CN105591105A - Preparation method for coating surfaces of electrodes with solid electrolyte complex liquid - Google Patents
Preparation method for coating surfaces of electrodes with solid electrolyte complex liquid Download PDFInfo
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- CN105591105A CN105591105A CN201610148968.8A CN201610148968A CN105591105A CN 105591105 A CN105591105 A CN 105591105A CN 201610148968 A CN201610148968 A CN 201610148968A CN 105591105 A CN105591105 A CN 105591105A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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- 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
- H01M10/058—Construction or manufacture
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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
- H01M4/621—Binders
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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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- H—ELECTRICITY
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- 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
- H01M4/625—Carbon or graphite
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- 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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- 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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a high-circulation lithium ion battery and a preparation method thereof, and particularly discloses a preparation method for coating the surfaces of a positive electrode and a negative electrode with solid electrolyte complex liquid and preparing a positive compound electrode and a negative compound electrode to prepare the lithium ion battery. The solid electrolyte complex liquid is mainly prepared from solid electrolyte, conductive agent, film forming agent, adhesive and solvent. The prepared positive electrode and the prepared negative electrode contain solid electrolyte compound; due to the excellent ion electric conductivity of solid electrolyte and the electronic conductivity of conductive agent, on one hand, the ion electric conductivity of the electrodes can be improved, and therefore the internal resistance of the lithium ion battery is effectively reduced; on the other hand, the electronic transmission speed and liquid absorption capacity of the battery can be increased through the electronic conductivity of conductive agent, the shrinkage rate of an adhesive in the active substance and the shrinkage rate of an adhesive in an electrolyte layer in the drying process of the electrodes are reduced to be basically the same through the film forming agent, the adhesion force between different layers of the electrodes is improved, and therefore the electrochemical performance of lithium ions is comprehensively improved.
Description
Technical field
The invention belongs to secondary cell field, compound by both positive and negative polarity pole piece surface coating solid electrolyte specificallyLiquid is prepared the cycle performance of pole piece raising lithium ion battery.
Background technology
Lithium-ion-power cell is good with its cycle life, environmental friendliness, energy density advantages of higher and be widely used in electricityThe field such as electrical automobile, energy storage, is cost but restrict the key that its lithium-ion-power cell generally applies, and affect cost because ofElement mainly contains material price, product percent of pass and battery thereof. By extending lithium ion battery be service lifeA kind of feasible, effectively reduce lithium ion battery cost method. Improve at present cycle life of lithium ion battery method a lot, mainBy adopting high performance material and material modification thereof, the design of optimization battery/pole piece and add conductive agent etc. in material, optimizeOne of pole piece method for designing is to improve lithium ion battery at the surperficial material that applies one deck raising cycle life of active materialCycle life. Such as patent (CN105098227A) discloses all solid state lithium ion battery and preparation method thereof, adopt sprayChina ink printing technique is prepared all solid state lithium ion battery, improves the conductance of lithium ion, the capacity of maximum performance active materialMatter improves its cycle performance, but this preparation method at present, poor stability immature in process aspect technology, be difficult to promote and makeWith. And if adopt at both positive and negative polarity pole piece surface coating solid electrolyte complex liquid, can bring into play its solid electrolyte excellenceThe electron conduction of ionic conductivity and conductive agent, and improve the cycle life of lithium ion battery, its method is simple, is easy to industryChange and promote.
Summary of the invention
The present invention is just based on defects such as current cycle life of lithium ion battery are poor, and object is to provide a kind of by pole pieceSurface coating solid electrolyte complex liquid with improve lithium ion battery cycle life at pole piece surface coating solid electrolyteThe preparation method of complex liquid.
Technical scheme of the present invention is achieved in the following ways: a kind of compound at pole piece surface coating solid electrolyteThe preparation method of liquid, is at positive and negative electrode pole piece surface coating solid electrolyte complex liquid, described solid electrolyte complex liquid bySolid electrolyte, conductive agent, film forming agent, binding agent and solvent composition thereof, its mass ratio is: solid electrolyte: conductive agent: film formingAgent: binding agent: solvent=1 ~ 10:1 ~ 5:0.5 ~ 2:1 ~ 10:100; It is characterized in that:
1), first take binding agent and dissolve and stir in nmp solvent, add solid electrolyte, conductive agent, film forming agent logicalAfter crossing high speed dispersor and stirring, add again solvent allotment viscosity and obtain coating liquid to 500-3000mpas;
2), by intaglio printing technology, coating liquid is coated in to the pole piece surface of iron phosphate lithium positive pole or negative pole, coating thickness is1-5 μ m, obtains the composite pole piece of negative or positive electrode after dry.
