CN111384436B - All-solid-state lithium ion battery with negative electrode coated with solid electrolyte slurry and preparation method thereof - Google Patents
All-solid-state lithium ion battery with negative electrode coated with solid electrolyte slurry and preparation method thereof Download PDFInfo
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Abstract
The invention provides an all-solid-state lithium ion battery with a composite negative electrode plate coated with solid electrolyte slurry and a preparation method thereof, belonging to the technical field of lithium batteries. The invention firstly uses aqueous polymer solid electrolyte to prepare a composite negative pole piece, then slurry mixed with oily organic binder and high oxide solid electrolyte content is coated on the composite negative pole piece for drying and rolling, and then the composite negative pole piece and the composite positive pole prepared by the high-pressure resistant oily polymer electrolyte are assembled into the battery. And adding a small amount of organic solvent between the positive electrode and the negative electrode in the battery assembly process to wet an interface, and drying the organic solvent before packaging the battery. The all-solid-state battery assembled by the method has excellent safety performance, high energy density and good cycle performance.
Description
Technical Field
The invention relates to an all-solid-state lithium ion battery with a negative electrode coated with solid electrolyte slurry and a preparation method thereof, belonging to the technical field of lithium batteries.
Background
With the wide application of lithium ion batteries in electric vehicles and energy storage power stations, people have raised higher requirements on the energy density, the rapid charge and discharge performance and the like of the lithium ion batteries, and the potential safety hazards are increased continuously. The all-solid-state lithium ion battery uses non-combustible or non-combustible solid electrolyte to replace combustible organic electrolyte in the traditional battery, so that the safety problem of the lithium ion battery can be fundamentally solved, and the service temperature range, the cycle life and the energy density of the battery can be improved.
The interface problem that is difficult to solve in the all-solid battery is the biggest obstacle that limits its practical application. The polymer electrolyte has good flexibility and can ensure better interface contact in the battery, the oxide electrolyte has higher lithium ion conductivity and safety performance, and the preparation of the battery by combining the polymer electrolyte and the oxide electrolyte is hopeful to obtain the all-solid-state battery with the electrochemical performance meeting the actual requirement.
Most of the research at present uses PEO-based polymer electrolytes to assemble all-solid batteries. The PEO-based polymer electrolyte has the advantages of good low-voltage stability, low interface impedance and the like, but can be oxidized and decomposed at a voltage of more than 4V, and only a lithium iron phosphate material can be matched with a common cathode material, so that the energy density of the battery is limited. Meanwhile, the conductivity of the PEO-based polymer electrolyte is low, and the assembled all-solid-state battery can only operate at high temperature and low rate.
The aqueous polymer electrolyte represented by PEO is only used for preparing a composite negative electrode, and then the electrolyte layer with high oxide electrolyte content and the composite positive electrode prepared by the high-voltage-resistant oily polymer electrolyte are combined, so that the safety, the energy density and the cycle performance of the all-solid-state battery can be obviously improved.
Disclosure of Invention
The invention provides an all-solid-state lithium ion battery with a negative electrode coated with solid electrolyte slurry and a preparation method thereof, belonging to the technical field of lithium batteries. The invention firstly uses aqueous polymer solid electrolyte to prepare a composite negative pole piece, then slurry mixed with oily organic binder and high oxide solid electrolyte content is coated on the composite negative pole piece for drying and rolling, and then the composite negative pole piece and the composite positive pole prepared by the high-pressure resistant oily polymer electrolyte are assembled into the battery. And adding a small amount of organic solvent between the positive electrode and the negative electrode in the battery assembly process to wet an interface, and drying the organic solvent before packaging the battery. The preparation method comprises the following specific steps:
(1) mixing a solid electrolyte composed of a water-based polymer solid electrolyte or a mixture of the water-based polymer solid electrolyte and an oxide solid electrolyte, a negative electrode active substance, an electronic conductive additive and a water-based solvent to prepare a slurry, coating the slurry on a copper foil, and drying to obtain a composite negative electrode piece;
(2) mixing oxide solid electrolyte, oily organic binder and oily solvent to prepare slurry, coating the slurry on the composite negative electrode plate obtained in the step (1), drying and rolling, wherein the solid electrolyte accounts for 70-95% of the total mass of the solid electrolyte and the oily organic binder
(3) Mixing a solid electrolyte composed of an oily polymer solid electrolyte or a mixture of the oily polymer solid electrolyte and an oxide solid electrolyte, a positive active substance, an electronic conductive additive and an oily solvent to prepare a slurry, coating the slurry on an aluminum foil, and drying to obtain a composite positive pole piece;
(4) and (3) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece lamination obtained in the step (3), adding a small amount of oily solvent to wet an interface between the cathode and the anode during lamination, standing for 0.5-10 hours, drying and drying the oily solvent, and packaging to obtain the all-solid-state battery.
