CN104425846A - Method for preparing lithium secondary battery and lithium secondary battery prepared with method - Google Patents

Method for preparing lithium secondary battery and lithium secondary battery prepared with method Download PDF

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Publication number
CN104425846A
CN104425846A CN201410167785.1A CN201410167785A CN104425846A CN 104425846 A CN104425846 A CN 104425846A CN 201410167785 A CN201410167785 A CN 201410167785A CN 104425846 A CN104425846 A CN 104425846A
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lithium secondary
secondary battery
electrode
electrode assemblie
preparation
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CN104425846B (en
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宋治勋
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Samsung SDI Co Ltd
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Samsung SDI Co Ltd
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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
    • 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
    • H01M10/0585—Construction or manufacture of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators
    • 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
    • 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
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings, jackets or wrappings of a single cell or a single battery
    • H01M50/116—Primary casings, jackets or wrappings of a single cell or a single battery characterised by the material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings, jackets or wrappings of a single cell or a single battery
    • H01M50/116—Primary casings, jackets or wrappings of a single cell or a single battery characterised by the material
    • H01M50/124—Primary casings, jackets or wrappings of a single cell or a single battery characterised by the material having a layered structure
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/46—Separators, membranes or diaphragms characterised by their combination with electrodes
    • H01M50/461—Separators, membranes or diaphragms characterised by their combination with electrodes with adhesive layers between electrodes and separators
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention provides a method for preparing a lithium secondary battery and the lithium secondary battery prepared with the method. The method prepares the lithium secondary battery through at least two times of ageing process circulation for a stacked electrode assembly with injected electrolyte. The method comprises a step of performing at least one time of hot press process circulation at the temperature of 95 DEG C or above on the electrode assembly between the ageing process circulations.

Description

The method preparing lithium secondary battery and the lithium secondary battery using the method to prepare
The cross reference of related application
This application claims the rights and interests of No. 10-2013-0099878th, the korean patent application submitted on August 22nd, 2013 to Korean Intellectual Property Office, its full content is incorporated herein by reference.
Technical field
One or more execution mode of the present invention relates to the method preparing lithium secondary battery and the lithium secondary battery using described method to prepare.
Background technology
Comprise personal digital assistant for being used in, mobile phone increases for the demand of information with the secondary cell in the electronic apparatus communicated and electric bicycle or electric automobile rapidly with notebook computer, and according to manufacturing the trend of compact size and lightweight electronic installation, can be compact, lightweight and can the lithium secondary battery that recharges of high power capacity just in commercialization.
Lithium secondary battery all types of in, lithium ion polymer battery receives significant concern.The size and dimension of lithium ion polymer battery can freely control, and the energy density of the Unit Weight of lithium ion polymer battery is high.In order to make these features of lithium ion polymer battery maximize, usually use pouch-type lithium ion polymer battery.
But, detect as fail safe, when being heated at 130 DEG C or higher temperature detection, due to the generation of gas in pouch-type lithium ion polymer battery, the distortion of the electrode assemblie reeled with the shape of film may occur, thus can short circuit be caused.Equally, the dividing plate be included in electrode assemblie can shrink on MD direction or TD direction, thus can occur hard short circuit or micro-short circuit (fine short).
Therefore, the method manufacturing the lithium secondary battery of the fail safe with improvement by preventing the contraction of the dividing plate comprised in electrode assemblie and the lithium secondary battery using described method to manufacture still is needed.
Summary of the invention
One or more execution mode of the present invention comprises the method that preparation has the lithium secondary battery of the fail safe of improvement.
One or more execution mode of the present invention comprises the lithium secondary battery using described method to prepare.
In the following description part will be illustrated other side, and to a certain extent, will become obvious by these aspects of specification, or these aspects are understood by implementing the execution mode that presents herein.
According to one or more execution mode of the present invention, the method preparing lithium secondary battery comprises by arranging the first electrode, the second electrode and the dividing plate between described first electrode and described second electrode and prepares electrode assemblie; Stacking described electrode assemblie also injects electrolyte in described stacking electrode assemblie; On the described stacking electrode assemblie being injected with described electrolyte, at least twice-aged process (aging process is carried out with passing through, ageing process) circulate and prepare lithium secondary battery, wherein, described prepare lithium secondary battery be included in described ageing process circulation between carry out under 95 DEG C or higher temperature on described electrode assemblie at least one times hot pressing circulation.
In one embodiment, at about 200kgf/cm 2to about 500kgf/cm 2described hot pressing is carried out under pressure in scope.
In one embodiment, at the temperature within the scope of about 95 DEG C to about 120 DEG C and about 250kgf/cm 2to about 450kgf/cm 2described hot pressing is carried out under pressure in scope.
In one embodiment, described hot pressing carries out about 100 seconds to about 180 seconds.
In one embodiment, at room temperature described ageing process is carried out.
