JP4935358B2 - 積層体及び二次電池 - Google Patents
積層体及び二次電池 Download PDFInfo
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- JP4935358B2 JP4935358B2 JP2006543219A JP2006543219A JP4935358B2 JP 4935358 B2 JP4935358 B2 JP 4935358B2 JP 2006543219 A JP2006543219 A JP 2006543219A JP 2006543219 A JP2006543219 A JP 2006543219A JP 4935358 B2 JP4935358 B2 JP 4935358B2
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- Prior art keywords
- resin layer
- layer
- group
- laminate
- fluorine
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- Y02E60/10—Energy storage using batteries
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Description
このように構成することにより、金属接着性を有するオレフィン系樹脂層と熱接着性樹脂層とを水蒸気バリアー性、耐熱性、接着性に優れるフッ素系樹脂層を介して積層するために、水分透過が極めて少なく、耐電解液性、耐クラック性、耐短絡性等に優れた積層体とすることができる。
2 基材層
3 アルミニウム箔
4 化成処理層
5 金属接着性を有するオレフィン系樹脂層
6 フッ素系樹脂層
7 熱接着性樹脂層
図1は本発明にかかる積層体の一実施例の層構成を図解的に示す図であって、積層体1は、基材層2の上に、アルミニウム箔3、化成処理層4、金属接着性を有するオレフィン系樹脂層5、フッ素系樹脂層6、熱接着性樹脂層7を順次積層したものである。
水素原子、ヒドロキシル基及びヒドロキシアルキル基のいずれかである。また、R1、R2はヒドロキシル基、アルキル基、ヒドロキシアルキル基を示し、同じ基であってもよいし、異なる基であってもよいものである。
[2層からなる基材層の作製]
9μm厚さの2軸延伸PETフィルムと15μm厚さの2軸延伸ONフィルムとを2液硬化型ポリウレタン系接着剤を介して積層して2層からなる基材層〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm〕を作製した。
予め、アミノ化フェノール重合体、三価クロム化合物、および、リン化合物を含有する化成処理液で処理して化成処理層を両面に形成したアルミニウム箔(100μm厚さ)の一方の面と12μm厚さの2軸延伸PENフィルムとを2液硬化型ポリウレタン系接着剤を介して積層して第1中間積層体〔2軸延伸PENフィルム12μm/化成処理層/アルミニウム箔100μm/化成処理層〕を作製した。
予め、アミノ化フェノール重合体、三価クロム化合物、および、リン化合物を含有する化成処理液で処理して化成処理層を両面に形成したアルミニウム箔(100μm厚さ)の一方の面と前記2層からなる基材層のON面とを2液硬化型ポリウレタン系接着剤を介して積層して第2中間積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔100μm/化成処理層〕を作製した。
予め、アミノ化フェノール重合体、三価クロム化合物、および、リン化合物を含有する化成処理液で処理して化成処理層を両面に形成したアルミニウム箔(80μm厚さ)の一方の面と前記2層からなる基材層のON面とを2液硬化型ポリウレタン系接着剤を介して積層して第3中間積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔80μm/化成処理層〕を作製した。
予め、アミノ化フェノール重合体、三価クロム化合物、および、リン化合物を含有する化成処理液で処理して化成処理層を両面に形成したアルミニウム箔(40μm厚さ)の一方の面と前記2層からなる基材層のON面とを2液硬化型ポリウレタン系接着剤を介して積層して第4中間積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔40μm化成処理層〕を作製した。
予め、アミノ化フェノール重合体、三価クロム化合物、および、リン化合物を含有する化成処理液で処理して化成処理層を両面に形成したアルミニウム箔(40μm厚さ)の一方の面と25μm厚さの2軸延伸ONフィルムとを2液硬化型ポリウレタン系接着剤を介して積層して第5中間積層体〔2軸延伸ONフィルム25μm/化成処理層/アルミニウム箔40μm/化成処理層〕を作製した。
