WO2013157902A1 - 세퍼레이터의 제조방법, 이로부터 형성된 세퍼레이터 및 이를 포함하는 전기화학소자 - Google Patents
세퍼레이터의 제조방법, 이로부터 형성된 세퍼레이터 및 이를 포함하는 전기화학소자 Download PDFInfo
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- WO2013157902A1 WO2013157902A1 PCT/KR2013/003413 KR2013003413W WO2013157902A1 WO 2013157902 A1 WO2013157902 A1 WO 2013157902A1 KR 2013003413 W KR2013003413 W KR 2013003413W WO 2013157902 A1 WO2013157902 A1 WO 2013157902A1
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/52—Separators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
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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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
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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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/443—Particulate material
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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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic 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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
- H01M50/451—Separators, membranes or diaphragms characterised by the material having a layered structure comprising layers of only organic material and layers containing inorganic material
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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
- 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
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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
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/491—Porosity
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
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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
- 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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- 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
- Y02E60/13—Energy storage using capacitors
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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
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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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
- 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
Definitions
- the present invention relates to a method for manufacturing a separator of an electrochemical device such as a lithium secondary battery, a separator formed therefrom, and an electrochemical device including the same, and a method of manufacturing a separator having a porous coating layer formed on a porous substrate having a plurality of pores, It relates to a separator formed from and an electrochemical device including the same.
- the electrochemical device is the most attracting field in this respect, and the development of a secondary battery capable of charging and discharging has been the focus of attention, and in recent years in the development of such a battery in order to improve the capacity density and specific energy
- the research and development of the design of the battery is progressing.
- lithium secondary batteries developed in the early 1990s have a higher operating voltage and greater energy density than conventional batteries such as Ni-MH, Ni-Cd, and sulfuric acid-lead batteries that use an aqueous electrolyte solution. I am in the spotlight.
- lithium ion batteries have safety problems such as ignition and explosion due to the use of the organic electrolyte, and are difficult to manufacture.
- the lithium ion polymer battery has been considered as one of the next generation batteries by improving the weakness of the lithium ion battery, but the capacity of the battery is still relatively low compared to the lithium ion battery, and the discharge capacity is improved due to insufficient discharge capacity at low temperatures. This is urgently needed.
- electrochemical devices are produced by many companies, but their safety characteristics show different aspects. It is very important to evaluate the safety and secure the safety of these electrochemical devices. The most important consideration is that the electrochemical device should not cause injury to the user in case of malfunction. For this purpose, safety standards strictly regulate the ignition and smoke in the electrochemical device. In the safety characteristics of the electrochemical device, there is a high possibility that an explosion occurs when the electrochemical device is overheated to cause thermal runaway or the separator penetrates. In particular, polyolefin-based porous substrates commonly used as separators for electrochemical devices exhibit extreme heat shrinkage behavior at temperatures of 100 ° C. or higher due to material properties and manufacturing process characteristics including elongation, thereby providing a short circuit between the cathode and the anode. There is a problem that causes.
- a separator in which a porous coating layer is formed by coating a mixture of inorganic particles and a binder polymer on at least one surface of a porous substrate having a plurality of pores has been proposed.
- the inorganic particles in the porous coating layer formed on the porous substrate serve as a kind of spacer that can maintain the physical form of the porous coating layer, thereby suppressing thermal shrinkage of the porous substrate when the electrochemical device is overheated.
- an interstitial volume exists between the inorganic particles to form fine pores.
- the formed separator is advantageous in bonding because an electrode adhesive layer is exposed to a considerable amount on the porous substrate layer because the separator is required to be stacked and folded in the process.
- the separator is required to be stacked and folded in the process.
- the problem to be solved by the present invention is a method of manufacturing a separator that is excellent in the assembly performance and prevent the performance degradation of the electrochemical device by the electrode adhesive layer by implementing a thin electrode bonding layer, without impairing the thermal stability of the separator, It is to provide a separator formed therefrom and an electrochemical device including the same.
- a second slurry is continuously coated on the porous coating layer through a slide portion adjacent to the slot portion to form an electrode adhesive layer.
- an angle ⁇ formed by the slot part and the slide part may be 10 to 80 °.
- the viscosity of the first slurry and the second slurry may be 5 cP to 100 cP independently of each other.
- the discharge speed of the first slurry may be greater than the discharge speed of the second slurry.
