JP6818557B2 - 多孔性ポリオレフィン系分離膜およびその製造方法 - Google Patents
多孔性ポリオレフィン系分離膜およびその製造方法 Download PDFInfo
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- JP6818557B2 JP6818557B2 JP2016575432A JP2016575432A JP6818557B2 JP 6818557 B2 JP6818557 B2 JP 6818557B2 JP 2016575432 A JP2016575432 A JP 2016575432A JP 2016575432 A JP2016575432 A JP 2016575432A JP 6818557 B2 JP6818557 B2 JP 6818557B2
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- Prior art keywords
- separation membrane
- polyolefin
- stretching
- based separation
- pressure
- Prior art date
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Images
Classifications
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/20—Manufacture of shaped structures of ion-exchange resins
- C08J5/22—Films, membranes or diaphragms
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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
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
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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
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
- B29C55/14—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively
- B29C55/143—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial successively firstly parallel to the direction of feed and then transversely thereto
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Description
粘度平均分子量が600,000g/molの高密度ポリエチレン(High−density polyethylene、HDPE;三井化学社製品)を二軸押出機に供給した後、流動パラフィン(極東油化)を前記ポリエチレンとの重量比がポリエチレン30対流動パラフィン70となる量で前記二軸押出機に注入して押出した。
前記実施例1において、103℃で長手方向(Machine Direction、MD)延伸および105℃で幅方向(Transverse Direction、TD)延伸(延伸倍率:8.5(MD)×8.5(TD))したことを除いては、前記実施例1と同様の方法で厚さ12.3μmの分離膜を製造した。
前記実施例1において、120℃で長手方向(Machine Direction、MD)延伸および123℃で幅方向(Transverse Direction、TD)延伸(延伸倍率:8(MD)×8(TD))したことを除いては、前記実施例1と同様の方法で厚さ12.2μmの分離膜を製造した。
前記実施例2において、長手方向(Machine Direction、MD)延伸および幅方向(Transverse Direction、TD)延伸倍率を7(MD)×7(TD)としたことを除いては、前記実施例2と同様の方法で厚さ12.3μmの分離膜を製造した。
前記実施例1および2、並びに比較例1および2で製造された分離膜に対して、以下に開示された測定方法により、気孔度、通気度、引張強度、伸び率、収縮率、バブルポイントおよび平均ポイント圧力、および水滴接触角を測定し、その結果を表2に示した。
前記実施例および比較例で製造された分離膜それぞれを、直径26mmの円でサンプリングした。PMI社の毛細管流動気孔測定器に分離膜自体を装着後、GalwickTM溶液(表面張力15.9dyne/cm)に十分に浸す。前記機器をWet up Calc.modeに設定した後、圧力別のN2の流量の流れを測定して湿潤曲線を描く。前記湿潤曲線で最初のバブルが感知される圧力をバブルポイント圧力(psi)として記録する。また、前記実施例および比較例で製造された分離膜それぞれを、直径26mmの円でサンプリングし、前記機器に分離膜自体を装着後、前記機器をDry up Calc.modeに設定し、圧力別N2の流速を測定してこれを乾燥曲線グラフに示した。測定された乾燥曲線グラフで原点から直線性を有するポイントまで直線を延長し、前記直線の傾きの半分となる仮想の直線を描き、この仮想の直線と前記湿潤曲線との交わる地点の圧力を平均ポイント圧力(psi)として記録する。
前記実施例1および2、並びに比較例1および2で製造された各分離膜の10cm×10cmの試料を切取って、その体積(cm3)と質量(g)を求め、前記体積および質量と、分離膜の密度(g/cm3)から、次の式を用いて気孔度を計算した。
