WO2016159658A1 - Membrane de séparation multicouche à base de cellulose - Google Patents

Membrane de séparation multicouche à base de cellulose Download PDF

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Publication number
WO2016159658A1
WO2016159658A1 PCT/KR2016/003270 KR2016003270W WO2016159658A1 WO 2016159658 A1 WO2016159658 A1 WO 2016159658A1 KR 2016003270 W KR2016003270 W KR 2016003270W WO 2016159658 A1 WO2016159658 A1 WO 2016159658A1
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WO
WIPO (PCT)
Prior art keywords
cellulose
secondary battery
polyethylene
battery separator
resin
Prior art date
Application number
PCT/KR2016/003270
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English (en)
Korean (ko)
Inventor
박종필
김종훈
Original Assignee
주식회사 엘지화학
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
Priority claimed from KR1020160037844A external-priority patent/KR101894134B1/ko
Application filed by 주식회사 엘지화학 filed Critical 주식회사 엘지화학
Priority to JP2017562951A priority Critical patent/JP6685331B2/ja
Priority to US15/545,129 priority patent/US10586967B2/en
Publication of WO2016159658A1 publication Critical patent/WO2016159658A1/fr

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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
    • 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
    • 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
    • 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
    • H01M50/497—Ionic conductivity
    • 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 secondary battery separator, and more particularly to a secondary battery separator with improved shutdown function.
  • 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.
  • the lithium secondary battery is composed of a positive electrode, a negative electrode, an electrolyte, and a separator.
  • a required characteristic of the separator is to separate the positive electrode and the negative electrode and to electrically insulate the lithium ion based on its high porosity.
  • the separator used may be a polyolefin-based material or cellulose.
  • Polyolefin-based polymer substrates are advantageous for pore formation and excellent in chemical resistance, mechanical properties, and thermal properties, but have severe heat shrinkage at high temperatures and are physically weak.
  • the cellulose substrate may be manufactured as a separator having a physically high strength, but has a problem in that it cannot act to cut off current in an abnormal operating environment.
  • the present invention has been made in view of the prior art as described above, and an object of the present invention is to provide a secondary battery separator and a method of manufacturing the same that can improve the shutdown function of the cellulose-based separator having a physically high strength.
  • the base material layer It is provided on one side or both sides of the said base material layer, and is provided with the resin layer which consists of polyolefin resin.
  • the polyolefin resin may be at least one selected from the group consisting of polyethylene, polypropylene, polybutylene, and polypentene.
  • the polyethylene nanoparticles may have a melting point of 80 to 100 ° C.
  • the polyolefin resin may have a melting point of 100 to 140 ° C.
  • the resin layer may further include inorganic particles and a polymer binder.
  • the resin layer may be laminated in a lamination method.
  • the resin layer may have a thickness of 3 to 20 ⁇ m, and the base layer may have a thickness of 5 to 20 ⁇ m.
  • the cellulose-based nanofibers may be made of one selected from the group consisting of cellulose acetate, cellulose triacetate and cellulose butyrate.
  • the diameter of the cellulose-based nanofibers is 10 nm to 500 nm, the length is 1 ⁇ m to 10 mm, the polyethylene nanoparticles may have a particle size of 50 nm to 500 nm.
  • the cellulose-based nanofibers and polyethylene nanoparticles may be included in a weight ratio of 7: 3 to 9: 1.
  • the method for producing a secondary battery separator according to the present invention using a mixture of cellulose nanofibers and polyethylene nanoparticles dispersed in a solvent, preparing a sheet; Removing the solvent of the mixture to prepare a porous base layer; And laminating a resin layer made of a polyolefin resin on one or both surfaces of the substrate layer in a lamination method.
  • the solvent may be the one paper phase selected from the group consisting of water, methyl alcohol, ethyl alcohol, propyl alcohol, acetone, ethyl acetate, methyl ethyl ketone and toluene to the pore-forming resin.
  • the pore-forming resin may be at least one selected from the group consisting of polyethylene glycol, polyvinyl talcol, and polyvinyl propylene.
  • Separation membrane according to the present invention has a high physical strength and excellent safety, it is possible to ensure a high safety by improving the shutdown function.
  • FIG. 1 is a view schematically showing a cross-sectional structure of a separator according to an aspect of the present invention.
  • the present invention can provide a shutdown function by providing a resin layer made of a polyolefin resin on at least one surface of the base material layer containing cellulose nanofibers, and has a relatively low melting point in the base material layer containing cellulose nanofibers.
  • the shutdown characteristic can be further improved.
