dielectric and preparation method and application |
| CN106654362A (en) * | 2016-12-07 | 2017-05-10 | 珠海光宇电池有限公司 | Composite solid electrolyte membrane, preparation method and lithium-ion battery |
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