JP6877130B2 - 多孔性接着層を含む分離膜およびこれを含む電気化学電池 - Google Patents
多孔性接着層を含む分離膜およびこれを含む電気化学電池 Download PDFInfo
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- JP6877130B2 JP6877130B2 JP2016237500A JP2016237500A JP6877130B2 JP 6877130 B2 JP6877130 B2 JP 6877130B2 JP 2016237500 A JP2016237500 A JP 2016237500A JP 2016237500 A JP2016237500 A JP 2016237500A JP 6877130 B2 JP6877130 B2 JP 6877130B2
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- separation membrane
- polyvinylidene fluoride
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Images
Classifications
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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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
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- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Cell Separators (AREA)
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- Health & Medical Sciences (AREA)
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Description
転写率(%)=(A1/A0)×100 (式1)
(充電)4.35V、0.2C、50mA cut−off、5時間
(放電)0.2C、3V cut−off、5時間
(充電)0.5C、4V cut−off、2時間
(実施例1)
<1.多孔性接着層組成物の製造>
重量平均分子量が約500,000、ヘキサフルオロプロピレン(HFP)含有量が12重量%の第1ポリビニリデンフルオライド系重合体(Solef21216、Solvay社)を、アセトン(大井化金社)に10重量%となるように溶解させ、撹拌機を用いて、25℃で4時間撹拌し、第1ポリビニリデンフルオライド系重合体溶液を製造した。
製造された接着層組成物を、厚さ9μmのポリエチレン単一膜の基材フィルムの両面にディップコーティング方式でコーティングした後、これを、乾燥温度80℃、風速15m/秒の条件で0.03時間乾燥処理して、接着層の総厚さが2μmの分離膜を製造した。
実施例1において、第1ポリビニリデンフルオライド系重合体溶液と第2ポリビニリデンフルオライド系重合体溶液とを、各重合体が3:7の重量比を有するように混合したことを除いては、実施例1と同様に、接着層組成物および分離膜を製造した。
実施例1において、第1ポリビニリデンフルオライド系重合体溶液と第2ポリビニリデンフルオライド系重合体溶液とを、各重合体が5:5の重量比を有するように混合し、アルミナ(Al2O3、日本軽金属社、日本)を、アセトンに25重量%添加し、ボールミルを用いて、25℃で3時間ミリングして製造した無機分散液を、第1および第2ポリビニリデンフルオライド系重合体:アルミナの重量比が5:5となるように混合したことを除いては、実施例1と同様に、接着層組成物および分離膜を製造した。
実施例1において、重量平均分子量が約1,100,000、アクリル酸(AA)含有量が1重量%以内の第2ポリビニリデンフルオライド系重合体の代わりに、重量平均分子量が約1,000,000、カルボキシル基含有量が約1重量%の第2ポリビニリデンフルオライド系重合体(KF9300、Kureha製造会社)を使用したことを除いては、実施例1と同様に実施して、接着層組成物および分離膜を製造した。