The aqueous polymer solid electrolyte in the step (1) is a mixture of an aqueous polymer matrix and lithium salt, the lithium salt accounts for 10% -60%, wherein the aqueous polymer matrix is one or a mixture of polyethylene oxide (PEO), polyethylene glycol (PEG) and polypropylene oxide (PPO), and the lithium salt is LiN (SO)2CF3)2、LiClO4、LiSO2CF3、LiB(C2O4)2、LiPF6And LiI, or a mixture of two or more of the same.
The oxide solid electrolyte in the steps (1) to (3) is one or a mixture of more of Lithium Lanthanum Zirconium Oxide (LLZO), tantalum-doped lithium lanthanum zirconium oxide (Ta-LLZO), gallium-doped lithium lanthanum zirconium oxide (Ga-LLZO), Lithium Lanthanum Titanium Oxide (LLTO), titanium aluminum lithium phosphate (LATP) and germanium aluminum lithium phosphate (LAGP).
The oily polymer solid electrolyte in the step (3) is a mixture of an oily polymer matrix and lithium salt, the lithium salt accounts for 10% -60%, wherein the oily polymer matrix is one or a mixture of polyvinylidene fluoride (PVDF), polyvinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP) and Polyacrylonitrile (PAN), and the lithium salt is LiN (SO)2CF3)2、LiClO4、LiSO2CF3、LiB(C2O4)2、LiPF6And LiI, or a mixture of two or more of the same.
The oily organic binder in the step (2) is one or a mixture of PVDF, PVDF-HFP, PAN or the oily polymer solid electrolyte in the step (3).
The aqueous solvent in the step (1) is one or a mixture of water, acetonitrile, ethanol, acetone and tetrahydrofuran.
The oily solvent in the steps (2) - (4) is one or a mixture of several of Dimethylformamide (DMF), Dimethylacetamide (DMAC), Tetramethylurea (TMU), dimethyl sulfoxide (DMSO), triethyl phosphate and N-methyl-2-pyrrolidone (NMP).
The positive active material in the steps (1) and (3) is one or a mixture of more of lithium cobaltate, lithium manganate, nickel cobalt manganese ternary, lithium iron phosphate and nickel lithium manganate, the negative active material is one or a mixture of more of graphite, amorphous carbon, mesocarbon microbeads, nano silicon, a silicon carbon material and lithium titanate, and the electronic conductive additive is one or a mixture of more of carbon black, conductive graphite, carbon nanotubes, graphene and carbon fibers.
The oily solvent in the step (4) comprises: dimethylformamide (DMF), Dimethylacetamide (DMAC), Tetramethylurea (TMU), Dimethylsulfoxide (DMSO), triethylphosphate, N-methyl-2-pyrrolidone (NMP), and the like.
According to the invention, the aqueous polymer electrolyte represented by PEO is only used for preparing the composite negative electrode, and then the electrolyte layer with high oxide electrolyte content and the composite positive electrode prepared by the high-voltage-resistant oily polymer electrolyte are combined, so that the safety, the energy density and the cycle performance of the all-solid-state battery can be obviously improved.
The all-solid-state lithium ion battery prepared by the method has excellent safety performance and good cycle performance. The method has the advantages of good matching performance with the coating process in the existing lithium ion battery industry, simple process, low cost and good product consistency, and is suitable for industrial batch production.