- the discharge rate of the first slurry and the second slurry may be 500 ml / min to 2,000 ml / min and 200 ml / min to 1,200 ml / min, respectively.
- the thickness of the electrode adhesive layer may be 0.1 times or less than the thickness of the porous coating layer.
- the porous substrate may be a polyolefin-based porous membrane.
- the slot portion and the slide portion may be formed in an integrated slide-slot die, or may be formed independently of each other in the slot die and the slide die.
- the average particle diameter of the inorganic particles may be 0.001 ⁇ m to 10 ⁇ m, and the inorganic particles may be used individually or in combination of inorganic particles having a dielectric constant of 5 or more, or inorganic particles having lithium ion transfer ability.
- the inorganic particles having a dielectric constant of 5 or more include BaTiO 3 , Pb (Zr x , Ti 1-x ) O 3 (PZT, where 0 ⁇ x ⁇ 1) and Pb 1-x La x Zr 1-y Ti y O 3 (PLZT, where 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1), (1-x) Pb (Mg 1/3 Nb 2/3 ) O 3 -xPbTiO 3 (PMN-PT, where , 0 ⁇ x ⁇ 1), Hafnia (HfO 2 ), SrTiO 3 , SnO 2 , CeO 2 , MgO, NiO, CaO, ZnO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , SiC and TiO 2 It may be any one inorganic particles selected from the group consisting of or a mixture of two or more thereof.
- the inorganic particles having the lithium ion transfer ability include lithium phosphate (Li 3 PO 4 ), lithium titanium phosphate (Li x Ti y (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 3), and lithium Aluminum titanium phosphate (Li x Al y Ti z (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 3), (LiAlTiP) x O y series glass (0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 13), lithium lanthanum titanate (Li x La y TiO 3, 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 3), lithium germanium thiophosphate (Li x Ge y P z S w , 0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 1, 0 ⁇ w ⁇ 5), lithium nitride (Li x N x N
- first binder polymer and the second binder polymer are independently of each other, polyvinylidene fluoride-co-hexafluoro propylene, polyvinylidene fluoride-trichloroethylene, and polyvinylidene fluoride.
- an electrochemical device including a cathode, an anode, and a separator interposed between the cathode and the anode is provided, wherein the separator is the aforementioned separator.
- the electrochemical device may be a lithium secondary battery.
- the porous coating layer and the electrode Inter-mixing of the adhesive layer can be prevented, so that the electrode adhesive layer can be formed more effectively.
- the adhesion to the electrode can be improved, and the performance of the electrochemical device can be prevented.
- FIG. 1 is a process diagram schematically showing a method of manufacturing a separator according to an embodiment of the present invention.
- FIG. 2 is a diagram illustrating an angle ⁇ formed between a slot portion and a slide portion of a slide-slot die according to an embodiment of the present invention.
- Figure 3 is a photograph showing the side when the slurry is discharged from the double slot die, according to a comparative example of the present invention.
- Figure 4 is a photograph showing the side when the slurry is discharged from the slide-slot die, according to an embodiment of the present invention.
- FIG. 5 is an enlarged SEM photograph of a cross section of a separator manufactured according to an embodiment of the present invention.
- FIG. 6 is an enlarged SEM photograph of a cross section of a separator manufactured according to a comparative example of the present invention.
- FIG. 7 is an enlarged SEM photograph of a side surface of a separator manufactured according to an embodiment of the present invention.
- a planar porous substrate having a plurality of pores is prepared.
- any porous substrate commonly used in an electrochemical device may be used.
- a polyolefin-based porous membrane or a nonwoven fabric may be used, but is not particularly limited thereto.
- polyolefin-based porous membrane examples include polyethylene, polypropylene, polybutylene, polypentene, such as high density polyethylene, linear low density polyethylene, low density polyethylene, ultra high molecular weight polyethylene, respectively, or a mixture thereof
- polyolefin-based polymers such as polyethylene, polypropylene, polybutylene, polypentene, such as high density polyethylene, linear low density polyethylene, low density polyethylene, ultra high molecular weight polyethylene, respectively, or a mixture thereof
- polyethylene such as polyethylene, polypropylene, polybutylene, polypentene, such as high density polyethylene, linear low density polyethylene, low density polyethylene, ultra high molecular weight polyethylene, respectively, or a mixture thereof
- polypentene such as high density polyethylene, linear low density polyethylene, low density polyethylene, ultra high molecular weight polyethylene, respectively, or a mixture thereof
- the nonwoven fabric may be, for example, polyethylene terephthalate, polybutyleneterephthalate, polyester, polyacetal, polyamide, polycarbonate, or polycarbonate. ), Polyimide, polyetheretherketone, polyethersulfone, polyphenyleneoxide, polyphenylenesulfidro, polyethylenenaphthalene, etc. Or the nonwoven fabric formed from the polymer which mixed these is mentioned.