  • the separator 100 for a secondary battery includes a base layer 110 including cellulose-based nanofibers and polyethylene nanoparticles; And a resin layer 120 made of polyolefin resin formed on both surfaces of the substrate layer.
  • the polyethylene nanoparticles included in the base layer may have a melting point of 80 to 100 ° C. and a particle size of 50 nm to 500 nm. Unlike conventional polyethylene, the polyethylene nanoparticles may have a relatively low melting point, thereby improving shutdown characteristics of a separator including a cellulose substrate. In addition, the polyethylene nanoparticles may have an average molecular weight of 500 g / mole to 900 g / mole.
  • polyethylene nanoparticles will be described in detail below, for example, but not limited thereto.
  • Ni-methyl complex (Me (OCH 2 CH 2 ) n NH 2 ) was added to 100 ml of distilled water at room temperature, and the mixture was stirred for 2 minutes to prepare a uniform solution.
  • the solution was placed in a pressurized reactor at a pressure of 40 bar and under stirring, a constant amount of ethylene was continuously injected.
  • the polyethylene nanoparticles may be prepared in the form of nanoparticles using a Ni catalyst, prepared in the form of PE magnetic composite particles with iron oxide particles, and then prepared by a method of removing metal components through acid treatment. Can be.
  • the cellulose-based nanofibers and polyethylene nanoparticles may be included in a weight ratio of 7: 3 to 9: 1. When the weight ratio is satisfied, it may be easily prepared as a separator without interfering with the binding between the cellulose nanofibers, and may provide an appropriate level of shutdown characteristics.
  • the resin layer may be formed in a film form and formed on one or both sides of the base layer in a lamination method.
  • a lamination method a method in which a polymer resin is dissolved and applied to a solvent is used, and a process is long and productivity is low.
  • the resin layer is manufactured in the form of a film and laminated in a lamination manner, so that it is not necessary to use a solvent, thereby simplifying the process.
  • characteristics, such as thickness, porosity, and composition of a resin layer can be adjusted easily.
  • the resin layer may have a thickness of 3 to 20 ⁇ m, and the base layer may have a thickness of 5 to 20 ⁇ m.
  • the polyolefin resin may be at least one selected from the group consisting of polyethylene, polypropylene, polybutylene and polypentene.
  • the polyethylene may be low density polyethylene (LDPE).
  • the polyolefin resin may be one having a melting point of 100 to 140 ° C.
  • the resin layer may further include inorganic particles and a polymer binder.
  • 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 are not particularly limited as long as the oxidation and / or reduction reactions do not occur in the operating voltage range (for example, 0 to about 5 V on the basis of Li / Li + ) of the applied electrochemical device. In particular, in the case of using the inorganic particles having the ion transport ability, it is possible to improve the performance by increasing the ion conductivity in the 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 may include high dielectric constant inorganic particles having a dielectric constant of about 5 or more, such as about 10 or more, inorganic particles having a lithium ion transfer ability, or a mixture thereof.
  • inorganic particles having a dielectric constant of about 5 or more include BaTiO 3 , Pb (Zr, Ti) O 3 (PZT), Pb 1 - x La x Zr 1 - y Ti y O 3 (PLZT), PB (Mg 1/3 Nb 2/3 ) O 3 -PbTiO 3 (PMN-PT), Hafnia (HfO 2 ), SrTiO 3 , SnO 2 , CeO 2 , MgO, NiO, CaO, ZnO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , TiO 2 , SiC, boehmite or mixtures thereof.
  • the inorganic particles having a lithium ion transfer capacity refers to inorganic particles containing lithium elements but having a function of transferring lithium ions without storing lithium, and the inorganic particles having lithium ion transfer ability are present in the particle structure. Since the lithium ions can be transferred and moved due to a kind of defect, the lithium ion conductivity in the battery is improved, thereby improving battery performance.
  • Non-limiting examples of the inorganic particles having a lithium ion transfer capacity is 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 (LixAlyTiz (PO 4 ) 3 , 0 ⁇ x ⁇ 2, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 3), 14Li 2 O-9Al 2 O 3 -38TiO 2 -39P 2 O 5 , etc.
  • LiAlTiP lithium lanthanum titanate
  • Li x La y TiO 3 Li 3 . 25 Ge 0 .25 P 0.
  • the polymer binder may be polymethylmethacrylate, polyacrylonitrile, polyvinylpyrrolidone, polyvinylacetate, ethylene-co-vinyl acetate, Polyethylene oxide, cellulose acetate, cellulose acetate butyrate, cellulose acetate propionate, cyanoethylpullulan, cyanoethylpolyvinyl alcohol (cyanoethylpolyvinylalcohol), cyanoethylcellulose, cyanoethylsucrose, pullulan, carboxyl methyl cellulose, acrylonitrile-styrene-butadiene copolymer (acrylonitrile-styrene-butadiene copolymer, polyimide, etc. Or combinations thereof, but can be used by mixing two or more kinds, without being limited thereto.
  • the cellulose-based nanofibers are ethyl cellulose (Ethylcellulose), methyl cellulose (Methylcellulose), hydroxypropyl cellulose (Hydroxypropyl cellulose), hydroxyethyl cellulose (Hydroxyethyl cellulose), hydroxypropyl methyl cellulose (Hydroxypropyl methyl cellulose), hydroxyethyl Hydroxyethyl methyl cellulose, Carboxymethyl cellulose, Cellulose acetate, Cellulose triacetate, Cellulose acetate phthalate, Nitrocellulose, Cellulose acetate , Cellulose acetate propionate and their ammonium or salts.
