CN113707880A - Positive pole piece containing solid electrolyte and preparation method and application thereof - Google Patents
Positive pole piece containing solid electrolyte and preparation method and application thereof Download PDFInfo
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
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- 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
Abstract
The invention relates to a positive pole piece containing solid electrolyte and a preparation method and application thereof. The positive pole piece includes: an active material, a conductive agent, a binder, and a solid electrolyte; the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ]; wherein the active material comprises: one of lithium iron phosphate LFP, lithium cobaltate LCO, lithium manganate LMO, lithium manganese iron phosphate LMFP or lithium nickel cobalt manganese oxide ternary material; the solid electrolyte includes: one or more of LISICON-type solid electrolyte, NASICON-type solid electrolyte, perovskite-type solid electrolyte, garnet-type solid electrolyte, or sulfide-type solid electrolyte.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a positive pole piece containing solid electrolyte and a preparation method and application thereof.
Background
With the development of the automobile industry, Hybrid Electric Vehicles (HEVs) and Electric Vehicles (EVs) have attracted attention as alternatives to future fuel-powered automobiles, and a mobile power supply system is one of the key components of an electric automobile. Therefore, high performance (i.e., high specific energy, long life, safety), low cost, and environmentally friendly batteries will be a major focus and hot spot for the development of the mobile power industry. Lithium ion batteries are a new generation of green high-energy rechargeable batteries that have been developed to meet this demand. It has the advantages of high voltage, small volume, light weight, high specific energy, no memory effect, no pollution, small self-discharge, long service life, etc.
The positive pole piece is used as an important component of the lithium ion battery and provides a basic source of lithium for the whole battery, but the problems of low ionic conductivity, small specific capacity and the like of the current positive pole are required to be solved; the solid electrolyte material is introduced into the positive pole piece, so that the problem of low ionic conductivity and the like can be effectively solved, and the development of the preparation method of the positive pole piece after the solid electrolyte is added has important practical significance.
Disclosure of Invention
The embodiment of the invention provides a positive pole piece containing a solid electrolyte, and a preparation method and application thereof, aiming at improving the rate capability, the cycle performance and the safety performance of a battery.
In a first aspect, an embodiment of the present invention provides a positive electrode plate containing a solid electrolyte, where the positive electrode plate includes: an active material, a conductive agent, a binder, and a solid electrolyte; the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ];
wherein the active material comprises: one of lithium iron phosphate LFP, lithium cobaltate LCO, lithium manganate LMO, lithium manganese iron phosphate LMFP or lithium nickel cobalt manganese oxide ternary material;
the solid electrolyte includes: one or more of LISICON-type solid electrolyte, NASICON-type solid electrolyte, perovskite-type solid electrolyte, garnet-type solid electrolyte, or sulfide-type solid electrolyte.
Preferably, the conductive agent includes: one or more of carbon black SUPER-P, conductive graphite KS-6, carbon nano-fiber, carbon nano-tube CNT, acetylene black, graphene, Keqin carbon, metal silver and metal gold;
the adhesive comprises: polyvinylidene fluoride, styrene-butadiene latex, styrene-acrylic latex, polyvinyl alcohol, ethylene-vinyl acetate, sodium alginate, polyacrylamide, polymethyl methacrylate-butyl acrylate, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyacrylamide, polyethylene oxide and polytetrafluoroethylene.
Preferably, the garnet-type solid electrolyte is specifically: li7A3Z2O12Wherein A is one or more of La, Ca, Sr, Ba and K, and Z is one or more of Zr, Ta, Nb or Hf;
the NASICON type solid electrolyte specifically comprises: li1+xAxZ2-x(PO4)3Wherein x is between 0.01 and 0.5, A is one or more of Al, Y, Ga, Cr, In, Fe, Se and La, and Z is one or more of Ti, Ge, Ta, Zr, Sn, Fe, V or Hf;
the LISICON-type solid electrolyte specifically comprises: li14A(ZO4)4Wherein A is one or more of Zr, Cr and Sn, and Z is one or more of Si, S and P;
the perovskite type solid electrolyte is specifically as follows: li3xA2/3-xZO3Wherein x is between 0.01 and 0.5, A is one or more of La, Al, Mg, Fe and Ta, and Z is one or more of Ti, Nb, Sr and Pr;
the sulfide solid electrolyte is specifically as follows: xLi2S-(1-x)P2S5、xLi2S-(1-x)Al2S3、xLi2S-(1-x)SiS2Or Li10AZ2S12Wherein, 0<x<1, A is one or more of Ge, Sn and Pb, and Z is one or more of P, S, Al.