In one embodiment, in the preparation of described electrode assemblie, described dividing plate is included in the polymer coating at least one surface of substrate.
In one embodiment, in the preparation of described electrode assemblie, described polymer coating comprises the polymer based on fluorine or the copolymer based on fluorine.
In one embodiment, the described polymer based on fluorine comprises Kynoar.
In one embodiment, the described copolymer based on fluorine is for being selected from least one in the group that is made up of Kynoar-hexafluoropropylene (PVdF-HFP) copolymer, Kynoar-polytetrafluoroethylene (PVdF-PTFE) copolymer and Kynoar-polytetrafluoroethylene-hexafluoropropylene (PVdF-PTFE-HFP) copolymer
In one embodiment, described electrolyte is organic electrolyte.
According to one or more execution mode of the present invention, provide the lithium secondary battery using described method to prepare.
In one embodiment, described lithium secondary battery can be pouch-type battery.
Accompanying drawing explanation
By in the following explanation of execution mode by reference to the accompanying drawings, these and/or other side will become obvious and be easier to understand, wherein:
Fig. 1 illustrates the flow chart preparing the method for lithium secondary battery according to the embodiment of the present invention;
Fig. 2 is the diagrammatic cross-sectional view of the electrode assemblie prepared according to the embodiment of the present invention;
Fig. 3 illustrates that the lithium secondary battery of preparation in embodiment 1 is heated the figure of the result detected after the charge/discharge of standard at the temperature of 130 DEG C;
Fig. 4 illustrates that the lithium secondary battery of preparation in comparative example 1 is heated the figure of the result detected after the charge/discharge of standard at the temperature of 130 DEG C;
Fig. 5 illustrates that the lithium secondary battery of preparation in comparative example 2 is heated the figure of the result detected after the charge/discharge of standard at the temperature of 130 DEG C;
Fig. 6 is after standard charging/electric discharge, keeps about 1 hour and the optical microscope image of the lithium secondary battery prepared in the embodiment 1 of decomposing at the temperature of 130 DEG C.
Embodiment
Hereafter by the method preparing lithium secondary battery explained according to the embodiment of the present invention and the lithium secondary battery using described method to prepare.Present will in detail with reference to each execution mode, embodiment is shown in the drawings, and wherein, Reference numeral identical in the whole text refers to identical key element.In this respect, present embodiment can have different forms, and should not be construed as the explanation being limited to and proposing here.Therefore, below by means of only describing these execution modes with reference to the accompanying drawings to explain each side of this specification.As used herein, term "and/or" comprises any of one or more relevant Listed Items and all combinations.When the expression of such as " at least one (one) " is after a series of key element, is modify permutation key element, instead of modifies the single key element in these row.
According to the embodiment of the present invention, provide the method preparing lithium secondary battery, wherein, described method comprises by arranging the first electrode, the second electrode and the dividing plate between described first electrode and the second electrode and prepares electrode assemblie; Stacking described electrode assemblie also injects electrolyte in described stacking electrode assemblie; Lithium secondary battery is prepared with by carrying out the circulation of at least twice-aged process on the described stacking electrode assemblie being injected with described electrolyte, wherein, described prepare lithium secondary battery be included in described ageing process circulation between carry out under 95 DEG C or higher temperature on described electrode assemblie at least one times hot pressing circulation.
The dividing plate such as polyolefin be used in electrode assemblie can shrink under specific higher temperature, and the bonding strength thus between the first electrode and the second electrode can weaken.Equally, there will be safety issue, such as, short circuit in lithium secondary battery.
As shown in Figure 1, the method preparing lithium secondary battery prepares lithium secondary battery by carrying out the circulation of at least twice-aged process on the stacking electrode assemblie being injected with electrolyte, wherein, on described stacking electrode assemblie, the hot pressing of at least one circulation can be carried out under 95 DEG C or higher temperature between described ageing process circulation, therefore the bonding strength between the first electrode and the second electrode can strengthen, to improve intensity and the fail safe of lithium secondary battery.
Can at about 200kgf/cm 2to about 500kgf/cm 2described hot pressing is carried out under pressure in scope.Such as, can at the temperature within the scope of about 95 DEG C to about 120 DEG C and about 250kgf/cm 2to about 450kgf/cm 2described hot pressing is carried out under pressure in scope.Described hot pressing can carry out about 100 seconds to about 180 seconds, preferably carries out about 100 seconds to about 150 seconds.
Hereinafter, the method preparing lithium secondary battery according to the embodiment of the present invention will be described.
First, electrode assemblie 10 is prepared.Fig. 2 is the diagrammatic cross-sectional view of the electrode assemblie 10 prepared according to the embodiment of the present invention.
Electrode assemblie 10 is prepared by the dividing plate 16 arranging the first electrode 11, second electrode 15 and arrange between the first electrode 11 and the second electrode 15.The polymer coating 12 and 14 that dividing plate 16 can comprise substrate 13 and be formed on two surfaces of substrate 13.