  • the diameter of the cellulose-based nanofibers may be 10 to 500 nm, the length may be 1 ⁇ m to 10 mm.
  • the method for producing a secondary battery separator using a mixture of cellulose nanofibers and polyethylene nanoparticles dispersed in a solvent, preparing a sheet; Removing the solvent of the sheet to prepare a porous base layer; And laminating a resin layer made of polyolefin resin on one or both surfaces of the substrate layer in a lamination method.
  • the method of manufacturing a separator for a secondary battery is provided.
  • the porosity and thickness of the substrate layer can be easily adjusted.
  • the cellulose nanofibers and the solvent may be included in a weight ratio of 6: 4 to 8: 2.
  • the solvent is a pore-forming resin to bind the cellulose nanofibers, and includes a pore-forming resin to form a porous structure of the substrate layer, water, methyl alcohol, ethyl alcohol, propyl alcohol, acetone, ethyl acetate, methyl ethyl ketone And toluene may further comprise one paper selected from the group consisting of.
  • the pore-forming resin may be used one or more selected from the group consisting of polyethylene glycol, polyvinyl talcol and polyvinyl propylene.
  • a mixture obtained by dispersing cellulose nanofibers and polyethylene nanoparticles in a solvent may be passed through a homogenizer to prepare a suspension, which may be prepared in a sheet form by reducing the pressure.
  • the sheets produced exhibit high tensile strength through strong hydrogen bonding between cellulose fibers.
  • the number of passes through the homogenizer may be 5 to 20 cycles. After decompression, the cellulose fibers are uniformly arranged to form a sheet of porous structure.
  • the porous sheet is formed by using at least one selected from the group consisting of water, methyl alcohol, ethyl alcohol, propyl alcohol, acetone, ethyl acetate, methyl ethyl ketone, and toluene.
  • the washing step can be performed.
  • the sheet is dried, and the solvent of the sheet is removed to prepare a substrate layer having a porous structure.
  • the drying process of the sheet may be performed at 40 ° C. to 80 ° C., in an air or inert gas or vacuum environment for 1 to 30 hours.
  • the process of drying the sheet may be performed in air at a temperature of 50 to 70 ° C. for 20 to 30 hours.
  • the solvent is removed through the drying process, and the portion from which the solvent is removed forms voids.
  • the drying of the sheet may include a process of dehydration drying using a vacuum filter, but is not limited thereto.
  • an electrochemical device including an anode, a cathode, and the aforementioned separator interposed between the anode and the cathode may be manufactured.
  • the electrochemical device of the present invention includes all devices that undergo an electrochemical reaction, and specific examples include capacitors such as all kinds of primary cells, secondary batteries, fuel cells, solar cells, or supercapacitor 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 is preferable among the secondary batteries.
  • Anodes, cathodes and the like can be readily prepared by processes and / or methods known in the art.
  • the positive electrode is prepared by, for example, applying a mixture of a positive electrode active material, a conductive agent, and a binder onto a positive electrode current collector, followed by drying, and optionally, a filler is further added to the mixture.
  • the positive electrode is manufactured in a form in which a positive electrode active material is bound to a positive electrode current collector according to a conventional method known in the art.
  • the negative electrode is manufactured in a form in which the negative electrode active material is bound to the negative electrode current collector according to conventional methods known in the art.
  • the negative electrode active material may be, for example, carbon such as hardly graphitized carbon or graphite carbon; Li x Fe 2 O 3 (0 ⁇ x ⁇ 1), Li x WO 2 (0 ⁇ x ⁇ 1), Sn x Me 1 - x Me ' y O z (Me: Mn, Fe, Pb, Ge; Me' Al, B, P, Si, a group 1, 2, 3 element of the periodic table, a halogen, a metal complex oxide of 0 ⁇ x ⁇ 1;1 ⁇ y ⁇ 3;1 ⁇ z ⁇ 8; Lithium metal; Lithium alloys; Silicon-based alloys; Tin-based alloys; SnO, SnO 2 , PbO, PbO 2 , Pb 2 O 3 , Pb 3 O 4 , Sb 2 O 3 , Sb 2 O 4 , Sb 2 O
  • a + comprises Li +, Na +, an alkali metal cation or an ion composed of a combination thereof, such as K + and 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 -
  • Salts containing ions consisting of anions such as C (CF 2 SO 2 ) 3 - or combinations thereof include propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC), Dipropyl carbonate (DPC), dimethyl sulfoxide, acetonitrile, dimethoxyethane, diethoxyethane, tetrahydrofuran, N-methyl-2-pyrrolidone (PC), propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (D
  • the injection of the electrolyte may be performed at an appropriate step in the battery manufacturing process, depending on the manufacturing process and the required physical properties of the final product.
  • a lamination (stack) and folding process of the separator and the electrode may be performed in addition to the general winding process.