In a second aspect, an embodiment of the present invention provides a method for preparing a positive electrode plate containing a solid electrolyte according to the first aspect, where the method for preparing the positive electrode plate contains:
firstly, dissolving a binder in an N-methylpyrrolidone (NMP) solvent, adding a conductive agent for stirring and dispersing, then continuously adding a solid electrolyte for dispersing, finally adding an active material, and preparing anode slurry after uniform dispersion; the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ];
transferring the prepared positive electrode slurry to a coating machine, coating the slurry on a current collector with a wet coating thickness of 100-;
and rolling, slitting and/or die cutting the dried and wound pole piece to obtain the anode pole piece containing the solid electrolyte.
Preferably, the current collector is any one of an aluminum foil, a porous aluminum foil, a carbon-coated aluminum foil or a porous carbon-coated aluminum foil, and the thickness of the current collector is 8-25 μm.
Preferably, the coating mode specifically includes one of knife coating, roll coating transfer coating and slot extrusion coating.
In a third aspect, an embodiment of the present invention provides a lithium battery including the positive electrode tab of the first aspect.
The positive pole piece containing the solid electrolyte provided by the embodiment of the invention can effectively improve the rate capability and the cycle performance of the battery and can improve the safety performance, and the preparation method is safe and easy to implement and is easy to realize large-scale batch production.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
FIG. 1 is a flow chart of a method for preparing a positive electrode plate containing a solid electrolyte according to an embodiment of the present invention;
FIG. 2 is a graph comparing the cycle performance of example 1 of the present invention with that of a comparative example.
Detailed Description
The invention is further illustrated by the following figures and specific examples, but it should be understood that these examples are for the purpose of illustration only and are not to be construed as in any way limiting the present invention, i.e., as in no way limiting its scope.
The invention provides a positive pole piece containing solid electrolyte, which comprises: an active material, a conductive agent, a binder, and a solid electrolyte; the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ];
wherein the active material comprises: one of lithium iron phosphate (LFP), Lithium Cobaltate (LCO), Lithium Manganate (LMO), lithium iron manganese phosphate (LMFP) or lithium nickel cobalt manganese oxide ternary materials;
the solid electrolyte includes: one or more of LISICON-type solid electrolyte, NASICON-type solid electrolyte, perovskite-type solid electrolyte, garnet-type solid electrolyte, or sulfide-type solid electrolyte.
Wherein, the garnet type solid electrolyte specifically comprises: li7A3Z2O12Wherein A is one or more of La, Ca, Sr, Ba and K, and Z is one or more of Zr, Ta, Nb or Hf;
the NASICON type solid electrolyte is specifically as follows: li1+xAxZ2-x(PO4)3Wherein x is between 0.01 and 0.5, A is one or more of Al, Y, Ga, Cr, In, Fe, Se and La, and Z is one or more of Ti, Ge, Ta, Zr, Sn, Fe, V or Hf;
the LISICON-type solid electrolyte is specifically: li14A(ZO4)4Wherein A is one or more of Zr, Cr and Sn, and Z is one or more of Si, S and P;
the perovskite type solid electrolyte is specifically: li3xA2/3-xZO3Wherein x is between 0.01 and 0.5, A is one or more of La, Al, Mg, Fe and Ta, and Z is one or more of Ti, Nb, Sr and Pr;
the sulfide solid electrolyte is specifically: xLi2S-(1-x)P2S5、xLi2S-(1-x)Al2S3、xLi2S-(1-x)SiS2Or Li10AZ2S12Wherein, 0<x<1, A is one or more of Ge, Sn and Pb, and Z is one or more of P, S, Al.
The conductive agent includes: one or more of carbon black SUPER-P, conductive graphite KS-6, carbon nano-fiber, carbon nano-tube CNT, acetylene black, graphene, Keqin carbon, metal silver and metal gold;
the adhesive comprises: polyvinylidene fluoride, styrene-butadiene latex, styrene-acrylic latex, polyvinyl alcohol, ethylene-vinyl acetate, sodium alginate, polyacrylamide, polymethyl methacrylate-butyl acrylate, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyacrylamide, polyethylene oxide and polytetrafluoroethylene.
Fig. 1 is a flowchart of a method for manufacturing a positive electrode sheet containing a solid electrolyte according to an embodiment of the present invention. As shown in fig. 1, the preparation method mainly comprises:
the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ]; the specific compositions of the active material, the conductive agent, the binder, and the solid electrolyte are as described above and will not be repeated here.
specifically, the coating mode specifically includes one of knife coating, roll coating transfer coating and slit extrusion coating.
The current collector can be any one of aluminum foil, porous aluminum foil, carbon-coated aluminum foil or porous carbon-coated aluminum foil, and the thickness of the current collector is 8-25 μm.
And step 130, rolling, slitting and/or die cutting the dried and wound pole piece to obtain the anode pole piece containing the solid electrolyte.
