JP6542290B2 - 2軸延伸微細多孔質膜 - Google Patents
2軸延伸微細多孔質膜 Download PDFInfo
- Publication number
- JP6542290B2 JP6542290B2 JP2017115807A JP2017115807A JP6542290B2 JP 6542290 B2 JP6542290 B2 JP 6542290B2 JP 2017115807 A JP2017115807 A JP 2017115807A JP 2017115807 A JP2017115807 A JP 2017115807A JP 6542290 B2 JP6542290 B2 JP 6542290B2
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- JP
- Japan
- Prior art keywords
- membrane
- tensile strength
- film
- range
- stretching
- 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.)
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Links
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- 239000012528 membrane Substances 0.000 claims description 62
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- 239000011148 porous material Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 10
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- 239000002245 particle Substances 0.000 claims description 9
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- 230000015572 biosynthetic process Effects 0.000 claims description 4
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- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920001021 polysulfide Polymers 0.000 claims description 3
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 7
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- ROGIWVXWXZRRMZ-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical compound CC(=C)C=C.C=CC1=CC=CC=C1 ROGIWVXWXZRRMZ-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- 238000000137 annealing Methods 0.000 description 2
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 2
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- 239000005995 Aluminium silicate Substances 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
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- 239000004593 Epoxy Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 229920007925 Ethylene chlorotrifluoroethylene (ECTFE) Polymers 0.000 description 1
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
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- 238000010622 cold drawing Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 239000003431 cross linking reagent Substances 0.000 description 1
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- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- QHSJIZLJUFMIFP-UHFFFAOYSA-N ethene;1,1,2,2-tetrafluoroethene Chemical group C=C.FC(F)=C(F)F QHSJIZLJUFMIFP-UHFFFAOYSA-N 0.000 description 1
- 239000004715 ethylene vinyl alcohol Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
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- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
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- 239000000446 fuel Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- RZXDTJIXPSCHCI-UHFFFAOYSA-N hexa-1,5-diene-2,5-diol Chemical compound OC(=C)CCC(O)=C RZXDTJIXPSCHCI-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
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- 229920000092 linear low density polyethylene Polymers 0.000 description 1
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- 239000004702 low-density polyethylene Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 229910052618 mica group Inorganic materials 0.000 description 1
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- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical class CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
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- 238000010094 polymer processing Methods 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
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- 239000011115 styrene butadiene Substances 0.000 description 1
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- 239000000080 wetting agent Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
