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WO2014084684A1 - Film de séparation destiné à un dispositif électrochimique et son procédé de fabrication - Google Patents

Film de séparation destiné à un dispositif électrochimique et son procédé de fabrication Download PDF

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Publication number
WO2014084684A1
WO2014084684A1 PCT/KR2013/011038 KR2013011038W WO2014084684A1 WO 2014084684 A1 WO2014084684 A1 WO 2014084684A1 KR 2013011038 W KR2013011038 W KR 2013011038W WO 2014084684 A1 WO2014084684 A1 WO 2014084684A1
Authority
WO
WIPO (PCT)
Prior art keywords
separator
electrochemical device
film
etching
pores
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2013/011038
Other languages
English (en)
Korean (ko)
Inventor
이주성
윤수진
성동욱
한다경
가경륜
김종훈
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LG Chem Ltd
Original Assignee
LG Chem Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LG Chem Ltd filed Critical LG Chem Ltd
Priority claimed from KR1020130147441A external-priority patent/KR101522657B1/ko
Publication of WO2014084684A1 publication Critical patent/WO2014084684A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • H01M50/406—Moulding; Embossing; Cutting
    • 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
    • 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
    • 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

Definitions

  • the present invention relates to a separator for an electrochemical device and a method of manufacturing the same, and more particularly, a plurality of pores are formed on both sides of the separator, each of the pores is truncated cone shape in the thickness direction from one side to the other side of the separator And a method for manufacturing the separator for an electrochemical device in which the separator surface having larger pores is formed to face the cathode, thereby preventing deterioration of battery performance by dendrite.
  • lithium ion secondary batteries developed in the early 1990s have a higher operating voltage and a higher energy density than conventional batteries such as Ni-MH, Ni-Cd, and sulfuric acid-lead batteries that use an aqueous electrolyte solution. It is attracting attention because of its great advantage.
  • lithium ion secondary batteries have safety problems such as ignition and explosion due to the use of the organic electrolyte, and are difficult to manufacture.
  • pores of the membrane due to the negative electrode by-products are formed on both sides of the separator.
  • the present invention is to provide a method for producing a separator as described above and an electrochemical device using the separator as described above.
  • the pores are formed on both sides of the separator, but the pores are formed in a truncated cone shape in the thickness direction from one side of the separator to the other side, and the pores are 1 to 50 on one side of the separator.
  • a separator for an electrochemical device having a diameter of nm and formed on the other side to have a diameter of 10 to 100 nm.
  • the pores may be formed in the separator to have an aeration time in the range of 5 to 1000 sec / 100cc.
  • the separator is a fluoropolymer, polyethylene, low density polyethylene, linear low density polyethylene, ultra high molecular weight polyethylene, polypropylene, polyethylene terephthalate, polybutylene terephthalate, polyester, polyacetal , Polyamide, polycarbonate, polyimide, polyetheretherketone, polyethersulfone, polyphenyleneoxide, polyphenylenesulfidro , Polyethylenenaphthalene, polysulfone, cellulose acetate, and polystyrene may be based on one or two or more kinds selected from the group consisting of.
  • the separator in the electrochemical device comprising a separator and an electrolyte interposed between the positive electrode, the negative electrode, the positive electrode and the negative electrode, the separator is the above-mentioned separator, the pores having a larger diameter of the separator
  • An electrochemical device is provided, characterized in that the surface formed faces the cathode.
  • the electrochemical device may be a lithium secondary battery.
  • the method comprising: preparing a film on which a track is formed as a separator substrate for an electrochemical device; And etching both sides of the film to different degrees, respectively.
  • the step of etching both sides of the film to different degrees may be to apply an etching solution containing a surfactant to both sides of the film after exposing ultraviolet light to only one side of the film.
  • the ultraviolet light has a wavelength range of 280 to 400 nm, and may be irradiated with an energy of 1 to 10 W / m 2.
  • the surfactant may be included in the concentration of 0.01 to 0.2% by weight in the etching solution.
  • Etching both sides of the film to different degrees may include applying two etching liquids having different etching capabilities to each of both sides of the film.
  • the two kinds of etchant may be an etchant having a concentration of 1 to 5 M and an etchant having a concentration of 3 to 10 M.
  • the two kinds of etching solutions are selected from the group consisting of sodium hydroxide (NaOH), potassium hydroxide (KOH), calcium hydroxide (Ca (OH) 2 ), sodium hypochlorite (NaClO) and hydrogen peroxide (H 2 O 2 ). It may be an etchant which is a mixture of species or more.
  • pores of different diameter sizes may be formed on both sides of the separator.
  • the technical problem that the membrane pores are occluded by the by-products in the secondary battery storage and cycle test by facing the separator surface on which the larger diameter pores are formed can be solved.
  • FIG. 1 is a perspective view schematically showing a separator according to an embodiment of the present invention.
  • FIG. 2 is a cross-sectional view schematically showing a separator according to an embodiment of the present invention.
  • FIG 3 is a view schematically showing a configuration in which a separator is interposed between an anode and a cathode according to an embodiment of the present invention.
