CN112421100A - Preparation method and application of glued solid electrolyte membrane - Google Patents
Preparation method and application of glued solid electrolyte membrane Download PDFInfo
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- CN112421100A CN112421100A CN201910774299.9A CN201910774299A CN112421100A CN 112421100 A CN112421100 A CN 112421100A CN 201910774299 A CN201910774299 A CN 201910774299A CN 112421100 A CN112421100 A CN 112421100A
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- 239000012528 membrane Substances 0.000 title claims abstract description 42
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000004026 adhesive bonding Methods 0.000 claims description 8
- 239000000084 colloidal system Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011247 coating layer Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- -1 polypropylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 238000004513 sizing Methods 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000002203 sulfidic glass Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims 1
- 238000007731 hot pressing Methods 0.000 abstract description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 7
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 7
- 239000003292 glue Substances 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
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Classifications
-
- 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
-
- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0407—Methods of deposition of the material by coating on an electrolyte layer
-
- 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
-
- 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
- H01M2300/0088—Composites
- H01M2300/0094—Composites in the form of layered products, e.g. coatings
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a preparation method and application of a gummed solid electrolyte membrane, and particularly relates to a method for coating a layer of glue layer on the surface of a solid electrolyte membrane, wherein the material of the gummed layer can conduct lithium ions when a battery is charged and discharged, and then the gummed solid electrolyte membrane is wound (or laminated) with a positive plate and a negative plate of the battery to form a bare cell and then is subjected to hot-pressing adhesion. The invention effectively improves the ionic conductivity between the solid electrolyte membrane of the solid lithium ion battery and the anode and cathode plates, and the internal resistance and the cycle performance of the solid lithium ion battery manufactured by the coating solid electrolyte membrane and the application process method thereof are obviously improved.
Description
Technical Field
The invention relates to the technical field of solid lithium ion batteries, in particular to a preparation method and application of a gummed solid electrolyte membrane.
Background
The development of pure electric vehicles is always restricted by low energy density of batteries. The energy density of the battery is not greatly broken through, and the endurance mileage of the pure electric vehicle cannot be greatly improved. At present, the single energy density of the ternary lithium battery is close to the limit, and the specific gravity of nickel in the battery needs to be further improved in order to further improve the energy density of the ternary lithium battery. However, when the specific gravity of nickel in the battery is increased, the thermal stability of high nickel is poor, so that the thermal reaction inside the battery is very severe, and thus safety problems are worried. By means of a ternary lithium battery technical route, the energy density of the power battery is required to reach the target of 350Wh/kg, and the difficulty is high. Because the solid-state battery has no liquid electrolyte, is nonflammable, non-corrosive, nonvolatile, has good performance at high temperature and higher safety, the technical problem of further improving the energy density and the safety performance of the battery by the solid-state battery is urgently needed to be solved in the field. However, the solid-state battery has technical challenges in terms of battery internal resistance and cycle life because the internal resistance of the interface contact between the electrolyte of the solid-state battery and the positive and negative electrode sheets is large.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a preparation method of a gummed solid electrolyte membrane, and the electrolyte membrane obtained by the method has the advantages of more compact solid-solid contact between a glue layer and a base membrane layer, higher ionic conductivity and more excellent performance in batteries.
The technical scheme of the invention is as follows:
a preparation method of a gummed solid electrolyte membrane comprises the following steps:
s1, dissolving the colloid main material in a required solvent, and mixing to obtain uniform gluing slurry;
and S2, coating the gluing slurry on the upper surface and the lower surface of the solid electrolyte membrane, and drying to obtain the gluing solid electrolyte membrane.
Preferably, the colloidal main material of the gummed slurry in S1 is one or more of polyvinylidene fluoride, polypropylene, polymethyl methacrylate and polyethylene oxide polymer.
Preferably, the solvent required by the sizing slurry in S1 is one or more of dimethylformamide, dimethyl sulfoxide, dichloromethane, N-methylpyrrolidone and deionized water.
Preferably, the mass ratio of the colloid main material to the solvent is 5-10: 100.
Preferably, a dispersing agent is also added into the S1, the dispersing agent is one or two of polyvinylpyrrolidone and sodium carboxymethyl cellulose, and the dispersing agent accounts for 0.5% of the weight of the main colloid material.
Preferably, the solid electrolyte membrane used in S2 is any one of a polymer, oxide, sulfide solid electrolyte membrane.
Preferably, in S2, a tape casting type, spraying type or gravure type coating device is adopted to carry out double-sided coating on the solid electrolyte membrane, and the thickness of a single coating layer is 0.2-10 μm; the drying temperature is 35-70 ℃.
The invention also provides application of the battery cell prepared by the method, and specifically the method further comprises the following steps:
and S3, winding or laminating the coated solid electrolyte membrane, the positive electrode plate and the negative electrode plate together to form a naked battery cell, and then carrying out hot-press bonding on the naked battery cell to obtain a final battery cell finished product.