Drawings
Fig. 1 is a schematic diagram of a preparation method of an all-solid-state battery.
FIG. 2 is a scanning electron microscope image of the surface of the negative electrode plate coated with the solid electrolyte in example 1.
Fig. 3 is a graph showing charge and discharge cycle characteristics of the all-solid battery prepared in example 2.
Detailed Description
The technical solution of the present invention is further described and illustrated by the following specific examples, but the present invention is not limited to the following examples.
Example 1
(1) PEO polymer solid electrolyte (LiN (SO)2CF3)2The content of 40 percent), graphite, conductive carbon black and water are mixed to prepare slurry, the slurry is coated on copper foil, and the composite negative pole piece is obtained after drying;
(2) mixing Ta-doped LLZO, PVDF and NMP to prepare slurry, coating the slurry on the composite negative electrode plate obtained in the step (1), drying and rolling, wherein the proportion of the solid electrolyte in the total mass of the solid electrolyte and the oily organic binder is 85 percent
(3) PVDF-HFP polymer solid electrolyte (LiN (SO)2CF3)2The content of 30 percent), the nickel-cobalt-manganese ternary material, the conductive carbon black, the carbon nano tube and NMP are mixed to prepare slurry, and the slurry is coated on an aluminum foil and dried to obtain a composite positive pole piece;
(4) and (3) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece lamination obtained in the step (3), adding a small amount of DMF (dimethyl formamide) between the anode and the cathode during lamination to wet an interface, standing for 3 hours, drying and drying the DMF, and packaging to obtain the all-solid-state battery.
Example 2
(1) PEO polymer solid electrolyte (LiN (SO)2CF3)235% content), PEG polymer solid electrolyte (LiN (SO)2CF3)2The content is 35 percent), mixing the solid electrolyte consisting of the mixture of the Ta-doped LLZO solid electrolyte, graphite, conductive carbon black and acetonitrile to prepare slurry, coating the slurry on a copper foil, and drying to obtain a composite negative pole piece;
(2) ta-doped LLZO, PVDF polymer solid electrolyte (LiN (SO)2CF3)2Content 25%) and DMF are mixed to prepare slurry, the slurry is coated on the composite negative electrode plate obtained in the step (1), and the slurry is dried and rolled, wherein the proportion of the solid electrolyte in the total mass of the solid electrolyte and the oily organic binder is 90%;
(3) PVDF polymer solid electrolyte (LiN (SO)2CF3)2The content is 25%), the solid electrolyte consisting of the mixture of LLZO solid electrolyte doped with Ta, the ternary material of nickel, cobalt and manganese, the conductive carbon black and DMF are mixed to prepare slurry, the slurry is coated on an aluminum foil, and the composite positive pole piece is obtained after drying;
(4) and (3) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece lamination obtained in the step (3), adding a small amount of DMAC (dimethylacetamide) wetting interface between the cathode and the anode during lamination, standing for 5 hours, drying and drying the DMAC, and packaging to obtain the all-solid-state battery.
Example 3
(1) PPO polymer solid electrolyte (LiClO)4The content of the lithium titanate is 20%), the conductive carbon black, the carbon nano tube and the tetrahydrofuran are mixed to prepare slurry, the slurry is coated on the copper foil, and the composite negative pole piece is obtained after drying;
(2) LAGP, PAN polymer solid electrolyte (LiN (SO)2CF3)2The content of the solid electrolyte is 20%) and DMSO are mixed to prepare slurry, the slurry is coated on the composite negative electrode plate obtained in the step (1), and the slurry is dried and rolled, wherein the solid electrolyte accounts for 75% of the total mass of the solid electrolyte and the oily organic binder;
(3) PVDF polymer solid electrolyte (LiClO)4The content is 35 percent), solid electrolyte, lithium cobaltate, conductive carbon black and NMP which are formed by the mixture of LATP solid electrolyte are mixed to prepare slurry to be coated on the aluminum foil, and the slurry is dried to obtain a composite positive pole piece;
(4) and (3) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece lamination obtained in the step (3), adding a small amount of TMU wetting interface between the anode and the cathode during lamination, standing for 1 hour, drying and drying the TMU, and packaging to obtain the all-solid-state battery.