第1中間積層体の化成処理面に不飽和カルボン酸でグラフト変性したポリプロピレン(以下、PPaと呼称する)を15μm厚さとなるようにTダイ押出機で加熱溶融押出しし、その後にPPa面にコロナ放電処理を施し、コロナ放電処理したPPa面にフッ素含有共重合体にイソシアネート系硬化剤をポリオールの水酸基(−OH基)1当量に対して1.1当量となるように添加したフッ素系樹脂溶液を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さの未延伸ポリプロピレンフィルム(以下、CPPフィルムと呼称する)をフッ素系樹脂層面に加熱圧着して本発明の積層体〔2軸延伸PENフィルム12μm/化成処理層/アルミニウム箔100μm/化成処理層/PPa15μm/フッ素系樹脂層3.0g/m2/CPPフィルム30μm〕を作製した。
第2中間積層体の化成処理面に不飽和カルボン酸でグラフト変性したポリエチレン(以下、PEaと呼称する)を12μm厚さとなるようにTダイ押出機で加熱溶融押出しし、その後にPEa面にコロナ放電処理を施し、コロナ放電処理したPEa面にフッ素含有共重合体にイソシアネート系硬化剤をポリオールの水酸基(−OH基)1当量に対して1.1当量となるように添加したフッ素系樹脂溶液を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さCPPフィルムをフッ素系樹脂層面に加熱圧着して本発明の積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔100μm/化成処理層/PEa15μm/フッ素系樹脂層3.0g/m2/CPPフィルム30μm〕を作製した。
第3中間積層体の化成処理面にPEaを12μm厚さとなるようにTダイ押出機で加熱溶融押出しし、その後にPEa面にコロナ放電処理を施し、コロナ放電処理したPEa面にフッ素含有共重合体にイソシアネート系硬化剤をポリオールの水酸基(−OH基)1当量に対して1.1当量となるように添加したフッ素系樹脂溶液を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さの未延伸ポリエチレンフィルム(以下、PEフィルムと呼称する)をフッ素系樹脂層面に加熱圧着して本発明の積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔80μm/化成処理層/PEa15μm/フッ素系樹脂層3.0g/m2/PEフィルム30μm〕を作製した。
第3中間積層体の化成処理面にPPaを12μm厚さとなるようにTダイ押出機で加熱溶融押出しし、その後にPPa面にコロナ放電処理を施し、コロナ放電処理したPPa面にフッ素含有共重合体にイソシアネート系硬化剤をポリオールの水酸基(−OH基)1当量に対して1.1当量となるように添加したフッ素系樹脂溶液を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さのPEフィルムをフッ素系樹脂層面に加熱圧着して本発明の積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔80μm/化成処理層/PPa12μm/フッ素系樹脂層3.0g/m2/PEフィルム30μm〕を作製した。
第4中間積層体の化成処理面に30μm厚さのPPaフィルムをサーマルラミネーション法で積層し、その後にPPa面にコロナ放電処理を施し、コロナ放電処理したPPa面にフッ素含有共重合体にイソシアネート系硬化剤をポリオールの水酸基(−OH基)1当量に対して1.1当量となるように添加したフッ素系樹脂溶液を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さCPPフィルムをフッ素系樹脂層面に加熱圧着して本発明の積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔40μm/化成処理層/PPaフィルム30μm/フッ素系樹脂層3.0g/m2/CPPフィルム30μm〕を作製した。
第4中間積層体の化成処理面に30μm厚さのPEaフィルムをサーマルラミネーション法で積層し、その後にPEa面にコロナ放電処理を施し、コロナ放電処理したPEa面にフッ素含有共重合体にイソシアネート系硬化剤をポリオールの水酸基(−OH基)1当量に対して1.1当量となるように添加したフッ素系樹脂溶液を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さCPPフィルムをフッ素系樹脂層面に加熱圧着して本発明の積層体〔2軸延伸PETフィルム9μm/2軸延伸ONフィルム15μm/化成処理層/アルミニウム箔40μm/化成処理層/PEaフィルム30μm/フッ素系樹脂層3.0g/m2/CPPフィルム30μm〕を作製した。
第5中間積層体の化成処理面に2液硬化型ポリウレタン系接着剤を乾燥後に3.0g/m2となるように塗布・乾燥すると共に30μm厚さのCPPフィルムを接着剤層面に加熱圧着して比較例とする積層体〔2軸延伸ONフィルム25μm/化成処理層/アルミニウム箔40μm/化成処理層/接着剤層3.0g/m2/CPPフィルム30μm〕を作製した。
第5中間積層体の化成処理面にPPaを15μm厚さとなるようにTダイ押出機で加熱溶融押出しすると共に30μm厚さのCPPフィルムをサンドイッチラミネーションして比較例とする積層体〔2軸延伸ONフィルム25μm/化成処理層/アルミニウム箔40μm/化成処理層/PPa15μm/CPPフィルム30μm〕を作製した。
第5中間積層体の化成処理面にPEaを15μm厚さとなるようにTダイ押出機で加熱溶融押出しすると共に30μm厚さのPEフィルムをサンドイッチラミネーションして比較例とする積層体〔2軸延伸ONフィルム25μm/化成処理層/アルミニウム箔40μm/化成処理層/PEa15μm/PEフィルム30μm〕を作製した。