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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 une membrane de séparation destinée à une batterie secondaire permettant d'améliorer une fonction d'arrêt d'une membrane de séparation multicouche à base de cellulose présentant une résistance physique élevée, et concerne plus particulièrement une membrane de séparation destinée à une batterie secondaire comprenant : une couche de base constituée de nanofibres à base de cellulose et de nanoparticules de polyéthylène ; et une couche de résine formée sur une surface ou sur les deux surfaces de la couche de base, et constituée d'une résine de polyoléfine.
PCT/KR2016/003270 2015-03-30 2016-03-30 Membrane de séparation multicouche à base de cellulose WO2016159658A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2017562951A JP6685331B2 (ja) 2015-03-30 2016-03-30 セルロース系多層分離膜
US15/545,129 US10586967B2 (en) 2015-03-30 2016-03-30 Cellulose-based multilayer separator

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2015-0044449 2015-03-30
KR20150044449 2015-03-30
KR1020160037844A KR101894134B1 (ko) 2015-03-30 2016-03-29 셀룰로오스계 다층 분리막
KR10-2016-0037844 2016-03-29

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WO2016159658A1 true WO2016159658A1 (fr) 2016-10-06

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111691069A (zh) * 2020-05-18 2020-09-22 苏州大学 一种耐穿刺纤维复合膜及其制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101040572B1 (ko) * 2010-10-11 2011-06-16 대한민국 셀룰로오스 나노섬유를 이용한 다공성 분리막 및 그 제조방법
KR20120109257A (ko) * 2011-03-28 2012-10-08 삼성전기주식회사 이차 전지 섬유상 분리막 및 그 제조 방법
KR20140078966A (ko) * 2012-12-18 2014-06-26 (주) 파이브레인 이차전지용 복합부직포 분리막 및 제조방법
KR20140085728A (ko) * 2012-12-27 2014-07-08 유펙스켐(주) 폴리올레핀 미세 다공막
KR20140146094A (ko) * 2012-07-27 2014-12-24 디아이씨 가부시끼가이샤 변성 셀룰로오스 나노 파이버 함유 폴리에틸렌 미다공막, 세퍼레이터, 및 그것을 사용한 리튬 이온 전지

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101040572B1 (ko) * 2010-10-11 2011-06-16 대한민국 셀룰로오스 나노섬유를 이용한 다공성 분리막 및 그 제조방법
KR20120109257A (ko) * 2011-03-28 2012-10-08 삼성전기주식회사 이차 전지 섬유상 분리막 및 그 제조 방법
KR20140146094A (ko) * 2012-07-27 2014-12-24 디아이씨 가부시끼가이샤 변성 셀룰로오스 나노 파이버 함유 폴리에틸렌 미다공막, 세퍼레이터, 및 그것을 사용한 리튬 이온 전지
KR20140078966A (ko) * 2012-12-18 2014-06-26 (주) 파이브레인 이차전지용 복합부직포 분리막 및 제조방법
KR20140085728A (ko) * 2012-12-27 2014-07-08 유펙스켐(주) 폴리올레핀 미세 다공막

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111691069A (zh) * 2020-05-18 2020-09-22 苏州大学 一种耐穿刺纤维复合膜及其制备方法
CN111691069B (zh) * 2020-05-18 2021-10-08 苏州大学 一种耐穿刺纤维复合膜及其制备方法

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