Example 4
(1) PEO polymer solid electrolyte (LiN (SO)2CF3)2The content is 10%), the silicon-carbon negative electrode, the conductive carbon black, the carbon nano tube and water are mixed to prepare slurry, the slurry is coated on the copper foil, and the composite negative electrode pole piece is obtained after drying;
(2) mixing Ga-doped LLZO, PVDF and DMAC to prepare slurry, coating the slurry on the composite negative electrode plate obtained in the step (1), drying and rolling, wherein the proportion of the solid electrolyte in the total mass of the solid electrolyte and the oily organic binder is 95%;
(3) PVDF-HFP Polymer solid electrolyte (LiB (C)2O4)2The content is 25%), the solid electrolyte consisting of the mixture of the LLTO solid electrolyte, lithium-rich lithium manganate, conductive carbon black and triethyl phosphate are mixed to prepare slurry, and the slurry is coated on an aluminum foil and dried to obtain a composite positive pole piece;
(4) and (3) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece obtained in the step (3), adding a small amount of NMP between the anode and the cathode during lamination to wet an interface, standing for 0.5 hour, drying and drying the NMP, and packaging to obtain the all-solid-state battery.
Example 5
(1) PEO polymer solid electrolyte (LiPF)6 Content 40%), PEG polymer solid electrolyte (LiPF)6 Content 40%), PPO polymer solid electrolyte (LiPF)6The content of 40 percent), graphite, conductive carbon black and acetone are mixed to prepare slurry, the slurry is coated on copper foil, and the composite negative pole piece is obtained after drying;
(2) mixing LAGP, PAN polymer solid electrolyte (LiB (C)2O4)2Content of 15%) and NMP to prepare slurry, coating the slurry on the composite negative electrode plate obtained in the step (1), drying and rolling, wherein the solid electrolyte accounts for 80% of the total mass of the solid electrolyte and the oily organic binder;
(3) PAN polymer solid electrolyte (LiN (SO)2CF3)260% content) of a solid electrolyte mixture with LLTOMixing the state electrolyte, the lithium manganate, the conductive carbon black and the DMAC to prepare slurry, coating the slurry on the aluminum foil, and drying to obtain a composite positive pole piece;
(4) and (3) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece lamination obtained in the step (3), adding a small amount of DMSO (dimethyl sulfoxide) between the anode and the cathode during lamination to wet an interface, standing for a period of time, drying and drying the organic solvent, and packaging to obtain the all-solid-state battery.
Battery performance testing
The batteries prepared in examples 1 to 5 were subjected to 50 and 100 cycles of capacity retention rate tests at 60 ℃ under 0.2C conditions, and the results are shown in Table 1.
TABLE 1 conservation rate of 60 deg.C and 0.2C charge-discharge cycle capacity of all-solid-state battery
| Numbering | Capacity retention rate at 50 cycles | Capacity retention ratio of 100 cycles |
| Example 1 | 95.3％ | 93.2％ |
| Example 2 | 98.5％ | 97.1％ |
| Example 3 | 97.6％ | 95.5％ |
| Example 4 | 90.9％ | 88.7％ |
| Example 5 | 93.1％ | 90.3％ |
The embodiments described above were chosen and described in order to best explain the principles of the invention, but are not intended to be exhaustive or to limit the invention to the precise forms disclosed, and many modifications and variations are possible to those skilled in the art to best utilize the invention, the scope of which is defined by the appended claims.