実施例1において、第1ポリビニリデンフルオライド系重合体溶液を使用せず、第2ポリビニリデンフルオライド系重合体溶液のみを使用したことを除いては、実施例1と同様に実施して、比較例1の接着層組成物および分離膜を製造した。
実施例1において、第2ポリビニリデンフルオライド系重合体溶液を使用せず、第1ポリビニリデンフルオライド系重合体溶液のみを使用したことを除いては、実施例1と同様に実施して、比較例2の接着層組成物および分離膜を製造した。
実施例1において、第2ポリビニリデンフルオライド系重合体溶液の代わりに、重量平均分子量が約1,600,000、ヘキサフルオロプロピレン(HFP)含有量が1重量%以内のポリビニリデンフルオライド系バインダー(HSV500、Arkema社)を、アセトン/DMAc混合溶液(アセトン:DMAcの重量比=10:90)に8重量%となるように溶解させ、撹拌機を用いて、25℃で4時間撹拌して製造されたポリビニリデンフルオライド系バインダー溶液を使用したことを除いては、実施例1と同様に実施して、比較例3の接着層組成物および分離膜を製造した。
前記製造された実施例1乃至4および比較例1乃至3の分離膜に対して、下記の方法で物性を測定し、その結果を表2および表3に示す。
前記実施例および比較例で製造された分離膜のそれぞれを、直径1インチ(inch)以上の円が入る大きさに、互いに異なる10の地点で裁断した10個の試験片を作製した後、通気度測定装置EG01−55−1MR(Asahi Seiko社)を用いて、前記各試験片で空気100ccが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、平均値を計算して通気度(sec/100cc)を測定した。
正極活物質としてLCO(LiCoO2)を、厚さ20μmのアルミニウム箔に厚さ94μmにコーティングし、乾燥、圧延して、総厚さ114μmの正極を製造した。負極活物質として天然黒鉛と人造黒鉛(1:1)を、厚さ10μmの銅箔に厚さ120μmにコーティングし、乾燥、圧延して、総厚さ130μmの負極を製造した。電解液としては、EC/EMC/DEC+0.2%LiBF4+5.0%FEC+1.0%VC+3.00%SN+1.0%PS+1.0%SAの有機溶媒に混合された1.5M LiPF6(PANAX ETEC CO.,LTD.)を使用した。
(充電)4.35V、0.2C、50mA cut−off、5時間
(放電)0.2C、3V cut−off、5時間
(充電)0.5C、4V cut−off、2時間
前記面積(A1)を分離膜の全体面積(A0)で割り、100を掛け算して、正極または負極活物質の分離膜への転写率(%)を計算した。
韓国工業規格KS−A−01107(粘着テープおよび粘着シートの試験方法)の8項により試験を行った。前記実施例および比較例で製造された分離膜のそれぞれを幅25mm、長さ250mmに裁断し、両面にそれぞれテープ(nitto31B)を貼り付けて試験片を作った後、2kg荷重の圧着ローラを用いて、300mm/分の速度で1回往復させて試験片を圧着させた。圧着後30分経過後、試験片を180°ひっくり返して約25mmを剥がした後、分離膜と分離膜の一面に貼り付けられたテープを引張強度機(Instron Series 1X/s Automated materials Tester−3343、Instron)の上側クリップに固定させた。分離膜の他面に貼り付けられたテープは下側クリップに固定させた後、60mm/分の引張速度で引っ張って、多孔性接着層が多孔性基材から剥がされる時の圧力を測定した。
韓国工業規格KS−A−01107(粘着テープおよび粘着シートの試験方法)の8項により試験を行った。各製造された分離膜フィルムを幅25mm、長さ250mmに裁断し、分離膜の一面にテープ(nitto31B)を貼り付けて試験片を作った後、他の一面に正極フィルム(LCO(lithium cobalt oxide)正極活物質/バインダーのスチレンブタジエンゴム(SBR)+カルボキシメチルセルロース(CMC)/導電剤(carbon black)=95/2.5/2.5)を、2kg荷重の圧着ローラを用いて、300mm/分の速度で1回往復させて試験片を圧着させた。圧着後30分経過後、試験片を180°ひっくり返して約25mmを剥がした後、分離膜と分離膜の一面に貼り付けられたテープを引張強度機(Instron Series 1X/s Automated materials Tester−3343、Instron)の上側クリップに固定させた。分離膜の他面の正極フィルムは下側クリップに固定させた後、60mm/分の引張速度で引っ張って、正極フィルムが分離膜から剥がされる時の圧力を測定した。