Preferably, the hot-pressing bonding mode in S3 is air cylinder pressing plate type hot-pressing bonding, the pressure is 0.2-1.0 MPa, the pressing plate temperature is 60-110 ℃, and the hot-pressing pressure is maintained for 20-100S.
The material of the glue coating layer can conduct lithium ions when the battery is charged and discharged, and can effectively conduct the lithium ions between the solid electrolyte membrane and the anode and cathode pole pieces. The solid electrolyte membrane coated with the glue layer can be tightly adhered to the positive pole piece and the negative pole piece under the high-temperature hot-pressing condition, so that the ionic conductivity between the solid electrolyte membrane and the positive pole piece and the negative pole piece is greatly improved, and further, the cycle performance of the solid lithium ion battery is improved.
Description of the drawings:
FIG. 1 is a schematic view of a rubberized solid electrolyte membrane according to the invention;
fig. 2 is a schematic view of the hot-press bonding of bare cells according to the present invention;
FIG. 3 is a graph of a battery capacity cycling test according to an embodiment of the present invention;
in the figure, 1-solid electrolyte membrane, 2-glue coating layer, 3-naked electric core, 4-upper hot pressing plate, 5-lower hot pressing plate and 6-pressure cylinder.
The specific implementation mode is as follows:
example 1
A preparation method of a gummed solid electrolyte membrane comprises the following steps:
dissolving polymethyl methacrylate and polyethylene oxide colloid main materials in a mass ratio of 1:2 into a mixed solvent of dichloromethane and dimethylformamide in a mass ratio of 1:1, and performing mixed stirring for 60-300 min by using a 50L volume planetary stirrer to perform revolution at 30rpm and disperse at 1200 rpm.
And adding 0.5 mass percent (relative to the main colloid material) of polyvinylpyrrolidone dispersing agent into the mixed slurry, and performing revolution at 30rpm and dispersion at 1200rpm for mixing and stirring for 30-90 min to obtain the low-viscosity (viscosity is 50-500cp) non-Newtonian fluid gluing slurry.
Coating the gluing slurry on the surfaces (upper surface and lower surface) of the solid electrolyte membrane by using a gravure coater, and drying by using a drying channel oven at 35-70 ℃ to obtain the glued solid electrolyte membrane, as shown in figure 1.
And winding the coated solid electrolyte membrane, a positive pole piece and a negative pole piece (the positive pole is LNCM523, and the negative pole is artificial graphite) into a naked battery cell (the theoretical design capacity of the battery cell is 6.5Ah) according to the lamination sequence of the coated solid electrolyte membrane, the positive pole piece, the coated solid electrolyte membrane and the negative pole piece.
Placing the bare cell in a hot-pressing board clamping groove of a hot-pressing device, and carrying out hot-pressing adhesion by using parameters of 85 ℃, 0.8MPa and 40s to obtain a tightly and hard wound cell in which the adhesive-coated solid electrolyte membrane is adhered to the positive and negative pole pieces, as shown in figure 2.
And (3) finishing the manufacture of a battery finished product (the battery is finally charged to 3.850V by using a 0.5C constant current and a constant voltage) by the steps of tab welding, external packaging treatment, high-temperature baking, pre-packaging, standing, formation, degassing, packaging, aging and capacity grading test.
The OCV, ACR, capacity of the battery in the above embodiment 1 were measured, see table 1.
3 normal cells from example 1 were selected for 0.5C/0.5C capacity cycling tests, see FIG. 3.
Comparative example 1
The conventional (non-coated) solid electrolyte membrane was used to prepare the cell, with the following steps:
the solid electrolyte membrane without glue coating and positive and negative pole pieces (the positive pole is LNCM523, the negative pole is artificial graphite) are wound into a naked cell (the theoretical design capacity of the cell is 6.5Ah) according to the lamination sequence of the solid electrolyte membrane, the positive pole piece, the solid electrolyte membrane and the negative pole piece.
Placing the naked electric core in a hot pressing plate clamping groove of hot pressing equipment, performing hot pressing adhesion by using parameters of 85 ℃, 0.8MPa and 40s, wherein the electric core after hot pressing is basically unchanged from the electric core before hot pressing.
And (3) finishing the manufacture of a battery finished product (the battery is finally charged to 3.850V by using a 0.5C constant current and a constant voltage) by the steps of tab welding, external packaging treatment, high-temperature baking, pre-packaging, standing, formation, degassing, packaging, aging and capacity grading test.
The OCV, ACR, capacity of the cell of comparative example 1 above was tested and is shown in table 1.
3 normal cells of comparative example 1 above were selected for 0.5C/0.5C capacity cycling tests, see FIG. 3.
Table 1: example 1 and example 2 cell OCV, ACR/capacity test data.
The above embodiment is one of the embodiments implemented in the scope of the present invention, and any other hot press bonding processes (including but not limited to) using the gummed slurry made of various materials with other compounding ratios derived from the various materials described in the scope of the present invention, and other process parameters derived from the hot press bonding process method described in the present invention belong to the scope of the present invention.