According to the invention, the anode plate containing the solid electrolyte is obtained by selecting a proper material adding proportion and assisting a proper material adding sequence, so that the materials can be fully and uniformly dispersed to prepare the slurry under the condition of not changing the state, coating the slurry on the current collector according to the coating requirement, and performing the working procedures of drying, rolling, slitting and die cutting. The obtained positive pole piece containing the solid electrolyte can effectively improve the rate capability and the cycle performance of the battery and can improve the safety performance. The preparation method is safe and easy to implement, and is easy to realize large-scale batch production.
In order to better understand the technical scheme provided by the invention, the following specific examples are used to respectively illustrate the specific preparation process and characteristics of the positive electrode plate using the invention.
Example 1
Lithium iron phosphate as active material, Super-P and CNT as conductive agent (mass ratio 2: 1), polyvinylidene fluoride as binder and Li as NASICON type solid electrolyte material1.2Al0.2Ti1.8(PO4)3(LATP) specific activity material by mass: conductive agent: adhesive: solid electrolyte 90: 3: 2: preparing, dissolving a binder in an NMP solvent, adding a conductive agent, stirring and dispersing, continuously adding a solid electrolyte for dispersing, and finally adding an active material, and mixing in a charging sequence to prepare anode slurry;
and then starting the coating machine, adjusting the coating thickness and the temperature of the oven, controlling the wet coating thickness to be 450 mu m, controlling the temperature of the oven to be 120 ℃, and rolling, slitting and die cutting the dried pole piece to obtain the anode pole piece A containing the solid electrolyte.
For the convenience of illustrating the properties of the materials, comparative example 1 below was used for comparison.
Comparative example 1
Active material lithium iron phosphate, conductive agents Super-P and CNT (mass ratio of 2: 1) and a binder polyvinylidene fluoride are mixed according to the mass ratio of active materials: conductive agent: binder 90: 3: 2, preparing, dissolving a binder in an NMP solvent, adding a conductive agent, stirring and dispersing, and finally adding an active material, and mixing to obtain anode slurry;
then starting a coating machine, adjusting the coating thickness and the temperature of an oven, controlling the wet coating thickness to be 450 mu m, controlling the temperature of the oven to be 120 ℃, and rolling, slitting and die cutting the dried pole piece to obtain a positive pole piece B which does not contain solid electrolyte;
the positive electrode sheets of example 1 and comparative example 1 were subjected to surface quality, compaction and porosity tests in the same test method, and the test results are shown in table 1.
TABLE 1
The positive electrode sheets of example 1 and comparative example 1 were assembled into cells under the same conditions, respectively, and full charge was performed at a current of 0.1C, and then the cells were subjected to a nail penetration test (nail diameter of 3.5 mm). The test results are shown in table 2, where the test results are passed without ignition or explosion.
TABLE 2
The cells of example 1 and comparative example 1 were compared for capacity retention, and the test results are shown in fig. 2. It can be seen from the comparison that, in embodiment 1, the solid electrolyte contained in the positive electrode slurry is beneficial to the transmission and infiltration of the electrolyte in the transverse direction and the longitudinal direction of the pole piece, and is beneficial to the storage and infiltration of the electrolyte, and the expansion of the pole piece is also beneficial to the relief in the cycle process of the battery cell, so that the amount of the electrolyte extruded under pressure in the expansion process of the pole piece is reduced, and the battery cell still contains rich electrolyte after long-term circulation, thereby ensuring the normal transmission of lithium ions, and further improving the cycle performance.
Example 2
Active material lithium cobaltate, conductive agent Super-P, adhesive meta-polyvinyl fluoride and NASICON type solid electrolyte material Li1.2Al0.2Ti1.8(PO4)3(LATP) specific activity material by mass: conductive agent: adhesive: solid electrolyte 94: 2: 2: 2, preparing, dissolving a binder in an NMP solvent, adding a conductive agent, stirring and dispersing, continuously adding a solid electrolyte for dispersing, and finally adding an active material, and mixing in a charging sequence to prepare anode slurry;
and then starting the coating machine, adjusting the coating thickness and the temperature of the oven, controlling the wet coating thickness to be 400 mu m, controlling the temperature of the oven to be 105 ℃, and rolling, slitting and die cutting the dried pole piece to obtain the anode pole piece containing the solid electrolyte.
Example 3
Active material nickel cobalt manganese ternary material, conductive agent KS-6, adhesive agent polyvinylidene fluoride and LISICON type solid electrolyte material Li14ZrTi1.8(PO4)4(LZTP) specific activity materials by mass: conductive agent: adhesive: solid electrolyte 96: 1.5: 1.5: 1, preparing, dissolving a binder in an NMP solvent, adding a conductive agent, stirring and dispersing, continuously adding a solid electrolyte for dispersing, and finally adding an active material, and mixing in a charging sequence to prepare anode slurry;
and then starting the coating machine, adjusting the coating thickness and the temperature of the oven, controlling the wet coating thickness to be 360 mu m, controlling the temperature of the oven to be 115 ℃, and rolling, slitting and die cutting the dried pole piece to obtain the anode pole piece containing the solid electrolyte.