Claims (4)
1. A method for preparing an all-solid-state lithium ion battery by coating solid electrolyte slurry on a negative electrode is characterized by comprising the following steps:
(1) mixing a solid electrolyte consisting of a mixture of an aqueous polymer solid electrolyte and an oxide solid electrolyte, a negative electrode active substance, an electronic conductive additive and an aqueous solvent to prepare a slurry, coating the slurry on a copper foil, and drying to obtain a composite negative electrode piece;
(2) mixing an oxide solid electrolyte, an oily organic binder and an oily solvent to prepare a slurry, coating the slurry on the composite negative electrode plate obtained in the step (1), drying and rolling, wherein the solid electrolyte accounts for 70-95% of the total mass of the solid electrolyte and the oily organic binder;
(3) mixing a solid electrolyte composed of a mixture of an oily polymer solid electrolyte and an oxide solid electrolyte, a positive active substance, an electronic conductive additive and an oily solvent to prepare a slurry, coating the slurry on an aluminum foil, and drying to obtain a composite positive pole piece;
(4) assembling the battery by using the composite cathode pole piece coated with the solid electrolyte obtained in the step (2) and the composite anode pole piece lamination obtained in the step (3), adding an oily solvent to wet an interface between the cathode and the anode during lamination, standing for 0.5-10 hours, drying and drying the oily solvent, and packaging to obtain an all-solid battery;
wherein the aqueous solvent in the step (1) is one or a mixture of water, acetonitrile, ethanol, acetone and tetrahydrofuran; the oily solvent in the steps (2) - (4) is one or a mixture of more of Dimethylformamide (DMF), Dimethylacetamide (DMAC), Tetramethylurea (TMU), dimethyl sulfoxide (DMSO), triethyl phosphate and N-methyl-2-pyrrolidone (NMP); the positive active material in the steps (1) and (3) is one or a mixture of more of lithium cobaltate, lithium manganate, nickel cobalt manganese ternary, lithium iron phosphate and nickel lithium manganate, the negative active material is one or a mixture of more of graphite, amorphous carbon, mesocarbon microbeads, nano silicon, a silicon carbon material and lithium titanate, and the electronic conductive additive is one or a mixture of more of carbon black, conductive graphite, carbon nanotubes, graphene and carbon fibers;
the aqueous polymer solid electrolyte in the step (1) is a mixture of an aqueous polymer matrix and lithium salt, the lithium salt accounts for 10% -60%, wherein the aqueous polymer matrix is one or a mixture of polyethylene oxide (PEO), polyethylene glycol (PEG) and polypropylene oxide (PPO), and the lithium salt is LiN (SO)2CF3)2、LiClO4、LiSO2CF3、LiB(C2O4)2、LiPF6And one or more of LiI;
the oxide solid electrolyte in the steps (1) - (3) is one or a mixture of more of Lithium Lanthanum Zirconium Oxide (LLZO), tantalum-doped lithium lanthanum zirconium oxide (Ta-LLZO), Lithium Lanthanum Titanium Oxide (LLTO), titanium aluminum lithium phosphate (LATP) and germanium aluminum lithium phosphate (LAGP).
2. The method for preparing an all-solid-state lithium ion battery by coating the solid electrolyte slurry on the negative electrode according to claim 1, wherein the oily polymer solid electrolyte in the step (3) is a mixture of an oily polymer matrix and a lithium salt, the lithium salt accounts for 10% -60%, wherein the oily polymer matrix isThe body is one or more of polyvinylidene fluoride (PVDF), polyvinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP) and Polyacrylonitrile (PAN) mixed, and the lithium salt is LiN (SO)2CF3)2、LiClO4、LiSO2CF3、LiB(C2O4)2、LiPF6And LiI, or a mixture of two or more of the same.
3. The method for preparing an all-solid-state lithium ion battery by coating the solid electrolyte slurry on the negative electrode according to claim 1, wherein the oily organic binder in the step (2) is one or more of PVDF, PVDF-HFP, PAN, or the oily polymer solid electrolyte in the step (3).
4. An all-solid-state lithium ion battery, characterized in that it is produced by the method according to any one of claims 1 to 3.
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| CN108232318A (en) * | 2018-01-30 | 2018-06-29 | 陕西煤业化工技术研究院有限责任公司 | A kind of production method of all solid state power lithium-ion battery |
| CN108630985A (en) * | 2018-05-11 | 2018-10-09 | 清陶（昆山）新能源材料研究院有限公司 | A kind of high ionic conductivity solid electrolyte and preparation method thereof and its application in all-solid lithium-ion battery |
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