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- B32—LAYERED PRODUCTS
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- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
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- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
-
- 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
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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
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249955—Void-containing component partially impregnated with adjacent component
- Y10T428/249958—Void-containing component is synthetic resin or natural rubbers
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249975—Void shape specified [e.g., crushed, flat, round, etc.]
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Textile Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Cell Separators (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Fuel Cell (AREA)
- Laminated Bodies (AREA)
Description
New York, NY, (1985)を参照されたい。微細多孔質膜を製造するための3つの商業的に
実行可能なプロセスとしては、乾燥−延伸法(CELGARDプロセスとしても知られる)、湿式法及び粒子延伸法がある。
は、湿式法及び粒子延伸法と異なる。一般的に、湿式法(いくつか挙げれば、相転化法、または抽出法もしくはTIPS法としても知られる)においては、高分子原材料がプロセス油(しばしば、可塑剤と呼ばれる)と混合され、この混合物は押し出され、次いで、プロセス油が除去されるとき孔が生成する(この薄膜は、油の除去前又は後に延伸される)。本明細書において、引用文献として組み込まれるKesting, Ibid. p. 237-286を参照。
一般的に、粒子延伸法においては、重合性原材料は粒子と混合され、この混合物は押し出され、延伸の過程において延伸力によってポリマーと粒子間の境界に割れが生じるときに孔が生成する。本明細書において、引用文献として組み込まれる米国特許第6,057,061号明細書及び米国特許第6,080,507号明細書を参照。
Polymeric Membranes, A structural perspective, Second Edition, John Wiley & Sons, New York, NY, (1985) p. 290-297を参照。乾燥−延伸法は、上述したように、湿式法及び粒子延伸法とは異なる。
の比であるアスペクト比によって特徴付けられる。本発明の膜の1つの実施態様において、アスペクト比は0.75〜1.25の範囲である。これは、5.0を超える従来の乾燥−延伸膜のアスペクト比と対比される。下記の表を参照されたい。
いて、0.5〜5.0の間である。この比率は、10.0を超える従来技術の膜の対応する比と対比される。下記の表を参照されたい。
横方向の引張り強度である。上記の値は例示の値であり、これに限定されるものではなく、したがって、本発明の膜の単なる代表例として見るべきである。
、水酸化アンモニウム、アルミナ3水和物、及び燐酸エステルのような難燃剤、(7)架橋又はカップリング剤、(8)ポリマー加工助剤、及び(9)ポリプロピレンのためのベータ核剤を含むいずれかの種類の核剤がある。(しかしながら、本発明の膜は、本明細書に引用文献として組み込まれる米国特許第6,602,593号明細書に開示されるベータ核化ポリプロピレンを特定的に除く。ベータ核化ポリプロピレンはポリプロピレン中のベータ結晶の生成を引き起す物質である。)
てTm−50℃とTm−15℃の間の温度で実施することができる。いくつかの材料、例えば、ポリブテンのような押出し後に高い結晶性を有するものはアニーリングを必要としない。
施することができ、他の実施態様においてTm−80℃未満で実施することができる。1
つの実施態様において熱間延伸はTm−10℃未満で実施することができる。1つの実施
態様において、総縦方向延伸率は50〜500%の範囲であってもよく、他の実施態様において、100〜300%の範囲であってもよい。縦方向延伸の過程では、前駆体は横方向に収縮することがある(従来法)。
るとき、前駆体は同時に縦方向には制御された態様で、収縮が可能となる(すなわち、緩和される)ことを意味する。横方向延伸は冷間工程又は熱間工程又はこれらの組合せで行うことができる。1つの実施態様において、総横方向延伸率は、100〜1200%の範囲、他の実施態様においては、200〜900%の範囲であり得る。1つの実施態様において、制御された縦方向の緩和率は5〜80%の範囲であってもよく、他の実施態様においては、15〜65%の範囲であってもよい。1つの実施態様において、横方向延伸は複数の工程で実施され得る。横方向延伸の過程において、前駆体は縦方向に収縮することが可能であってもよく、又は可能でなくともよい。複数工程の横方向延伸の実施態様においては、第1の横方向工程は、制御された縦方向緩和を伴う横方向延伸、これに続いて横方向及び縦方向の同時延伸、さらにこれに続いて横方向に緩和し、縦方向には延伸及び緩和を行わない工程を含むことができる。
伸される。最終の薄膜は19.4ミクロンの厚さ及び63%の空隙率を有する。最終薄膜のTD引張り強度は350kg/cm2である。図2を参照。
℃である。次いで、溶融したポリマーは215℃に設定された同時押出しダイに供給される。溶融したポリマーは吹込空気によって冷却される。押出された薄膜は40ミクロンの厚さを有し、0.0110の複屈折率を有する。次いで、押出された前駆体は105℃で2分間アニールされる。次いで、アニールされた薄膜は室温で36%まで冷間延伸され、次いで264%まで熱間圧延され、109℃で29%まで緩和される(総縦方向延伸率=271%)。MD延伸薄膜は、厚さ23.8ミクロン、空隙率29.6%を有する。次いで、MD延伸薄膜は、75%のMD緩和を伴いながら110℃で1034%TD延伸される。最終の薄膜は16.8ミクロンの厚さ及び46%の空隙率を有する。最終薄膜のTD引張り強度は1037kg/cm2である。
Claims (8)
- ほぼ丸い形状の孔を有し、(縦方向の引張り強度)/(横方向の引張り強度)の比が0.6〜3.8の範囲であり、厚さが24ミクロン未満である層を少なくとも一つ含む多層微細多孔質ポリオレフィン薄膜から構成され、孔形成に必要な油及び粒子を使用しない、膜。
- 横方向の引張り強度は286Kg/cm2以上である、請求項1に記載の膜。
- 前記微細多孔質ポリオレフィン薄膜の空隙率は37〜63%の範囲である、請求項1又は2に記載の膜。
- 前記(縦方向の引張り強度)/(横方向の引張り強度)比が0.9〜1.8の範囲であり、前記横方向の引張り強度が350Kg/cm2以上であり、前記ほぼ丸い形状の孔が0.75〜1.25の範囲のアスペクト比を有する、請求項1〜3のいずれかに記載の膜。
- 前記微細多孔質ポリオレフィン薄膜の平均孔径は、0.03〜0.30ミクロンの範囲である、請求項1〜4のいずれかに記載の膜。
- 前記ポリオレフィンは、20〜80%の範囲の結晶性を有する半結晶質ポリマーである、請求項1〜5のいずれかに記載の膜。
- 前記ポリオレフィンは、フルオロカーボン、ポリアミド、ポリエステル、ポリアセタール(又はポリオキシメチレン)、ポリスルフィド、ポリビニルアルコール、これらのコポリマー及びこれらの組合せからなる群より選択されるポリマーとの混合物である、請求項1〜5のいずれかに記載の膜。
- 請求項1〜7のいずれかに記載の膜を含む電池セパレータ。
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