First electrode 11 is positive electrode, and this first electrode 11 can be prepared as the first battery lead plate as positive electrode plate.
Preparation first electrode as described below: prepare positive electrode active compound composition by mixed cathode active material, electric conducting material, jointing material and solvent.The first battery lead plate it being formed with positive electrode active material layer is prepared by direct coating on aluminium electrode base board and dry positive electrode active compound composition.Or positive electrode active compound composition may be cast on independent supporter, and can be laminated on aluminium electrode base board from the positive electrode active material films that above support is peeled off, to prepare the first battery lead plate it being formed with described positive electrode active material layer.First battery lead plate can be cut into suitable size to prepare the first electrode 11.
Any material usually used in this field can be used for positive active material, but especially, can use and reversibly can embed the compound with deintercalate lithium ions.Be in particular the metal being selected from cobalt, manganese, nickel and their combination, or be selected from containing at least one in the compound of lithium.The example of the described compound containing lithium comprises by being selected from Li aa 1-bb1 bd 2(0.90≤a≤1.8,0≤b≤0.5); Li ae 1-bb1 bo 2-cd c(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05); LiE 2-bb1 bo 4-cd c(0≤b≤0.5,0≤c≤0.05); Li ani 1-b-cco bb1 cd α(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05,0< α≤2); Li ani 1-b-cco bb1 co 2-αf1 α(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05,0< α <2); Li ani 1-b-cco bb1 co 2-αf1 2(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05,0< α <2); Li ani 1-b-cmn bb1 cd α(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05,0< α≤2); Li ani 1-b-cmn bb1 co 2-αf1 α(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05,0< α <2); Li ani 1-b-cmn bb1 co 2-αf1 2(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.05,0< α <2); Li ani be cg do 2(0.90≤a≤1.8,0≤b≤0.9,0≤c≤0.5,0.001≤d≤0.1); Li ani bco cmn dg eo 2(0.90≤a≤1.8,0≤b≤0.9,0≤c≤0.5,0≤d≤0.5,0.001≤e≤0.1); Li aniG bo 2(0.90≤a≤1.8,0.001≤b≤0.1); Li acoG bo 2(0.90≤a≤1.8,0.001≤b≤0.1); Li amnG bo 2(0.90≤a≤1.8,0.001≤b≤0.1); Li amn 2g bo 4(0.90≤a≤1.8,0.001≤b≤0.1); LiQO 2; LiQS 2; LiV 2o 5; LiZO 2; LiNiVO 4; Li (3-f)j 2(PO 4) 3(0≤f≤2); Li (3-f)fe 2(PO 4) 3(0≤f≤2); And LiFePO 4the compound of chemical formulation.And the example of described positive active material comprises LiMn 2o 4, LiNi 2o 4, LiCoO 2, LiNiO 2, LiMnO 2, Li 2mnO 3, LiFePO 4and LiNi xco yo 2(0<x≤0.15,0<y≤0.85).
In superincumbent chemical formula, A is Ni, Co, Mn or their combination; B1 is Al, Ni, Co, Mn, Cr, Fe, Mg, Sr, V, rare earth element or their combination; D is O, F, S, P or their combination; E is Co, Mn or their combination; F1 is F, S, P or their combination; G is Al, Cr, Mn, Fe, Mg, La, Ce, Sr, V or their combination; Q is Ti, Mo, Mn or their combination; Z is Cr, V, Fe, Sc, Y or their combination; And J is V, Cr, Mn, Co, Ni, Cu or their combination.
Described compound can have coating, or described compound and the cated compound of described tool can be in conjunction with.Described coating can comprise coating element compound, such as, be coated with the oxide of element, hydroxide, the hydroxyl carbonate of the oxyhydroxide of coating element, the carbonic acid oxonium salt of coating element or coating element.Formed that the compound of coating can be amorphous or crystallization.The example comprising coating element in the coating comprises Mg, Al, Co, K, Na, Ca, Si, Ti, V, Sn, Ge, Ga, B, As, Zr and their mixture.Coating forming procedure can be not cause the mode of negative effect on described compound, be coated with any coating process (such as spraying, impregnating) of described element to the performance of positive active material, because those of ordinary skill in the art know this process, so omit the detailed description of described process.
The example of electric conducting material comprises carbon black, graphite granule, native graphite, Delanium, acetylene black, Ketjen black, carbon fiber, carbon nano-tube; The metal dust of copper, nickel, aluminium or silver, metallic fiber or metal tube; And conducting polymer, such as polypheny lene derivatives, but be not limited thereto, and any electric conducting material as known in the art can be used.