- the structure of the nonwoven can be a spunbond nonwoven or melt blown nonwoven composed of long fibers.
- the thickness of the porous substrate is not particularly limited, but is 1 ⁇ m to 100 ⁇ m, or 5 ⁇ m to 50 ⁇ m.
- the pore size and pore present in the porous substrate are also not particularly limited, but may be 0.001 ⁇ m to 50 ⁇ m and 10% to 95%, respectively.
- the first slurry including the inorganic particles, the first binder polymer, and the first solvent is coated on at least one surface of the porous substrate through the slot to form the porous coating layer, and includes the second binder polymer and the second solvent.
- the second slurry is continuously coated on the porous coating layer through the slide portion adjacent to the slot portion to form an electrode adhesive layer.
- the inorganic particles are not particularly limited as long as they are electrochemically stable. That is, the inorganic particles that can be used in the present invention is not particularly limited as long as the oxidation and / or reduction reactions do not occur in the operating voltage range (for example, 0 to 5 V on the basis of Li / Li + ) of the applied electrochemical device.
- the ionic conductivity of the electrolyte may be improved by contributing to an increase in the dissociation degree of the electrolyte salt, such as lithium salt, in the liquid electrolyte.
- the inorganic particles preferably include high dielectric constant inorganic particles having a dielectric constant of 5 or more, or 10 or more.
- inorganic particles having a dielectric constant of 5 or more include BaTiO 3 , Pb (Zr x , Ti 1-x ) O 3 (PZT, where 0 ⁇ x ⁇ 1), Pb 1-x La x Zr 1 -y Ti y O 3 (PLZT, where 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1), (1-x) Pb (Mg 1/3 Nb 2/3 ) O 3 -xPbTiO 3 (PMN-PT , Wherein 0 ⁇ x ⁇ 1), hafnia (HfO 2 ), SrTiO 3 , SnO 2 , CeO 2 , MgO, NiO, CaO, ZnO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , SiC and It may be any one
- inorganic particles having lithium ion transfer capability that is, inorganic particles containing lithium elements but having a function of transferring lithium ions without storing lithium
- inorganic particles having a lithium ion transfer capacity include lithium phosphate (Li 3 PO 4 ), lithium titanium phosphate (Li x Ti y (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 3) , Lithium aluminum titanium phosphate (Li x Al y Ti z (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 3), 14Li 2 O-9Al 2 O 3 -38TiO 2 -39P (LiAlTiP) x O y series glass such as 2 O 5 (0 ⁇ x ⁇ 4, 0 ⁇ y ⁇ 13), lithium lanthanum titanate (Li x La y TiO 3 , 0
- Li x P y S z such as (Li x Si y S z , 0 ⁇ x ⁇ 3, 0 ⁇ y ⁇ 2, 0 ⁇ z ⁇ 4), LiI-Li 2 SP 2 S 5, etc.) , 0 ⁇ x ⁇ 3, 0 ⁇ y ⁇ 3, 0 ⁇ z ⁇ 7) or mixtures thereof.
- the average particle diameter of the inorganic particles is not particularly limited, but may be in the range of 0.001 ⁇ m to 10 ⁇ m for forming a porous coating layer having a uniform thickness and proper porosity.
- the dispersibility of the inorganic particles may be prevented from being lowered, and the porous coating layer may be adjusted to an appropriate thickness.