Described solid electrolyte is: LiTi2(PO4)3、Li1.3Al0.3Ti1.7(PO4)3、Li4Ge0.5V0.5O4In one.
Described film forming agent is in diglycol list alkane ether, propane diols list alkane ether, dipropylene glycol list alkane etherA kind of.
Described conductive agent is any one in CNT, Graphene, gas-phase carbon fiber, carbon black.
Described binding agent is one or both of polyacrylic acid, polypropylene cyanogen, its mass ratio: polyacrylic acid: polypropyleneCyanogen=1 ~ 9:1 ~ 9.
Described solvent is redistilled water.
The present invention, adopts solid electrolyte can improve the transfer rate of lithium ion, and film forming agent can reduce pole piece simultaneouslyIn dry run, the contraction of binding agent causes separation between layers, improves the adhesion of its pole piece interlayer, simultaneously conductionAgent can improve again electric transmission speed, and therefore improves multiplying power and the cycle performance of its lithium ion battery.
Brief description of the drawings
Fig. 1 is the cyclic curve figure that embodiment and comparative example are prepared lithium ion battery.
Detailed description of the invention
Embodiment 1:
First take 5 grams of polyacrylic acid binding agents and be dissolved in 50gNMP solvent and stir, add afterwards 5gLiTi2(PO4)3GuBody electrolyte, the agent of 3g carbon nanotube conducting, 1g diglycol list alkane ether film forming agent also stirs by high speed dispersorAdd again afterwards 50gNMP solvent allotment viscosity and finally obtain coating liquid to 2000mpas, afterwards will by intaglio printing technologyCoating liquid is coated in iron phosphate lithium positive pole pole piece surface, and coating thickness is 5 μ m, after being dried, obtains anodal composite pole piece.
Embodiment 2:
First take 1 gram of polypropylene cyanogen binding agent and be dissolved in 50gNMP solvent and stir, add afterwards 1gLi1.3Al0.3Ti1.7(PO4)3Solid electrolyte, the agent of 1g graphene conductive, 0.5g propane diols list alkane ether film forming agent also stirs by high speed dispersorAdd again afterwards 50gNMP solvent allotment viscosity and finally obtain coating liquid to 500mpas, will be coated with by intaglio printing technology afterwardsCover liquid and be coated in ternary material anode pole piece surface, coating thickness is 1 μ m, after being dried, obtains anodal composite pole piece.
Embodiment 3:
First take 5 grams of polypropylene cyanogen binding agents and 5g polyacrylic acid binding agent, and stir in molten 50gNMP solvent, afterwardsAdd 10gLi4Ge0.5V0.5O4Solid electrolyte, the agent of 5g gas phase electric conduction of carbon fiber, 2g dipropylene glycol list alkane ether film forming agent is alsoAfter stirring by high speed dispersor, add again 50gNMP solvent allotment viscosity and finally obtain coating liquid to 3000mpas,By intaglio printing technology, coating liquid is coated in to graphite cathode pole piece surface afterwards, coating thickness is 2 μ m, after being driedTo negative pole composite pole piece.
Comparative example 1: prepare anode pole piece as a comparison case 1 with the ternary material of purchasing on market;
Comparative example 2: prepare cathode pole piece as a comparison case 2 with the Delanium of purchasing on market;
(1) pattern test.
The pattern that uses the cathode pole piece making in SEM method test implementation example 1, result as shown in Figure 1.
(2) make button cell test.
By the anode slice of lithium ion battery/cathode pole piece obtaining in comparative example 1-2 and embodiment 1-3 as followsBe assembled into button cell test:
1) in 95g negative material, 1g binding agent LA132,4g conductive agent SP, add 220mL solvent redistilled water, stir allThe even cathode size of preparing, is coated on Copper Foil, dries, and roll-in makes cathode pole piece.
2) in 95g positive electrode, 1g binding agent LA132,4g conductive agent SP, add 220mL solvent redistilled water, stirMix and evenly prepare anode sizing agent, be coated on aluminium foil, dry, roll-in makes anode pole piece.
Electrolyte uses LiPF6For electrolyte, concentration is 1.3mol/L, and the EC that volume ratio is 1:1 and DEC are solvent, goldBelong to lithium sheet as to electrode, barrier film adopts polyethylene (PE), and polypropylene (PP) or poly-second propylene (PEP) composite membrane, filling hydrogenGlove box according to existing method assembling button cell. The lithium ion battery obtaining in comparative example 1-2 and embodiment 1-3 respectivelyBe numbered B1, B2, A1, A2, A3.