  • pores are formed on both sides of the separator, but the pores are formed in a truncated cone shape in one direction from one side to the other side of the separator, and the pores have a diameter of 1 to 50 nm on one side of the separator. It may have a diameter of 10 to 100 nm on the other side of the separator. That is, the diameters of the pores formed in the separator are different in the thickness direction, and the separator surface on which the larger pores are formed is assembled to face the negative electrode in a subsequent battery assembly process, thereby preventing pore blockage due to by-products generated in the negative electrode.
  • the term "diameter" of pores is understood to refer to the longest diameter (longest diameter) of the pores.
  • each pore is formed in the separator in a truncated cone shape, and at one side of the separator, an end having a relatively large diameter of each pore is formed. It is understood that the other side means that an end having a relatively small diameter of each pore is formed. That is, referring to FIGS. 1 and 2, a larger diameter of the pores 2 of the separator 1 is defined. It can be seen that the pores 2a having are formed on one side of the separation membrane, and the pores 2b having a smaller diameter are formed on the other side of the separation membrane.
  • the pores may be formed in the film such that the resulting membrane has an aeration time (air permeability) in the range of 5 to 1000 sec / 100 cc. If the air permeability is larger than the upper limit, the mechanical properties of the separator are lowered, and if the air permeability is smaller than the lower limit, smooth movement of lithium ions cannot be ensured.
  • air permeability air permeability
  • the film used as the separator substrate in the present invention is not particularly limited as long as it can be track etched and used as a separator in the art, and is not limited to fluoropolymer, polyethylene, low density polyethylene, linear low density polyethylene, ultra high molecular weight polyethylene, polypropylene, polyethylene tere Phthalate (polyethyleneterephthalate), polybutyleneterephthalate (polyester), polyester (polyester), polyacetal, polyamide, polycarbonate, polyimide, polyetheretherketone ), One or two selected from the group consisting of polyethersulfone, polyphenyleneoxide, polyphenylenesulfidro, polyethylenenaphthalene, polysulfone, cellulose acetate and polystyrene It may be a mixture of.
  • Preferred films are fluoropolymer films, and more preferred films are polyvinylidene fluoride (PVdF) films.
  • the film may have a thickness of 1 ⁇ m to 100 ⁇ m or 5 ⁇ m to 50 ⁇ m, but is not particularly limited thereto, as long as it may be used as a separator.
  • Separation membrane comprises the steps of preparing a film with a track formed; And etching both sides of the film to different degrees, respectively.
  • track is understood to mean damage-trail formed on a film by an ion beam or the like.
  • the method of forming the track in the film in the present invention is not particularly limited, and may be performed by, for example, irradiating an ion beam having argon, krypton, xenon, bismuth or a combination thereof.
  • the irradiation amount or irradiation time of the ion beam may vary depending on the film used or the desired track density. For example, an ion beam having an acceleration voltage of 100 to 300 MeV is irradiated, and the irradiation time may be 1 to 30 minutes, but is not limited thereto. It doesn't happen.
  • the track density can be determined according to the pore diameter and air permeability of the desired separator.
  • Etching both sides of the film to different degrees may be performed by applying ultraviolet light to only one side of the film, and then applying an etchant including a surfactant to both sides of the film, or applying two etching solutions having different etching capabilities to each side of the film. It can be carried out by a method applied to.
  • Ultraviolet rays are irradiated on only one side of the film to make the irradiated film side hydrophobic. Subsequently, when the etching solution containing the surfactant is applied to both sides of the film, the hydrophobicity of both sides of the film is different, and thus the surfactant adsorption rate on both sides of the film is also different. As a result, more surfactant is adsorbed on the surface of the film not irradiated with UV light, so that etching is less, and pores of smaller diameter are formed. On the other hand, less surface area is irradiated with the surface of the UV-irradiated film. Rises to form pores of larger diameter.
  • Irradiation of ultraviolet rays has a wavelength range of 280 to 400 nm, and is carried out by irradiation with energy of 1 to 10 W / m 2.
  • Water-soluble or water-dispersible surfactants may be used as the surfactant, and may be at least one surfactant selected from the group consisting of anionic, cationic, nonionic, amphoteric and zwitterionic surfactants.
  • Nonionic surfactants that can be used in the present invention include, but are not limited to, alkoxylated alcohols including ethoxylated and propoxylated alcohols, as well as ethoxylated and propoxylated alkyl phenols.
  • Other species include sorbitan fatty esters and fatty acids of unsaturated alcohols.
  • nonionic surfactants include polysaccharides such as polyglycosides, hydrophilic groups, as well as alkylpolysaccharides having hydrophobic groups containing about 6 to 30 carbon atoms, preferably about 10 to 16 carbon atoms. .
  • the surfactant may be included in the concentration of 0.01 to 0.2% by weight or 0.02 to 0.1% by weight in the etching solution.
  • the etching solution may be selected according to the film, for example, sodium hydroxide (NaOH), potassium hydroxide (KOH), calcium hydroxide (Ca (OH) 2 ), sodium hypochlorite (NaClO) and hydrogen peroxide (H 2 O 2 ) It may be one or a mixture of two or more selected from the group consisting of, but is not limited thereto.