- Non-limiting examples of the first binder polymer and the second binder polymer include polyvinylidene fluoride-co-hexafluoro propylene, polyvinylidene fluoride-trichloroethylene ( polyvinylidene fluoride-co-trichloro ethylene, polyvinylidene fluoride-co-chlorotrifluoro ethylene, polymethyl methacrylate, polyacrylonitrile, polyvinyl Pyrrolidone (polyvinylpyrrolidone), polyvinylacetate, ethylene vinyl acetate copolymer (polyethylene-co-vinyl acetate), polyethylene oxide, cellulose acetate, cellulose acetate butyrate ), Cellulose acetate propionate tate propionate, cyanoethylpullulan, cyanoethylpolyvinylalcohol, cyanoethyl cellulose, cyanoethylsucrose, pullulan, carboxy
- the first solvent of the present invention disperses the inorganic particles while dissolving the binder polymer
- the second solvent is not particularly limited as long as it can disperse and dissolve the binder polymer, it may be more advantageous that the boiling point is low. This is to facilitate solvent removal later.
- Non-limiting examples of the first and second solvents that can be used include acetone, tetrahydrofuran, methylene chloride, chloroform, dimethylform amide, N-methyl -2-pyrrolidone (N-methyl-2-pyrrolidone, NMP), cyclohexane, water or a mixture thereof.
- the slot 1 and the slide 2 may be formed in the integrated slide-slot die 10, but are not limited thereto.
- the slide portion 2 may be formed in the slot die and the slide die, respectively, independently of each other.
- the slide portion 2 is positioned adjacent to the slot portion 1, and inclined with the ground so that the second slurry can slide down the upper surface of the slide portion 2 by gravity alone without any external force. It can be formed by.
- a strong shear stress may act to mix the first slurry and the second slurry at the discharge part of the die.
- inter-mixing of the porous coating layer and the electrode adhesive layer inter- mixing
- the angle ⁇ formed by the slot 1 and the slide 2 may be positioned to form an angle of 10 ° to 80 °, or 30 ° to 60 °.
- the numerical range is satisfied, even when the first slurry and the second slurry have low viscosity, adjustment of the thickness to be coated becomes easy.
- the slide portion 2 is too long may cause a problem that the second slurry is volatilized, thereby causing a non-uniform thickness of the electrode adhesive layer.
- inorganic particles are dispersed in a first solvent and a first slurry dissolved therein is supplied.
- a second slurry in which the binder polymer is dispersed and dissolved in a second solvent is supplied through the slide unit 2.
- the viscosity of the first slurry may be 5 cP to 100 cP, or 10 cP to 20 cP
- the viscosity of the second slurry may be 5 cP to 100 cP, or 10 cP to 20 cP.
- the discharge rate of the first slurry may be greater than the discharge rate of the second slurry, wherein, the discharge rate of the first slurry is 500 ml / min to 2,000 ml / min, or 1,000 ml / min to 1,500 ml / min, the discharge rate of the second slurry may be 200 ml / min to 1,200 ml / min, or 500 ml / min to 900 ml / min.
- a thin electrode adhesive layer may be formed without intermixing two layers.
- FIG. 1 only a method of forming a coating layer on only one surface of the porous substrate is exemplified.
- the present invention is not limited thereto, and the separator may be manufactured by forming the coating layers on both surfaces of the porous substrate.
- the thickness of the electrode adhesive layer may be, for example, 0.1 times or less, or 0.001 times to 0.05 times the thickness of the porous coating layer.
- the electrode adhesive layer can be formed to a thin thickness.
- the porous coating layer may have a thickness of 0.01 ⁇ m to 20 ⁇ m, and the thickness of the electrode adhesive layer may be 0.0001 ⁇ m to 2 ⁇ m, or 0.0005 ⁇ m to 1 ⁇ m, but is not limited thereto.
- the electrode assembly used in the electrochemical device may be manufactured by laminating a separator prepared according to the above method between the cathode and the anode.
- Electrochemical devices include all devices that undergo an electrochemical reaction, and specific examples thereof include capacitors such as all kinds of primary, secondary cells, fuel cells, solar cells, or super capacitor devices.
- a lithium secondary battery including a lithium metal secondary battery, a lithium ion secondary battery, a lithium polymer secondary battery or a lithium ion polymer secondary battery among the secondary batteries is preferable.
- Both electrodes of the cathode and the anode to be applied together with the separator of the present invention are not particularly limited, and the electrode active material may be prepared in a form bound to the electrode current collector according to conventional methods known in the art.
- Non-limiting examples of the cathode active material of the electrode active material may be a conventional cathode active material that can be used for the cathode of the conventional electrochemical device, in particular lithium manganese oxide, lithium cobalt oxide, lithium nickel oxide, lithium iron oxide or a combination thereof It is preferable to use one lithium composite oxide.