The example of jointing material comprises vinylidene fluoride/hexafluoropropylene copolymer, Kynoar, polyacrylonitrile, polymethyl methacrylate, polytetrafluoroethylene (PTFE), their mixture and butadiene-styrene rubber base polymer.The example of solvent comprises 1-METHYLPYRROLIDONE (NMP), acetone and water, but is not limited thereto, and can use any solvent as known in the art.
In some embodiments, plasticizer can join in positive electrode active compound composition further, to form pore in battery lead plate.The amount of positive active material, electric conducting material, jointing material and solvent can be normally used amount in lithium secondary battery field.
Second electrode 15 is negative electrode, and can be formed as the second electrode 15 for the second battery lead plate of negative electrode plate.
Except using negative electrode active material to replace except positive active material, mode that can be identical with preparation first electrode 11 prepares the second electrode 15.
That is, the same with during preparation the first electrode 11, prepare composition of cathode active materials by mixing negative electrode active material, electric conducting material, jointing material and solvent.Then, the second battery lead plate is prepared by being directly coated with composition of cathode active materials on copper electrode substrate.Or composition of cathode active materials may be cast on independent supporter, and can be laminated on copper electrode substrate from the negative electrode active material plasma membrane that above support is peeled off, to prepare the second battery lead plate.Second battery lead plate can be cut into suitable size to prepare the second electrode 15.
The example of negative electrode active material comprises lithium salts, can form the material of the metal material of alloy, transition metal oxide, the elements doped lithium that can adulterate/can go with lithium, and reversibly can embed the material with deintercalate lithium ions.
The example that can form the metal material of alloy with lithium comprises Si, Sn, Al, Ge, Pb, Bi, Sb, Si-Y alloy (here, Y is alkali metal, alkaline-earth metal, the 13 to 16 race's element, transition metal, rare earth element or their combination, and be not Si), with Sn-Y alloy (Y is alkali metal, alkaline-earth metal, the 13 to 16 race's element, transition metal, rare earth element or their combination, and is not Sn).The example of Y can be Mg, Ca, Sr, Ba, Ra, Sc, Y, Ti, Zr, Hf, Rf, V, Nb, Ta, Db, Cr, Mo, W, Sg, Tc, Re, Bh, Fe, Pb, Ru, Os, Hs, Rh, Ir, Pd, Pt, Cu, Ag, Au, Zn, Cd, B, Al, Ga, Sn, In, Tl, Ge, P, As, Sb, Bi, S, Se, Te, Po or their combination.
The example of transition metal oxide comprises barium oxide and lithium-barium oxide, and the example of material of doping and dedoping lithium can comprise Si, SiO x(0<x<2), Si-Y alloy (Y is alkali metal, alkaline-earth metal, the 13 to 16 race's element, transition metal, rare earth element or their combination, and is not Si), Sn, SnO 2with Sn-Y alloy (Y is alkali metal, alkaline-earth metal, the 13 to 16 race's element, transition metal, rare earth element or their combination, and is not Sn), or at least one selected by above-mentioned substance and SiO 2mixture.The example of Y comprises Mg, Ca, Sr, Ba, Ra, Sc, Y, Ti, Zr, Hf, Rf, V, Nb, Ta, Db, Cr, Mo, W, Sg, Tc, Re, Bh, Fe, Pb, Ru, Os, Hs, Rh, Ir, Pd, Pt, Cu, Ag, Au, Zn, Cd, B, Al, Ga, Sn, In, Tl, Ge, P, As, Sb, Bi, S, Se, Te, Po and their combination.
Can reversibly embed with the material of deintercalate lithium ions is material with carbon element, and can use usually with any negative electrode active material based on carbon in the lithium secondary battery.Example based on the negative electrode active material of carbon comprises crystalline carbon, amorphous carbon or their mixture.The example of crystalline carbon comprises graphite, such as unbodied, tabular, sheet, spherical or fibrous natural or Delanium.The example of amorphous carbon comprises soft carbon (carbon in relatively low heat-treated) or hard carbon, mesophase pitch carbide and heat treated coke.
But negative electrode active material is not limited thereto, and can uses and can be used as reversibly embedding any material with the negative electrode active material of deintercalate lithium ions.
In composition of cathode active materials, electric conducting material, jointing material and solvent can with use when preparation first electrode 11 identical.In some embodiments, plasticizer can be added further in composition of cathode active materials, to form pore in the second battery lead plate.
The amount of negative electrode active material, electric conducting material, jointing material and solvent can be normally used amount in lithium secondary battery field.According to purposes and the structure of lithium secondary battery, at least one in electric conducting material, jointing material and solvent can be omitted.
Then, the dividing plate 16 be arranged between the first electrode 11 and the second electrode 15 is prepared.Dividing plate 16 can have lower resistance relative to the Ion transfer of electrolyte and excellent electrolyte absorbability.