  • the method of applying the etching solution to the film includes a method of passing the film through the etching solution or dipping, but is not limited to these methods.
  • the two etchant is classified according to the etching ability.
  • Etching ability can be suitably adjusted by differentiating i) the kind of etching compound used for etching liquid, or ii) the density
  • Etching liquid with greater etching ability can be applied to the film surface to form larger pores.
  • the type of etchant that can be used is, for example, one selected from the group consisting of sodium hydroxide (NaOH), potassium hydroxide (KOH), calcium hydroxide (Ca (OH) 2 ), sodium hypochlorite (NaClO), and hydrogen peroxide (H 2 O 2 ). Or a mixture of two or more thereof, but is not limited thereto.
  • the concentration of the etchant that can be used may be an etchant of 3 to 10 M concentration for the formation of larger pores, and an etchant of 1 to 5 M concentration for the formation of smaller pores.
  • the method of applying two etching solutions to both sides of the film is to cover both sides of the film on which the track is formed with two cloths soaked with two etching solutions for a certain period of time, or to pour the first etching solution on one side of the film on which the track is formed.
  • spraying and etching there is a method of inverting and pouring or spraying the second etchant on the other side of the film, but all of these methods are exemplary and not limited thereto.
  • a surfactant may be applied to one surface to give a difference in etching performance on both sides of the substrate. That is, by applying a surfactant to only one surface of the substrate before immersion in the etchant to improve the wettability after immersion of the etchant can increase the etching rate for one surface.
  • the etching time is preferably in the range of 1 to 30 minutes since the etching of the desired pore diameter can be made without excessively large pores or by-products being generated.
  • the etching step may be followed by procedures common in the art, such as washing, drying and the like.
  • the separator prepared as described above may be used in an electrochemical device according to a conventional method known in the art, but as described above, the surface of the separator 1 in which pores 2a having a relatively large diameter are formed (A), and the surface in which the pores 2b having a relatively small diameter are formed in the separator 1 is in contact with the anode B (see FIG. 3).
  • Non-limiting examples of the positive electrode active material of the electrode active material that can be used in the electrochemical device may be a conventional positive electrode active material that can be used for the positive electrode of the conventional electrochemical device, for example, lithium manganese oxide, lithium cobalt oxide, lithium nickel oxide , Lithium iron oxide or a lithium composite oxide in combination thereof can be used.
  • Non-limiting examples of the negative electrode active material may be a conventional negative electrode active material that can be used for the negative electrode of the conventional electrochemical device, for example, lithium metal or lithium alloy, carbon, petroleum coke, activated carbon , Lithium adsorbents such as graphite or other carbons.
  • Non-limiting examples of the positive electrode current collector is a foil produced by aluminum, nickel or a combination thereof, and non-limiting examples of the negative electrode current collector is produced by copper, gold, nickel or copper alloy or a combination thereof Foil and the like.
  • the electrolyte solution which can be used in the present invention is formed by dissolving or dissociating an electrolyte salt having a structure such as A + B - in an electrolyte solvent.
  • a + is an alkali metal cation such as Li + , Na + , K + or these combination including ions consisting of
  • 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 - and comprising an ion composed of the same anion or combinations thereof
  • the electrolyte solvent is propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC), dipropyl carbonate (DPC), dimethyl sulfoxide, acetonitrile, dimethoxyethan
  • 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.
  • the electrode according to the present invention may optionally further include components such as a conductive material, a binder, and a filler as needed.
  • the conductive material uses acetylene black or carbon black, but is not limited thereto.
  • the binder used for the negative electrode and the positive electrode is polytetrafluoroethylene, polyvinylidene fluoride, polyvinyl fluoride, poly acrylonitrile, nitrile rubber, polybutadiene, polystyrene, styrene butadiene rubber, polysulfide rubber, butyl rubber, hydrogenated styrene butadiene It may be selected from the group consisting of rubber, nitro cellulose and carboxymethyl cellulose, but is not limited thereto.
  • a battery according to the present invention is prepared by a conventional method known in the art, for example, by dispersing an electrode active material and a binder in an organic solvent to produce a slurry, coating it on an electrode current collector, and then drying and compressing the same.
  • the electrode assembly is manufactured by interposing a separator therein, and a nonaqueous electrolyte is injected to prepare the electrode assembly.
  • PET polyethylene terephthalate
  • the surfactant Dowfax 2A1 (Dowchemicals, Inc.) was coated on only one surface of the specimen and then etched at 4 ° C. for 20 minutes at 4 M sodium hydroxide solution.
  • pores having an average pore diameter of 20 nm and 45 nm were formed at a time of 260 s / 100 cc aeration time, and the degree of curvature of the pores was measured as 1 when measured in cross section.
  • PET polyethylene terephthalate
  • pores having an average pore diameter of 30 nm were formed with an aeration time of 120 s / 100 cc, and the degree of curvature of the pores was measured as 1 when measured by a cross section.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Cell Separators (AREA)