- Non-limiting examples of the anode active material may be a conventional anode active material that can be used for the anode of the conventional electrochemical device, in particular lithium metal or lithium alloys, carbon, petroleum coke, activated carbon, Lithium adsorbents such as graphite or other carbons are preferred.
- Non-limiting examples of the cathode current collector include a foil made of aluminum, nickel or a combination thereof, and non-limiting examples of the anode current collector are copper, gold, nickel or a copper alloy or a combination thereof. Foils produced.
- Electrolyte that may be used in the electrochemical device of the present invention is A + B - A salt of the structure, such as, wherein A + comprises Li +, Na +, an alkali metal cation or an ion composed of a combination thereof, such as K + , wherein B - is PF 6 -, BF 4 -, Cl -, Br -, I -, ClO 4 -, AsF 6 -, CH 3 CO 2 -, CF 3 SO 3 -, N (CF 3 SO 2) 2 -, C (CF 2 SO 2 ) 3 - salts comprising the anions or an ion composed of a combination thereof, such as propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC ), Dipropyl carbonate (DPC), dimethyl sulfoxide, acetonitrile, dimethoxyethane, diethoxyethane, tetrahydrofuran, N-methyl
- the electrolyte injection may be performed at an appropriate stage of the battery manufacturing process, depending on the manufacturing process and the required physical properties of the final product. That is, it may be applied before the battery assembly or at the end of battery assembly.
- a process of laminating and stacking the separator and the electrode may be performed in addition to the general winding process.
- a mixture of aluminum oxide (Al 2 O 3 ) as inorganic particles, polyvinylidene fluoride-chlorotrifluoroethylene copolymer (PVdF-CTFE) and cyanoethyl pullulan as first binder polymer, and agent Acetone was mixed as a solvent in a weight ratio of 18: 2: 80 to prepare a first slurry. At this time, the viscosity of the first slurry was 10 cP.
- PVdF-CTFE polyvinylidene fluoride-chlorotrifluoroethylene copolymer
- cyanoethyl pullulan as a second binder polymer and acetone as a second solvent were mixed in a weight ratio of 3:97
- a second slurry was prepared. At this time, the viscosity of the second slurry was 10 cP.
- a polyolefin membrane (Celgard, C210) having a thickness of 16 ⁇ m was used as the porous substrate, and a second slurry was supplied to the slide section and a first slurry was supplied to the slot section using a slide-slot die to coat the porous substrate. .
- the first slurry was to be directly coated on the upper surface of the porous substrate to form a porous coating layer, while the second slurry was continuously coated on the upper surface of the porous coating layer to form an electrode adhesive layer.
- the slide portion and the slot portion is positioned to form an angle of 45 °, the discharge rate of the first slurry was adjusted to 1200ml / min, the discharge rate of the second slurry is 700ml / min.
- the first slurry is continuously coated onto the upper surface of the porous substrate to form a porous coating layer while continuously forming a second slurry.
- the separator was manufactured in the same manner as in Example, except that the upper surface of the porous coating layer was coated to form an electrode adhesive layer.
- Figure 3 is a photograph showing the side when the slurry is discharged from the double slot die, according to the comparative example
- Figure 4 is a side view of the slurry when discharged from the slide-slot die, according to an embodiment of the present invention It is a photograph.
- the Examples and Comparative Examples show almost the same electrode adhesive layer loading, but the separator adhesion of the Examples is about twice as high. This means that the embodiment prevents inter-mixing than that of the comparative example, so that there are more second binder polymers present in the surface layer of the separator, and that the electrode adhesive layer is evenly formed.
- 5 and 6 are SEM photographs showing enlarged cross-sections of separators manufactured according to one embodiment and one comparative example of the present invention, respectively.
- the dark portion is a portion where an electrode adhesive layer is formed, and in the embodiment, it can be seen that the electrode adhesive layer is more evenly and widely coated.
- Figure 7 is an SEM image showing an enlarged cross-section of the separator manufactured according to an embodiment of the present invention. Looking at Figure 7, it can be seen that the electrode adhesive layer thinly formed on the upper surface of the porous coating layer. Thereby, while improving the adhesive force with respect to an electrode, the performance fall of an electrochemical element can be prevented.