前記実施例および比較例で製造された分離膜それぞれを、直径1インチ(inch)の円が入る大きさに互いに異なる10個の地点で裁断した10個の試料を作製した後、通気度測定装置(旭精工社)を用いて、前記各試料で空気100ccの通過する時間を測定した。前記時間をそれぞれ5回ずつ測定した後、平均値を計算した。
前記実施例および比較例で製造された分離膜それぞれを、横(MD)10mm×縦(TD)50mmに互いに異なる10個の地点で裁断した10個の試料を作製した後、UTMに20mm部分を噛ませた後、上下に引いて強度を測定した。前記各試料の引張強度をそれぞれ3回ずつ測定した後、平均値を計算した。
前記実施例および比較例で製造された分離膜それぞれに対して、前記4.の引張強度の測定時、元の長さと破断点での長さとを比較して((破断点の長さ−20)/20mm)X100の値を百分率で表示する。
前記実施例および比較例で製造された分離膜それぞれを、横(MD)50mm×縦(TD)50mmに互いに異なる10個の地点で裁断した10個の試料を作製した。前記各試料を105℃のオーブンで1時間放置した後、各試料のMD方向およびTD方向の収縮程度を測定して、平均熱収縮率を計算した。
前記実施例および比較例で製造された分離膜それぞれを、横(MD)20mm×縦(TD)20mmに裁断して5個の試料を作製した。前記試料を接触角測定器(DSA−100、(株)マークテック貿易)に載せて水をスポイトで1滴落とした後、接触角を測定した。5個の試料の接触角は平均を出して計算した。
Claims (8)
- ポリオレフィン系樹脂を含有し、
毛細管流動気孔測定器(Capillary flow porometer)で測定した分離膜の湿潤および乾燥曲線で平均ポイント圧力(psi)/バブルポイント圧力(psi)の比が2.13〜2.4であり、
長手方向および幅方向の引張強度(kg/cm 2 )/伸び率(%)の比がそれぞれ15〜28であり、
通気度が50〜200sec/100cc以下であり、
前記平均ポイント圧力(psi)は、毛細管流動気孔測定器で乾燥直線を描き、前記乾燥直線で傾きが1/2となる仮想の直線と前記湿潤曲線との接する地点の圧力であり、
前記バブルポイント圧力(psi)は、毛細管流動気孔測定器で湿潤曲線が描かれる始点の圧力である、ポリオレフィン系分離膜。 - 前記分離膜の気孔度が40〜50%である、請求項1に記載のポリオレフィン系分離膜。
- 前記分離膜の水滴接触角が107°以下である、請求項1に記載のポリオレフィン系分離膜。
- 前記ポリオレフィン系樹脂が、粘度平均分子量が1×105〜9×105g/molの高密度ポリエチレンを含む、請求項1乃至3のいずれか1項に記載のポリオレフィン系分離膜。
- 前記ポリオレフィン系分離膜が、長手方向にT1温度でE1倍延伸および幅方向にT2温度でE2倍延伸されたもので、前記延伸時の温度条件が100℃<T1<115℃、100℃<T2<115℃、およびT2≧T1であり、前記延伸時の倍率条件がE1×E2=60〜80、E1≧7.5、およびE2≧8である、請求項1乃至3のいずれか1項に記載のポリオレフィン系分離膜。
- 前記倍率条件でE1/E2の比が0.85〜1である、請求項5に記載のポリオレフィン系分離膜。
- 請求項1乃至3のいずれか1項に記載のポリオレフィン系分離膜を含む電気化学電池。
- 前記電気化学電池は、リチウム二次電池である、請求項7に記載の電気化学電池。
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KR1020140080545A KR20160002447A (ko) | 2014-06-30 | 2014-06-30 | 다공성 폴리올레핀계 분리막 및 이의 제조 방법 |
PCT/KR2015/006201 WO2016003094A1 (ko) | 2014-06-30 | 2015-06-18 | 다공성 폴리올레핀계 분리막 및 이의 제조 방법 |
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JP7265349B2 (ja) * | 2018-12-07 | 2023-04-26 | 旭化成株式会社 | 微多孔膜の製造方法 |
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JP2005343958A (ja) * | 2004-06-01 | 2005-12-15 | Tonen Chem Corp | ポリエチレン微多孔膜の製造方法並びにその微多孔膜及び用途 |
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US20090226814A1 (en) * | 2008-03-07 | 2009-09-10 | Kotaro Takita | Microporous membrane, battery separator and battery |
US20110027660A1 (en) * | 2008-03-31 | 2011-02-03 | Hisashi Takeda | Polyolefin microporous film and roll |
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US8802272B2 (en) * | 2010-11-29 | 2014-08-12 | Takemoto Yushi Kabushiki Kaisha | Method of producing polyolefin microporous membrane and separator for lithium ion battery |
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