Substrate 13 can comprise polyolefin.Polyolefin has excellent against short-circuit effect, and can improve the stability of battery owing to closing effect.Such as, substrate 13 can be by comprising polyolefinic resin such as polyethylene, polypropylene, polybutene, polyvinyl chloride, or the film of their mixture or copolymer formation, but substrate 13 is not limited thereto, but can use any TPO film.Such as, substrate 13 can be the film formed by polyolefin resin, the film formed by manufacturing polyolefin fibrids, the aggregation that comprises polyolefinic nonwoven fabrics or insulating material particle.Such as, comprise the coating performance that polyolefinic substrate 13 can have the excellent polymer solution for the preparation of polymer coating 12 and 14, and the active substance part added in battery due to the film thickness by reducing dividing plate 16, so can improve the capacity of every volume.
Such as, the polyolefin as the material of substrate 13 can be the homopolymers of polyethylene, polypropylene etc., copolymer or mixture.Polyethylene can be low-density, intermediate density and highdensity polyethylene, and according to mechanical strength, can use highdensity polyethylene.Further, in order to provide flexible to substrate 13, the polyethylene of at least two types be selected from above can be mixed.The polymerization catalyst be used in poly preparation does not limit particularly, but can use the catalyst of Ziegler-Natta catalyst, Philips type or the catalyst of metallocene type.According to keeping mechanical strength and high light transmittance simultaneously, poly weight average molecular weight can 100,000 to 12, and 000,000, such as 200, in the scope of 000 to 3,000,000.Polypropylene can be homopolymers, random copolymer or block copolymer or their mixture.And polymerization catalyst does not have concrete restriction, and the catalyst of Ziegler-Natta catalyst or metallocene type can be used.In addition, polyacrylic tacticity does not have concrete restriction.Polypropylene can be isotactic, syndiotactic or atactic, but can use the isotactic polypropylene that cost is few relatively.And in the scope not violating effect of the present invention, except polyethylene or polypropylene, polyolefinic additive or antioxidant can join polyolefin.
The thickness of substrate 13 can in the scope of about 1 μm to about 100 μm.Such as, the thickness of substrate 13 can in the scope of about 1 μm to about 30 μm.Such as, the thickness of substrate 13 can in the scope of about 5 μm to about 30 μm.When the thickness of substrate 13 is less than 1 μm, the mechanical performance of substrate 13 can not be kept, and when the thickness of substrate 13 is greater than 100 μm, the resistance of battery can increase.
Substrate 13 can be porous.The substrate 13 of porous can have the porosity in about 5% to about 95% scope.When the porosity of substrate 13 is less than 5%, the resistance of battery can increase, and when the porosity of substrate 13 is greater than 95%, can not keep the mechanical performance of porous substrate 13.
Polymer coating 12 and 14 can comprise the polymer based on fluorine or the copolymer based on fluorine.The described polymer based on fluorine can comprise Kynoar.The described copolymer based on fluorine can be at least one in the group being selected from and being made up of Kynoar-hexafluoropropylene (PVdF-HFP) copolymer, Kynoar-polytetrafluoroethylene (PVdF-PTFE) copolymer and Kynoar-polytetrafluoroethylene-hexafluoropropylene (PVdF-PTFE-HFP) copolymer.The described polymer based on fluorine and the copolymer based on fluorine are not limited thereto, and can use available any polymer based on fluorine or the copolymer based on fluorine in this area.
Then, stacked electrodes assembly 10, then injects the electrolyte in stacking electrode assemblie 10.
Electrolyte can be the organic electrolyte that wherein can comprise lithium salts.
Organic electrolyte can comprise high dielectric solvent and low boiling point solvent.High dielectric solvent can be at least one in the group being selected from and being made up of ethylene carbonate, propylene carbonate, butylene carbonate and gamma butyrolactone.Low boiling point solvent can be at least one in the group being selected from and being made up of the derivative of dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, dipropyl carbonate, dimethoxy-ethane, diethoxyethane and fatty acid ester.
Lithium salts can be and is selected from by LiPF 6, LiBF 4, LiClO 4, Li (CF 3sO 2) 2, LiCF 3sO 3, LiSbF 6and LiAsF 6at least one in the group of composition.The concentration of lithium salts can in the scope of about 0.1M to about 0.2M.When the concentration of lithium salts is in above-mentioned scope, described electrolyte has suitable conductivity and viscosity, and thus battery can have excellent electrolyte property, and lithium ion can move effectively.
Then, the stacking electrode assemblie being injected with electrolyte carries out twice-aged process circulation, to prepare lithium secondary battery.
Such as, mode described below the process of described lithium secondary battery can be prepared.
That is, described process can comprise the first ageing process, pre-charge process, the first degassing procedure, hot pressing, the second ageing process and the second degassing procedure.