Abstract
Description
물성 | 실시예 | 비교예 |
세퍼레이터 두께 | 7.58 ㎛ | 7.83 ㎛ |
전극접착층 로딩량 | 14.48 g/m2(1.91 g/cm3) | 14.52 g/m2(1.86 g/cm3) |
걸리 지수 | 741 s/100cc | 728 s/100cc |
세퍼레이터의 접착력 | 24.2 gf/25mm | 12.3 gf/25mm |
Claims (16)
- 다수의 기공을 갖는 평면상의 다공성 기재를 준비하는 단계; 및무기물 입자, 제1 바인더 고분자 및 제1 용매를 포함하는 제1 슬러리를, 슬롯부를 통해 상기 다공성 기재의 적어도 일면에 코팅하여, 다공성 코팅층을 형성하면서, 제2 바인더 고분자 및 제2 용매를 포함하는 제2 슬러리를, 상기 슬롯부와 인접한 슬라이드부를 통해 상기 다공성 코팅층 위에 연속적으로 코팅하여, 전극 접착층을 형성하는 단계;를 포함하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 슬롯부와 상기 슬라이드부가 서로 형성하는 각도(θ)는, 10° 내지 80°인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 제1 슬러리 및 상기 제2 슬러리의 점도는, 서로 독립적으로 5 cP 내지 100 cP인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 제1 슬러리의 토출속도는, 상기 제2 슬러리의 토출속도보다 큰 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제4항에 있어서,상기 제1 슬러리 및 상기 제2 슬러리의 토출속도는, 각각 500 ml/min 내지 2,000 ml/min 및 200 ml/min 내지 1,200 ml/min인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 전극 코팅층의 두께가 상기 다공성 코팅층의 두께의 0.1배 이하인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 다공성 기재가 폴리올레핀계 다공성 막인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 슬롯부 및 상기 슬라이드부는 일체형의 슬라이드-슬롯 다이에 형성되거나, 서로 독립적으로 각각 슬롯 다이 및 슬라이드 다이에 형성되는 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 무기물 입자의 평균입경이 0.001㎛ 내지 10㎛인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 무기물 입자가 유전율 상수가 5 이상인 무기물 입자, 리튬 이온 전달 능력을 갖는 무기물 입자 및 이들의 혼합물로 이루어진 군으로부터 선택된 무기물 입자인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제10항에 있어서,상기 유전율 상수가 5 이상인 무기물 입자는, BaTiO3, Pb(Zrx,Ti1-x)O3(PZT, 여기서, 0<x<1임), Pb1-xLaxZr1-yTiyO3(PLZT, 여기서, 0<x<1, 0<y<1임), (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3(PMN-PT, 여기서, 0<x<1임), 하프니아(HfO2), SrTiO3, SnO2, CeO2, MgO, NiO, CaO, ZnO, ZrO2, Y2O3, Al2O3, SiC 및 TiO2로 이루어진 군으로부터 선택된 어느 하나의 무기물 입자 또는 이들 중 2종 이상의 혼합물인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제10항에 있어서,상기 리튬 이온 전달 능력을 갖는 무기물 입자는, 리튬 포스페이트(Li3PO4), 리튬 티타늄 포스페이트(LixTiy(PO4)3, 0<x<2, 0<y<3), 리튬 알루미늄 티타늄 포스페이트(LixAlyTiz(PO4)3, 0<x<2, 0<y<1, 0<z<3), (LiAlTiP)xOy계열 글래스(0<x<4, 0<y<13), 리튬 란탄 티타네이트(LixLayTiO3, 0<x<2, 0<y<3), 리튬 게르마니움 티오포스페이트(LixGeyPzSw, 0<x<4, 0<y<1, 0<z<1, 0<w<5), 리튬 나이트라이드(LixNy, 0<x<4, 0<y<2), SiS2(LixSiySz, 0<x<3, 0<y<2, 0<z<4)계열 글래스 및 P2S5(LixPySz, 0<x<3, 0<y<3, 0<z<7)계열 글래스로 이루어진 군으로부터 선택된 어느 하나의 무기물 입자 또는 이들 중 2종 이상의 혼합물인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항에 있어서,상기 제1 바인더 고분자 및 상기 제2 바인더 고분자는, 서로 독립적으로 폴리비닐리덴 플루오라이드-헥사플루오로 프로필렌(polyvinylidene fluoride-co-hexafluoro propylene), 폴리비닐리덴 플루오라이드-트리클로로 에틸렌(polyvinylidene fluoride-co-trichloro ethylene), 폴리비닐리덴 플루오라이드-클로로트리플루오로 