2) above-mentioned button cell is tested on new prestige 5V/10mA type cell tester to charging/discharging voltage scope 0.005-2.0V(negative plate), 2.5-3.65V (positive plate), charge-discharge magnification 0.1C, test result is as shown in table 1.
Table 1: button cell test result
| Detain battery | B1 | B2 | A1 | A2 | A3 |
| Discharge capacity (mAh/g) first | 153.9 | 365.4 | 158.9 | 159.9 | 360.3 |
| Efficiency (%) first | 97.1 | 94.8 | 97.3 | 98.1 | 94.1 |
Note: efficiency=discharge capacity/initial charge capacity first first in table.
(3) make soft-package battery test.
A) respectively using the anode slice of lithium ion battery that makes in comparative example 1 anode pole piece and embodiment 1-2 as positive poleMaterial, taking LiFePO 4 material as positive electrode, electrolyte uses LiPF6For electrolyte, concentration is 1.3mol/L, and volume ratio isThe EC of 1:1 and DEC are solvent, and barrier film uses Celgard2400 film, utilizes prior art to prepare 5Ah soft-package battery, contrastLithium ion battery in example 1 and embodiment 1-2 is numbered B1, A1, A2.
Respectively using the lithium ion battery negative electrode that makes in comparative example 2 cathode pole pieces and embodiment 3 as negative material,Taking graphite material as negative material, electrolyte uses LiPF6For electrolyte, concentration is 1.3mol/L, the EC that volume ratio is 1:1 andDEC is solvent, and barrier film uses Celgard2400 film, utilizes prior art to prepare 5Ah soft-package battery, comparative example 1 and enforcementLithium ion battery in example 1-2 is numbered B2, A3.
B) test high rate performance and the cycle performance of above-mentioned soft-package battery, wherein high rate performance is tested respectively it and is filled at 0.3CPerformance with 0.5C, 1.0C, 2.0C, 4.0C, 8.0C multiplying power discharging respectively after electricity, and test it with 2.0C charging, 2.0C electric discharge,The capability retention circulating after 500 times, result is as shown in table 2.
Table 2: soft-package battery test result
As can be seen from Table 1, adopt the button cell of embodiment 1～3 gained, its discharge capacity and efficiency are all apparently higher than contrastExample, shows can improve at its material surface coating solid electrolyte discharge capacity and the efficiency of battery. As can be seen from Table 2,The high rate performance of the soft-package battery that embodiment 1-3 prepares and cycle performance are obviously better than the soft-package battery of comparative example, its reasonImprove the cycle performance under its large multiplying power condition for solid electrolyte can provide more lithium ion, solid electrolyte is coated with simultaneouslyOverlay on active material surface and can improve again the stability of material surface structure.
Claims (6)
1. in a preparation method for pole piece surface coating solid electrolyte complex liquid, be to apply solid on positive and negative electrode pole piece surfaceBody electrolyte complex liquid, described solid electrolyte complex liquid is by solid electrolyte, conductive agent, film forming agent, binding agent and moltenAgent composition, its mass ratio is: solid electrolyte: conductive agent: film forming agent: binding agent: solvent=1 ~ 10:1 ~ 5:0.5 ~ 2:1 ~ 10:100; It is characterized in that:
1), first take binding agent and dissolve and stir in nmp solvent, add solid electrolyte, conductive agent, film forming agent logicalAfter crossing high speed dispersor and stirring, add again solvent allotment viscosity and obtain coating liquid to 500-3000mpas;
2), by intaglio printing technology, coating liquid is coated in to the pole piece surface of iron phosphate lithium positive pole or negative pole, coating thickness is1-5 μ m, obtains the composite pole piece of negative or positive electrode after dry.
2. a kind of preparation method at pole piece surface coating solid electrolyte complex liquid according to claim 1, its featureBe: described solid electrolyte is: LiTi2(PO4)3、Li1.3Al0.3Ti1.7(PO4)3、Li4Ge0.5V0.5O4In one.
3. a kind of preparation method at pole piece surface coating solid electrolyte complex liquid according to claim 1, its featureBe: described conductive agent is any one in CNT, Graphene, gas-phase carbon fiber, carbon black.
4. a kind of preparation method at pole piece surface coating solid electrolyte complex liquid according to claim 1, its featureBe: described film forming agent is one in diglycol list alkane ether, propane diols list alkane ether, dipropylene glycol list alkane etherKind.