First ageing process and the second ageing process are under static state, store the process being injected with the stacking electrode assemblie of electrolyte in order to stability.Such as, the first ageing process and the second ageing process can at room temperature be carried out about 22 little of about 26 hours.When the first ageing process and the second ageing process are carried out being longer than 26 constantly little, preparation process can be extended, and when the first ageing process and the second ageing process are carried out being less than 22 constantly little, electrolyte can not be absorbed equably in electrode assemblie, thus can hinder the generation of uniform solid electrolyte interface (SEI) layer in pre-charge process after this.
Further, in some embodiments, the first ageing process and the second ageing process can at high temperature be carried out.When at high temperature carrying out the first ageing process and the second ageing process, Absorbable organic halogens SEI layer, and form SEI layer with uniform thickness.At high temperature can carry out the first ageing process and the second ageing process can be about 12 little of about 24 hours at the temperature such as within the scope of about 30 DEG C to about 45 DEG C.When carrying out the first ageing process and the second ageing process within the scope of described temperature and time, the suitable thickness of SEI layer can be kept, thus because the capacity when initial charge can be kept, so the capacity of lithium secondary battery can be guaranteed.
Pre-charge process is the process forming SEI layer on the surface of negative electrode.Pre-charge process reduces uncharged area by causing side reaction gas, thus can increase reversible capacity significantly.Pre-charge process can be carried out about 5 minutes to about 7 minutes by voltage within the scope of such as about 2.0V to about 2.4V and the about 0.045C electric current extremely within the scope of about 0.055C.When carrying out pre-charge process under the condition in above-mentioned scope, uniform SEI layer can be produced, and lithium secondary battery can be produced in a large number.
First degassing procedure and the second degassing procedure remove the gas of the first ageing process and the generation of the second ageing process, therefore can prevent the swelling of electrode assemblie.
As mentioned above, the hot pressing of at least one circulation can be carried out under 95 DEG C or higher temperature.Such as, can at about 200kgf/cm 2to about 500kgf/cm 2hot pressing is carried out under pressure in scope.Such as, can at the temperature within the scope of about 95 DEG C to about 120 DEG C and about 250kgf/cm 2to about 450kgf/cm 2hot pressing is carried out about 100 seconds to about 150 seconds under pressure in scope.
When carrying out hot pressing under the condition in above-mentioned scope, the bonding strength between the first electrode and the second electrode can be improved, therefore can improve intensity and the fail safe of lithium secondary battery.
According to another implementation of the invention, the lithium secondary battery using said method to prepare is provided.
Described lithium secondary battery can have the structure of the substrate being included in melting on polymer coating as above.The dividing plate comprising polymer coating can cover the first electrode or the second electrode, can improve the fail safe of lithium secondary battery under being heated therefore even under 130 DEG C or higher temperature.
Described lithium secondary battery can comprise pouch-type battery.
Equally, multiple pouch-type battery can the form of electrode assemblie stacking, thus form battery pack.Described battery pack can be used on to be needed in high power capacity and the high any device exported.Such as, described battery pack can be used in laptop computer, smart mobile phone or electric automobile.
The present invention is illustrated in greater detail with reference to the following examples.These embodiments only for illustration of object, instead of be intended to limit the scope of the invention.
[embodiment]
preparation example 1: the preparation of lithium secondary battery
The preparation of 1.1: the first electrodes
The LiCoO of 97.2 weight portions is placed in solvent N-methyl pyrilidone 2the Kynoar of powder, 1.5 weight portions and the carbon black of 1.3 weight portions, to prepare the first electrode slurry.Use scraper (gap: 170mm) on aluminium electrode base board, be coated with the thickness of the first electrode slurry to about 145 μm.At the temperature of 100 DEG C, heat treatment is coated with the aluminium electrode base board about 5.5 hours of the first slurry in a vacuum, dry afterwards.Then, use roll press to suppress the aluminium electrode base board of described drying, to prepare the first battery lead plate it being formed with the first electrode active material layer, and this first battery lead plate cuts into the size of 457mm × 65.5mm and the shape of band, to prepare the first electrode.
The preparation of 1.2: the second electrodes
The butadiene-styrene rubber of the graphite of 98 weight portions, 1 weight portion and the carboxymethyl cellulose of 1 weight portion is disperseed, to prepare the second electrode slurry in solvent N-methyl pyrilidone.Use scraper (gap: 160mm) on copper electrode substrate, be coated with the thickness of the second electrode slurry to about 140 μm.In the temperature of 145 DEG C in a vacuum heat treatment be coated with the copper electrode substrate about 6.5 hours of the second slurry, dry afterwards.Then, use roll press to suppress the copper electrode substrate of described drying, to prepare the second battery lead plate it being formed with the second electrode active material layer, and this second battery lead plate cuts into the size of 448mm × 66.5mm and the shape of band, to prepare the second electrode.