에틸렌(polyvinylidene fluoride-co-chlorotrifluoro ethylene), 폴리메틸 메타크릴레이트(polymethyl methacrylate), 폴리아크릴로니트릴(polyacrylonitrile), 폴리비닐피롤리돈(polyvinylpyrrolidone), 폴리비닐아세테이트(polyvinylacetate), 에틸렌 비닐 아세테이트 공중합체 (polyethylene-co-vinyl acetate), 폴리에틸렌 옥사이드(polyethylene oxide), 셀룰로오스 아세테이트(cellulose acetate), 셀룰로오스 아세테이트 부틸레이트(cellulose acetate butyrate), 셀룰로오스 아세테이트 프로피오네이트(cellulose acetate propionate), 시아노에틸 풀루란(cyanoethylpullulan), 시아노에틸폴리비닐알콜(cyanoethylpolyvinylalcohol), 시아노에틸 셀룰로오스(cyanoethylcellulose), 시아노에틸 수크로오스(cyanoethylsucrose), 풀루란(pullulan), 카르복실 메틸 셀룰로오스(carboxyl methyl cellulose), 아크리로니트릴 스티렌부타디엔 공중합체(acrylonitrile-styrene-butadiene copolymer) 및 폴리이미드(polyimide)로 이루어진 군으로부터 선택된 어느 하나 또는 이들 중 2종 이상의 혼합물인 것을 특징으로 하는 세퍼레이터의 제조방법.
- 제1항 내지 제13항 중 어느 한 항에 따른 제조방법에 따라 형성된 세퍼레이터.
- 캐소드, 애노드, 상기 캐소드와 상기 애노드 사이에 개재된 세퍼레이터를 포함하는 전기화학소자에 있어서,상기 세퍼레이터가 제14항의 세퍼레이터인 전기화학소자.
- 제15항에 있어서,상기 전기화학소자는 리튬 이차전지인 것을 특징으로 하는 전기화학소자.
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CA2858735A CA2858735C (en) | 2012-04-20 | 2013-04-22 | Separator and electrochemical device having the same |
EP13778296.7A EP2840628B1 (en) | 2012-04-20 | 2013-04-22 | Method for manufacturing separator, separator formed thereby, and electrochemical device comprising said separator |
JP2014529627A JP6208663B2 (ja) | 2012-04-20 | 2013-04-22 | セパレータの製造方法、その方法で形成されたセパレータ、及びそれを含む電気化学素子 |
CN201380003260.8A CN103843171B (zh) | 2012-04-20 | 2013-04-22 | 隔膜以及具有所述隔膜的电化学装置 |
US14/191,738 US9853268B2 (en) | 2012-04-20 | 2014-02-27 | Separator and electrochemical device having the same |
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KR20130044338A KR101488829B1 (ko) | 2012-04-20 | 2013-04-22 | 세퍼레이터의 제조방법, 이로부터 형성된 세퍼레이터 및 이를 포함하는 전기화학소자 |
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JP2020064879A (ja) * | 2020-01-21 | 2020-04-23 | 三星エスディアイ株式会社Samsung SDI Co., Ltd. | リチウムイオン(lithium ion)二次電池用セパレータ(separator)及びリチウムイオン二次電池 |
JP7088969B2 (ja) | 2020-01-21 | 2022-06-21 | 三星エスディアイ株式会社 | リチウムイオン(lithium ion)二次電池用セパレータ(separator)及びリチウムイオン二次電池 |
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JP2014526776A (ja) | 2014-10-06 |
US20140178740A1 (en) | 2014-06-26 |
CN103843171A (zh) | 2014-06-04 |
US9853268B2 (en) | 2017-12-26 |
EP2840628A4 (en) | 2016-05-11 |
EP2840628A1 (en) | 2015-02-25 |
KR20130118835A (ko) | 2013-10-30 |
CA2858735C (en) | 2016-10-04 |
JP6208663B2 (ja) | 2017-10-04 |
CN103843171B (zh) | 2016-12-07 |
EP2840628B1 (en) | 2017-11-29 |
CA2858735A1 (en) | 2013-10-24 |
KR101488829B1 (ko) | 2015-02-04 |
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