Claims (10)
1. The preparation method of the gummed solid electrolyte membrane is characterized by comprising the following steps:
s1, dissolving the colloid main material in a required solvent, and mixing to obtain uniform gluing slurry;
and S2, coating the gluing slurry on the upper surface and the lower surface of the solid electrolyte membrane, and drying to obtain the gluing solid electrolyte membrane.
2. The method according to claim 1, wherein the colloidal host material of the gummed slurry in S1 is one or more of polyvinylidene fluoride, polypropylene, polymethyl methacrylate and polyethylene oxide polymer.
3. The preparation method according to claim 1, wherein the solvent required by the sizing slurry in S1 is one or more of dimethylformamide, dimethyl sulfoxide, dichloromethane, N-methylpyrrolidone and deionized water.
4. The preparation method according to claim 1, wherein the mass ratio of the colloid main material to the solvent is 5-10: 100.
5. The preparation method according to claim 1, wherein a dispersant is further added to S1, the dispersant is one or both of polyvinylpyrrolidone and sodium carboxymethylcellulose, and the dispersant accounts for 0.5% of the weight of the colloidal main material.
6. The production method according to claim 1, wherein the solid electrolyte membrane used in S2 is any one of a polymer, an oxide, and a sulfide solid electrolyte membrane.
7. The preparation method according to claim 1, wherein in S2, a casting type, spraying type or gravure type coating device is used for double-sided coating of the solid electrolyte membrane, and the thickness of a single coating layer is 0.2-10 μm; the drying temperature is 35-70 ℃.
8. Use of a solid electrolyte membrane prepared according to any of claims 1 to 7 in the preparation of a cell.
9. The use according to claim 8, further comprising the steps of:
and S3, winding or laminating the coated solid electrolyte membrane, the positive electrode plate and the negative electrode plate together to form a naked battery cell, and then carrying out hot-press bonding on the naked battery cell to obtain a final battery cell finished product.
10. The use according to claim 9, wherein the thermocompression bonding in S3 is a cylinder platen thermocompression bonding, the pressure is 0.2-1.0 MPa, the platen temperature is 60-110 ℃, and the thermocompression pressure is maintained for 20-100S.
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| CN201910774299.9A CN112421100A (en) | 2019-08-21 | 2019-08-21 | Preparation method and application of glued solid electrolyte membrane |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998037589A1 (en) * | 1997-02-21 | 1998-08-27 | Motorola Inc. | Polymeric electrolyte and electrochemical cell using same |
| US20130136999A1 (en) * | 2002-10-30 | 2013-05-30 | Nissan Motor Co., Ltd. | Polymer battery and related method |
| CN104617255A (en) * | 2007-03-29 | 2015-05-13 | Tdk株式会社 | Full solid lithium ion secondary battery and manufacturing method thereof |
| CN106450482A (en) * | 2016-12-09 | 2017-02-22 | 中国电子新能源（武汉）研究院有限责任公司 | Method for manufacturing all-solid soft-packaged lithium ion battery |
| CN107492681A (en) * | 2017-08-09 | 2017-12-19 | 上海纳晓能源科技有限公司 | Solid electrolyte film and preparation method thereof |
| CN107732297A (en) * | 2017-10-13 | 2018-02-23 | 中国科学院青岛生物能源与过程研究所 | A kind of high voltage withstanding multilevel hierarchy composite solid electrolyte applied to lithium battery |
| CN110556574A (en) * | 2019-08-12 | 2019-12-10 | 北京协同创新研究院 | Multilayer solid electrolyte, preparation method thereof, solid battery and electronic equipment |
-
2019
- 2019-08-21 CN CN201910774299.9A patent/CN112421100A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998037589A1 (en) * | 1997-02-21 | 1998-08-27 | Motorola Inc. | Polymeric electrolyte and electrochemical cell using same |
| US20130136999A1 (en) * | 2002-10-30 | 2013-05-30 | Nissan Motor Co., Ltd. | Polymer battery and related method |
| CN104617255A (en) * | 2007-03-29 | 2015-05-13 | Tdk株式会社 | Full solid lithium ion secondary battery and manufacturing method thereof |
| CN106450482A (en) * | 2016-12-09 | 2017-02-22 | 中国电子新能源（武汉）研究院有限责任公司 | Method for manufacturing all-solid soft-packaged lithium ion battery |
| CN107492681A (en) * | 2017-08-09 | 2017-12-19 | 上海纳晓能源科技有限公司 | Solid electrolyte film and preparation method thereof |
| CN107732297A (en) * | 2017-10-13 | 2018-02-23 | 中国科学院青岛生物能源与过程研究所 | A kind of high voltage withstanding multilevel hierarchy composite solid electrolyte applied to lithium battery |
| CN110556574A (en) * | 2019-08-12 | 2019-12-10 | 北京协同创新研究院 | Multilayer solid electrolyte, preparation method thereof, solid battery and electronic equipment |
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