韓国工業規格KS−A−01107(粘着テープおよび粘着シートの試験方法)の8項により試験を行った。各製造された分離膜フィルムを幅25mm、長さ250mmに裁断し、分離膜の一面にテープ(nitto31B)を貼り付けて試験片を作った後、他の一面に負極フィルム(natural graphite負極活物質/バインダー(スチレンブタジエンゴム(SBR)+カルボキシメチルセルロース(CMC)5%)/導電剤(carbon black)=98/1/1)を、2kg荷重の圧着ローラを用いて、300mm/分の速度で1回往復させて試験片を圧着させた。圧着後30分経過後、試験片を180°ひっくり返して約25mmを剥がした後、分離膜と分離膜の一面に貼り付けられたテープを引張強度機(Instron Series 1X/s Automated materials Tester−3343、Instron)の上側クリップに固定させた。分離膜の他面の負極フィルムは下側クリップに固定させた後、60mm/分の引張速度で引っ張って、負極フィルムが分離膜から剥がされる時の圧力を測定した。
Claims (9)
- 多孔性基材と、前記多孔性基材の一面あるいは両面に形成された多孔性接着層とを含む分離膜であって、
前記多孔性接着層は、(A)ポリビニリデンフルオライド系ホモポリマー;およびビニリデンフルオライド単量体由来単位とヘキサフルオロプロピレン単量体由来単位とを含むポリビニリデンフルオライド系コポリマーのうちの1種以上である第1ポリビニリデンフルオライド(Polyvinylidene fluoride、PVdF)系重合体、並びに
(B)(メタ)アクリレート単量体由来単位、またはエポキシ基、ヒドロキシ基、カルボキシル基、エステル基、および酸無水物基からなる群より選択された1つ以上の基を含有する1種以上の単量体由来単位(b1)と、ビニリデンフルオライド単量体由来単位(b2)とを含む第2ポリビニリデンフルオライド系重合体を含み、
前記(A)第1ポリビニリデンフルオライド系重合体と前記(B)第2ポリビニリデンフルオライド系重合体は、2:8または3:7の重量比として含まれるリチウム二次電池用の分離膜。 - 前記(A)第1ポリビニリデンフルオライド系重合体は前記ポリビニリデンフルオライド系コポリマーを含み、前記ポリビニリデンフルオライド系コポリマー中の前記ヘキサフルオロプロピレンの含有量が、前記コポリマーの総重量を基準として、5重量%以上20重量%以下である、請求項1に記載のリチウム二次電池用の分離膜。
- 前記(B)第2ポリビニリデンフルオライド系重合体の重量を基準として、前記(メタ)アクリレート単量体由来単位、またはエポキシ基、ヒドロキシ基、カルボキシル基、エステル基、および酸無水物基からなる群より選択された1つ以上の基を含有する1種以上の単量体由来単位(b1)の含有量が10重量%以下である、請求項1に記載のリチウム二次電池用の分離膜。
- 前記(B)第2ポリビニリデンフルオライド系重合体が、(メタ)アクリレート単量体由来単位およびビニリデンフルオライド単量体由来単位を含む重合体である、請求項1に記載のリチウム二次電池用の分離膜。
- 前記ポリビニリデンフルオライド系ホモポリマーの重量平均分子量(Mw)は、1,000,000以上であり、前記ビニリデンフルオライド単量体由来単位とヘキサフルオロプロピレン単量体由来単位とを含むポリビニリデンフルオライド系コポリマーの重量平均分子量(Mw)は、800,000以下である、請求項1乃至4のいずれか1項に記載のリチウム二次電池用の分離膜。
- 前記(B)第2ポリビニリデンフルオライド系共重合体の重量平均分子量(Mw)が800,000以上である、請求項1乃至4のいずれか1項に記載のリチウム二次電池用の分離膜。
- 前記多孔性接着層が無機粒子を追加的に含む、請求項1乃至4のいずれか1項に記載のリチウム二次電池用の分離膜。
- 前記(A)第1ポリビニリデンフルオライド系重合体および(B)第2ポリビニリデンフルオライド系重合体の重量と、前記無機粒子の重量との比率は、8:2、または7:3、または6:4、または5:5、または4:6、または3:7、または2:8のいずれか一つの割合である、請求項7に記載のリチウム二次電池用の分離膜。
- 正極と、負極と、請求項1乃至4のいずれか1項に記載のリチウム二次電池用の分離膜と、電解液とを含むリチウム二次電池。
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