1.3: the preparation of dividing plate
The Kynoar (obtaining from Solvay) of 5 weight portions is joined the solvent i.e. 1-METHYLPYRROLIDONE of 95 weight portions, to prepare slurry.Use the thickness of rod coater coating sizing-agent to 9 μm on two surfaces of polyethylene porous substrate (obtaining from Asahi), to prepare the dividing plate of the polyvinylidene fluoride coating of the thickness with 3 μm.
1.4: embodiment 1: the preparation of lithium secondary battery
By between the second electrode of preparing in first electrode prepare in preparation example 1.1 of baffle arrangement of preparation in preparation example 1.3 and preparation example 1.2, to prepare electrode assemblie.Stacking described electrode assemblie also inserts in bag, then by the LiPF of 1.13M 6and the electrolyte of the mixing of ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) (volume ratio with 3:5:2) injects in described stacking electrode assemblie.At room temperature on the stacking electrode assemblie of electrolyte being injected with mixing, carry out the first ageing process about 24 hours.Next, at the pre-charge electricity electrode assemblie about 1 hour of 0.2C, then on electrode assemblie, the first degassing procedure is carried out in a vacuum about 15 seconds.Then, at temperature and the about 350kgf/cm of about 100 DEG C 2pressure under on electrode assemblie, carry out hot pressing about 120 seconds with heating plate, thus prepare complete stacking electrode assemblie.Then, at room temperature on described complete stacking electrode assemblie, the second ageing process is carried out about 24 hours.Then, on electrode assemblie, carry out the second degassing procedure in a vacuum about 15 seconds and seal to prepare lithium secondary battery.
comparative example 1: the preparation of lithium secondary battery
By between the second electrode of preparing in first electrode prepare in preparation example 1.1 of baffle arrangement of preparation in preparation example 1.3 and preparation example 1.2, to prepare electrode assemblie.Stacking described electrode assemblie also inserts in bag, then by the LiPF of 1.13M 6and the electrolyte of the mixing of ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) (volume ratio with 3:5:2) injects in described stacking electrode assemblie.At room temperature on the stacking electrode assemblie of electrolyte being injected with mixing, carry out the first ageing process about 24 hours.Next, at the pre-charge electricity electrode assemblie about 1 hour of 0.2C, on electrode assemblie, the first degassing procedure is then carried out about 15 seconds.Then, at temperature and the about 350kgf/cm of about 93 DEG C 2pressure under on electrode assemblie, carry out hot pressing about 120 seconds with heating plate, thus prepare complete stacking electrode assemblie.Then, at room temperature on described complete stacking electrode assemblie, the second ageing process is carried out about 24 hours.Then, on electrode assemblie, carry out the second degassing procedure in a vacuum about 15 seconds and seal to prepare lithium secondary battery.
comparative example 2: the preparation of lithium secondary battery
By between the second electrode of preparing in first electrode prepare in preparation example 1.1 of baffle arrangement of preparation in preparation example 1.3 and preparation example 1.2, to prepare electrode assemblie.Stacking described electrode assemblie also inserts in bag, then by the LiPF of 1.13M 6and the electrolyte of the mixing of ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) (volume ratio with 3:5:2) injects in described stacking electrode assemblie.At room temperature on the stacking electrode assemblie of electrolyte being injected with mixing, carry out the first ageing process about 24 hours.Next, at the pre-charge electricity electrode assemblie about 1 hour of 0.2C, on electrode assemblie, the first degassing procedure is then carried out about 15 seconds.Then, at temperature and the about 350kgf/cm of about 100 DEG C 2pressure under on electrode assemblie, carry out hot pressing about 190 seconds with heating plate, thus prepare complete stacking electrode assemblie.Then, at room temperature on described complete stacking electrode assemblie, the second ageing process is carried out about 24 hours.Then, on electrode assemblie, carry out the second degassing procedure in a vacuum about 15 seconds and seal to prepare lithium secondary battery.
experimental example 1: be heated experiment and security verification experiment
The lithium secondary battery of at room temperature preparation in embodiment 1 and comparative example 1 and 2 carries out the formation charging/electric discharge of 2 circulations.In formation process, lithium secondary battery is in the constant current charge of 0.7C, until the voltage of lithium secondary battery reaches 4.35V, then lithium secondary battery discharges in the constant voltage of 4.35V, until the electric current of lithium secondary battery reaches 0.05C.Next, lithium secondary battery discharges at the constant current of 1.0C, until the voltage of lithium secondary battery reaches 2.75V.Then, it carries out have the lithium secondary battery of formation charging/electric discharge to charge in the same manner as described above at the constant current of 0.5C, and discharge with the constant current of 0.2C, until the voltage of lithium secondary battery reaches 3.0V.Here, charge/discharge condition is the charge/discharge condition of standard, and discharge capacity used herein is the capacity of standard.