5. a kind of preparation method at pole piece surface coating solid electrolyte complex liquid according to claim 1, its featureBe: described binding agent is one or both of polyacrylic acid, polypropylene cyanogen, its mass ratio: polyacrylic acid: polypropylene cyanogen=1~9：1~9。
6. a kind of preparation method at pole piece surface coating solid electrolyte complex liquid according to claim 1, its featureBe: described solvent is redistilled water.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105977522A (en) * | 2016-07-04 | 2016-09-28 | 深圳博磊达新能源科技有限公司 | Composite coating for improving high-temperature performance of lithium-ion battery, composite negative plate, preparation method of composite negative plate and lithium-ion battery |
| CN106099115A (en) * | 2016-08-19 | 2016-11-09 | 洛阳力容新能源科技有限公司 | Lithium ion battery combined conductive agent, lithium ion battery composite guide are electro-hydraulic and preparation method thereof, lithium ion battery |
| CN107591529A (en) * | 2017-10-10 | 2018-01-16 | 中南大学 | A kind of titanium phosphate lithium cladding nickel-cobalt-manganternary ternary anode material and preparation method thereof |
| CN108735972A (en) * | 2017-04-21 | 2018-11-02 | 日立化成株式会社 | The manufacturing method of secondary cell battery components |
| CN109273760A (en) * | 2018-09-30 | 2019-01-25 | 淮安新能源材料技术研究院 | A kind of lithium ion cell electrode piece and coating method with solid-state electrolyte layer |
| CN110556514A (en) * | 2019-09-09 | 2019-12-10 | 江西中汽瑞华新能源科技有限公司 | Preparation method of all-solid-state lithium ion battery |
| CN112670592A (en) * | 2019-10-16 | 2021-04-16 | 北京卫蓝新能源科技有限公司 | Pole piece and diaphragm compounding process and lithium battery cell preparation process |
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| CN103022415A (en) * | 2011-09-26 | 2013-04-03 | 比亚迪股份有限公司 | Positive pole, preparation method thereof and lithium-ion battery |
| CN105186032A (en) * | 2015-10-19 | 2015-12-23 | 东莞市凯欣电池材料有限公司 | High-voltage lithium-ion battery electrolyte and lithium-ion battery using high-voltage lithium-ion battery electrolyte |
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Patent Citations (2)
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| CN103022415A (en) * | 2011-09-26 | 2013-04-03 | 比亚迪股份有限公司 | Positive pole, preparation method thereof and lithium-ion battery |
| CN105186032A (en) * | 2015-10-19 | 2015-12-23 | 东莞市凯欣电池材料有限公司 | High-voltage lithium-ion battery electrolyte and lithium-ion battery using high-voltage lithium-ion battery electrolyte |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105977522A (en) * | 2016-07-04 | 2016-09-28 | 深圳博磊达新能源科技有限公司 | Composite coating for improving high-temperature performance of lithium-ion battery, composite negative plate, preparation method of composite negative plate and lithium-ion battery |
| CN105977522B (en) * | 2016-07-04 | 2019-02-12 | 深圳博磊达新能源科技有限公司 | It is a kind of to improve the composite coating of high-temperature lithium ion battery performance, composite negative plate and preparation method thereof, lithium ion battery |
| CN106099115A (en) * | 2016-08-19 | 2016-11-09 | 洛阳力容新能源科技有限公司 | Lithium ion battery combined conductive agent, lithium ion battery composite guide are electro-hydraulic and preparation method thereof, lithium ion battery |
| CN106099115B (en) * | 2016-08-19 | 2018-12-18 | 洛阳力容新能源科技有限公司 | Lithium ion battery combined conductive agent, lithium ion battery composite guide be electro-hydraulic and preparation method thereof, lithium ion battery |
| CN108735972A (en) * | 2017-04-21 | 2018-11-02 | 日立化成株式会社 | The manufacturing method of secondary cell battery components |
| CN107591529A (en) * | 2017-10-10 | 2018-01-16 | 中南大学 | A kind of titanium phosphate lithium cladding nickel-cobalt-manganternary ternary anode material and preparation method thereof |
| CN109273760A (en) * | 2018-09-30 | 2019-01-25 | 淮安新能源材料技术研究院 | A kind of lithium ion cell electrode piece and coating method with solid-state electrolyte layer |
| CN110556514A (en) * | 2019-09-09 | 2019-12-10 | 江西中汽瑞华新能源科技有限公司 | Preparation method of all-solid-state lithium ion battery |
| CN112670592A (en) * | 2019-10-16 | 2021-04-16 | 北京卫蓝新能源科技有限公司 | Pole piece and diaphragm compounding process and lithium battery cell preparation process |
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