Example 4
Active material lithium cobaltate, conductive agent Super-P, adhesive meta-polyvinyl fluoride and perovskite type solid electrolyte Li3AlTiO3Materials specific activity by mass: conductive agent: adhesive: solid electrolyte 94: 2: 2: 2, preparing, dissolving a binder in an NMP solvent, adding a conductive agent, stirring and dispersing, continuously adding a solid electrolyte for dispersing, and finally adding an active material, and mixing in a charging sequence to prepare anode slurry;
and then starting the coating machine, adjusting the coating thickness and the temperature of the oven, controlling the wet coating thickness to be 400 mu m, controlling the temperature of the oven to be 105 ℃, and rolling, slitting and die cutting the dried pole piece to obtain the anode pole piece containing the solid electrolyte.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A positive electrode sheet containing a solid electrolyte, comprising: an active material, a conductive agent, a binder, and a solid electrolyte; the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ];
wherein the active material comprises: one of lithium iron phosphate LFP, lithium cobaltate LCO, lithium manganate LMO, lithium manganese iron phosphate LMFP or lithium nickel cobalt manganese oxide ternary material;
the solid electrolyte includes: one or more of LISICON-type solid electrolyte, NASICON-type solid electrolyte, perovskite-type solid electrolyte, garnet-type solid electrolyte, or sulfide-type solid electrolyte.
2. The positive electrode sheet according to claim 1,
the conductive agent includes: one or more of carbon black SUPER-P, conductive graphite KS-6, carbon nano-fiber, carbon nano-tube CNT, acetylene black, graphene, Keqin carbon, metal silver and metal gold;
the adhesive comprises: polyvinylidene fluoride, styrene-butadiene latex, styrene-acrylic latex, polyvinyl alcohol, ethylene-vinyl acetate, sodium alginate, polyacrylamide, polymethyl methacrylate-butyl acrylate, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyacrylamide, polyethylene oxide and polytetrafluoroethylene.
3. The positive electrode sheet according to claim 1,
the garnet-type solid electrolyte specifically comprises: li7A3Z2O12Wherein A is one or more of La, Ca, Sr, Ba and K, and Z is one or more of Zr, Ta, Nb or Hf;
the NASICON type solid electrolyte specifically comprises: li1+xAxZ2-x(PO4)3Wherein x is between 0.01 and 0.5, A is one or more of Al, Y, Ga, Cr, In, Fe, Se and La, and Z is one or more of Ti, Ge, Ta, Zr, Sn, Fe, V or Hf;
the LISICON-type solid electrolyte specifically comprises: li14A(ZO4)4Wherein A is one or more of Zr, Cr and Sn, and Z is one or more of Si, S and P;
the perovskite type solid electrolyte is specifically as follows: li3xA2/3-xZO3Wherein x is between 0.01 and 0.5, A is one or more of La, Al, Mg, Fe and Ta, and Z is one or more of Ti, Nb, Sr and Pr;
the sulfide solid electrolyte is specifically as follows: xLi2S-(1-x)P2S5、xLi2S-(1-x)Al2S3、xLi2S-(1-x)SiS2Or Li10AZ2S12Wherein, 0<x<1, A is one or more of Ge, Sn and Pb, and Z is one or more of P, S, Al.
4. A method for preparing a positive electrode plate containing a solid electrolyte according to any one of claims 1 to 3, wherein the method comprises:
firstly, dissolving a binder in an N-methylpyrrolidone (NMP) solvent, adding a conductive agent for stirring and dispersing, then continuously adding a solid electrolyte for dispersing, finally adding an active material, and preparing anode slurry after uniform dispersion; the components in percentage by mass are as follows: active materials, conductive agents, binders, solid electrolytes [80-98]: 0.1-5]: 1.0-10]: 0.1-5 ];
transferring the prepared positive electrode slurry to a coating machine, coating the slurry on a current collector with a wet coating thickness of 100-;
and rolling, slitting and/or die cutting the dried and wound pole piece to obtain the anode pole piece containing the solid electrolyte.
5. The method for preparing the positive electrode plate according to claim 4, wherein the current collector is any one of an aluminum foil, a porous aluminum foil, a carbon-coated aluminum foil or a porous carbon-coated aluminum foil, and the thickness of the current collector is 8-25 μm.
6. The preparation method of the positive pole piece according to claim 4, wherein the coating mode specifically comprises one of knife coating, roll coating transfer coating and slit extrusion coating.
7. A lithium battery comprising the positive electrode sheet according to any one of claims 1 to 3.
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