Each lithium secondary battery of preparation in embodiment 1 and comparative example 1 and 2 is joined in room under the charge/discharge condition of standard, and with the speed of 5 DEG C per minute, the temperature of described room is brought up to 130 DEG C from room temperature, and the change observing lithium secondary battery keeps the temperature 1 hour of 130 DEG C simultaneously.Fig. 3 to 5 shows result.Here, dotted line represents that voltage over time, and solid line represents that temperature over time.
With reference to Fig. 3 to 5, when being exposed to the heating temperatures of 130 DEG C, the lithium secondary battery prepared in embodiment 1 shows constant voltage and reaches 90 minutes, keeps the temperature of 130 DEG C simultaneously.But when being exposed to the heating temperatures of 130 DEG C, in comparative example 1 and 2, each lithium secondary battery of preparation shows the variations in temperature fast from 130 DEG C to 300 DEG C, and the voltage respectively when about 45 seconds and 28 seconds increases fast and reduces.That is, the quick increase of the voltage of the lithium secondary battery prepared in comparative example 1 and 2 and reduction show the generation of short circuit in battery.
Therefore, can confirm that the fail safe of the lithium secondary battery of preparation in embodiment 1 is better than the fail safe of the lithium secondary battery of preparation in comparative example 1 and comparative example 2.
Equally, in embodiment 1, the lithium secondary battery of preparation is exposed to the temperature of 130 DEG C, to observe the change in battery, then divides electrolytic cell, with the dividing plate using observation by light microscope first electrode, the second electrode and be arranged between the first electrode, the second electrode.Result is shown in Fig. 6.
With reference to Fig. 6, even when then the temperature being exposed to 130 DEG C decomposes, in embodiment 1 preparation each lithium secondary battery in have as the polymer coating in dividing plate polyvinylidene fluoride layer (such as, part see " A " represents) be still attached on the first electrode and the second electrode, and the polyethylene porous substrate of melting in polyvinylidene fluoride layer (such as, see the part that " B " represents) partly adheres to.
In this respect, can confirm that the dividing plate owing to comprising described polymer coating surrounds described first electrode and described second electrode, so improve the fail safe of the lithium secondary battery of preparation in embodiment 1.
As mentioned above, according to of the present invention one or more above execution mode, the method preparing lithium secondary battery comprises by carrying out the circulation of at least twice-aged process on the stacking electrode assemblie being injected with electrolyte and prepares lithium secondary battery, and the lithium secondary battery therefore using described method to prepare can have intensity and the fail safe of improvement.
Be understood that illustrative embodiments described herein is only considered from the meaning illustrated, and unrestriced object.Feature in each execution mode or in explanation usually should be considered to other the similar feature in other execution mode or in be effective.
Although with reference to the accompanying drawings of one or more execution mode of the present invention, but it will be appreciated by those skilled in the art that when not deviating from the spirit and scope of the present invention of appended claims definition, form wherein and details can make various change.

Claims (12)

1. prepare a method for lithium secondary battery, described method comprises:
Electrode assemblie is prepared by arranging the first electrode, the second electrode and the dividing plate between described first electrode and described second electrode;
Stacking described electrode assemblie also injects electrolyte in described stacking electrode assemblie; With
Lithium secondary battery is prepared by carrying out the circulation of at least twice-aged process on the described stacking electrode assemblie being injected with described electrolyte,
Wherein, described prepare lithium secondary battery be included in described ageing process circulation between carry out under 95 DEG C or higher temperature on described electrode assemblie at least one times hot pressing circulation.
2. method according to claim 1, wherein, at 200kgf/cm 2to 500kgf/cm 2described hot pressing is carried out under pressure in scope.
3. method according to claim 1, wherein, under 95 DEG C to the temperature within the scope of 120 DEG C and 250kgf/cm 2to 450kgf/cm 2described hot pressing is carried out under pressure in scope.
4. method according to claim 1, wherein, described hot pressing carries out 100 seconds to 180 seconds.
5. method according to claim 1, wherein, at room temperature carries out described ageing process.
6. method according to claim 1, wherein, in the preparation of described electrode assemblie, described dividing plate comprises substrate and the polymer coating at least one surface of described substrate.
7. method according to claim 6, wherein, in the preparation of described electrode assemblie, described polymer coating comprises the polymer based on fluorine or the copolymer based on fluorine.
8. method according to claim 7, wherein, the described polymer based on fluorine comprises Kynoar.
9. method according to claim 7, wherein, the described copolymer based on fluorine is be selected from least one in the group that is made up of Kynoar-hexafluoropropylene copolymer, Kynoar-teflon-copolymers and Kynoar-polytetrafluoroethylene-hexafluoropropylene copolymer.
10. method according to claim 1, wherein, described electrolyte is organic electrolyte.
11. 1 kinds of lithium secondary batteries, described lithium secondary battery uses the method preparation according to any one of claim 1 to 10.
12. lithium secondary batteries according to claim 11, described lithium secondary battery is pouch-type battery.
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