Abstract

La présente invention concerne un film de séparation destiné à un dispositif électrochimique et son procédé de fabrication, les pores du film de séparation étant formés pour posséder une forme de cône tronqué dans le sens de l'épaisseur de sorte que les deux extrémités des pores possèdent des diamètres différents. Ainsi, étant donné qu'une surface possédant des pores de plus grand diamètre est tournée vers une anode, la présente invention résout le problème technique associé au colmatage du film de séparation par un sous-produit pendant le stockage et les tests cycliques d'une batterie secondaire et permet le fonctionnement à long terme d'un dispositif électrochimique.
PCT/KR2013/011038 2012-11-30 2013-11-29 Film de séparation destiné à un dispositif électrochimique et son procédé de fabrication Ceased WO2014084684A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR20120138413 2012-11-30
KR10-2012-0138413 2012-11-30
KR1020130147441A KR101522657B1 (ko) 2012-11-30 2013-11-29 전기화학소자용 분리막 및 그의 제조방법
KR10-2013-0147441 2013-11-29

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Publication Number Publication Date
WO2014084684A1 true WO2014084684A1 (fr) 2014-06-05

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PCT/KR2013/011038 Ceased WO2014084684A1 (fr) 2012-11-30 2013-11-29 Film de séparation destiné à un dispositif électrochimique et son procédé de fabrication

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3416211A1 (fr) * 2017-06-14 2018-12-19 Centre National De La Recherche Scientifique Membrane de polymer avec des pores de piste ioniques attaqués comme separateur de batterie
EP3321075A4 (fr) * 2015-07-09 2019-03-20 Nitto Denko Corporation Film de résine

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010041289A1 (en) * 2000-02-29 2001-11-15 Hikmet Rifat Ata Mustafa Lithium battery
WO2003058734A1 (fr) * 2002-01-03 2003-07-17 Neah Power Systems, Inc. Structures d'electrode de pile a combustible poreuses recouvertes de couches electriquement conductrices enrobantes
KR20080007692A (ko) * 2006-07-18 2008-01-23 주식회사 엘지화학 분리막으로서 감광성 고분자를 사용하는 리튬이온 폴리머전지
KR100925643B1 (ko) * 2006-04-28 2009-11-06 주식회사 엘지화학 겔 폴리머층을 포함하는 전지용 분리막
KR101040572B1 (ko) * 2010-10-11 2011-06-16 대한민국 셀룰로오스 나노섬유를 이용한 다공성 분리막 및 그 제조방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010041289A1 (en) * 2000-02-29 2001-11-15 Hikmet Rifat Ata Mustafa Lithium battery
WO2003058734A1 (fr) * 2002-01-03 2003-07-17 Neah Power Systems, Inc. Structures d'electrode de pile a combustible poreuses recouvertes de couches electriquement conductrices enrobantes
KR100925643B1 (ko) * 2006-04-28 2009-11-06 주식회사 엘지화학 겔 폴리머층을 포함하는 전지용 분리막
KR20080007692A (ko) * 2006-07-18 2008-01-23 주식회사 엘지화학 분리막으로서 감광성 고분자를 사용하는 리튬이온 폴리머전지
KR101040572B1 (ko) * 2010-10-11 2011-06-16 대한민국 셀룰로오스 나노섬유를 이용한 다공성 분리막 및 그 제조방법

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3321075A4 (fr) * 2015-07-09 2019-03-20 Nitto Denko Corporation Film de résine
EP3416211A1 (fr) * 2017-06-14 2018-12-19 Centre National De La Recherche Scientifique Membrane de polymer avec des pores de piste ioniques attaqués comme separateur de batterie
WO2018229235A1 (fr) * 2017-06-14 2018-12-20 Centre National De La Recherche Scientifique Membrane polymère poreuse à traces ioniques gravées en tant que séparateur pour une batterie
US12176476B2 (en) 2017-06-14 2024-12-24 Centre National De La Recherche Scientifique Porous etched ion-track polymer membrane as a separator for a battery

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