(耐電解液性評価方法)
3gの電解液〔6フッ化リン酸リチウムを混合液〔エチレンカーボネート/ジエチルカーボネート/ジメチルカーボネート=1/1/1(容積比)に溶解し、1モル/リットルの6フッ化リン酸リチウム溶液としたもの〕を充填した内寸が30×50mmでヒートシール幅が7mmの三方シール袋を積層体で作製し、これを85℃の恒温槽に2200時間保存した後に開封して、アルミニウム箔より内側の層の剥離の有無を目視評価した。
積層体を裁断して100mm角のテストサンプルを作製し、33×55mmの矩形状の雄型とこの雄型とのクリアランスが0.5mmの雌型を用い、雄型側に熱接着性樹脂層側が位置するように雌型上に短冊片を載置すると共に短冊片を0.1MPaの押え圧(面圧)で押えて、3mm深さに成形した成形品を各10サンプル作製し、それぞれに対応する100mm角のテストサンプルを熱接着性樹脂層側が対向するように重ね合わせ、一つの端縁を7mm幅の金属−金属系の熱板からなるヒートシール機でヒートシール(シール条件:190℃、1.0MPa、3秒)して熱接着部を形成し、次に熱接着部を10N/100mm幅で一瞬180度剥離し、その後に熱接着部に直交する方向を同様にしてヒートシールして一方が開放した成形体を作製し、電解液〔6フッ化リン酸リチウムを混合液〔エチレンカーボネート/ジエチルカーボネート/ジメチルカーボネート=1/1/1(容積比)に溶解し、1モル/リットルの6フッ化リン酸リチウム溶液としたもの〕を成形体の180度剥離した熱接着部が浸るように注入し、印加電圧を1〜100Vの間で変化させて電解液と積層体のアルミニウム箔との電気抵抗を測定し、100Vの印加電圧においても10MΩ以上を良として○印で示し、10の成形体中で一つでも0.1MΩ以下となったものを不可として×印で示して評価した。なお、×印で示したものは、0.1MΩ以下となる印加電圧も併せて表記した。
積層体を裁断して60mm角のテストサンプルを作製し、積層体のシーラントフィルム面同士を対向させて積層体を配置すると共に、幅が4mm、長さが55mm、厚さが70μmのニッケル端子を積層体間に挿入すると共にニッケル端子と積層体のアルミニウム箔にテスターの端子を接続し、この状態でニッケル端子の長さ方向に直交する方向に上下共に7mm幅の金属−金属系の熱板からなるヒートシール機でヒートシール(シール条件:190℃、1.0MPa)して、ニッケル箔と積層体のアルミニウム箔とが短絡するまでの時間(単位:秒)を評価した。
積層体を裁断して120×120mmの短冊片を作製し、MD方向に二つ折りし、短辺側の一方を10mm巾に、長辺側を3mm巾にシールして他方の短辺側が開口した袋を作製すると共に、その袋を真空オーブンで乾燥後にドライルーム内にて3gの混合液〔エチレンカーボネート/ジエチルカーボネート/ジメチルカーボネート=1/1/1(容積比)〕を前記袋に注入し、開口部を10mm巾でシールした水分透過性評価サンプルを作製した。この水分透過性評価サンプルを60℃、90%RHの恒温恒湿槽に7日間保存し、サンプル内部の水分の増加量をカールフィッシャー法で測定した。なお、短辺側のヒートシール条件は190℃、2.0MPa、3.0秒であり、長辺側のヒートシール条件は190℃、1.0MPa、3.0秒で行なった。
積層体を裁断して100×80mmの短冊片を作製し、33×55mmの矩形状の雄型とこの雄型とのクリアランスが0.5mmの雌型を用い、雄型側に熱接着性樹脂層側が位置するように雌型上に短冊片を載置すると共に短冊片を0.1MPaの押え圧(面圧)で押えて、0.5mmの成形深さから0.5mm単位で成形深さを変えて各10枚のサンプルについて冷間成形し、包装材に皺やアルミニウム箔にピンホールおよびクラックが10枚のサンプルのいずれにも発生していない成形深さを限界成形深さとし、その成形深さを評価値として示した。
Claims (7)
- 少なくとも、基材層、アルミニウム箔、化成処理層、金属接着性を有するオレフィン系樹脂層及び熱接着性樹脂層が順次積層された積層体であって、
前記のオレフィン系樹脂層と前記熱接着性樹脂層との間に、架橋性基を有するフッ素含有共重合体と該架橋性基と反応する硬化剤とにより形成されたフッ素系樹脂層を有する積層体。 - 前記のオレフィン系樹脂層が酸変性ポリオレフィン系樹脂である請求項1記載の積層体。
- 前記熱接着性樹脂層が、ポリオレフィン系樹脂又は酸変性ポリオレフィン系樹脂である請求項1記載の積層体。
- 前記のフッ素含有共重合体が、少なくともフルオロオレフィン単量体と水酸基含有単量体を単量体成分として含む請求項1記載の積層体。
- 前記硬化剤が、有機ポリイソシアネート化合物である請求項1記載の積層体。
- 前記化成処理層がアミノ化フェノール重合体、三価クロム化合物、および、リン化合物を含有する化成処理液により形成されていることを特徴とする請求項1記載の積層体。
- 電池本体の正極と負極にそれぞれ接合された複数のリードを電池容器から突出させた状態で、電池容器を密封してなる二次電池であって、
上記電池容器が、少なくとも、基材層、アルミニウム箔、化成処理層、金属接着性を有するオレフィン系樹脂層及び熱接着性樹脂層が順次積層された積層体であって、前記のオレフィン系樹脂層と前記熱接着性樹脂層との間に、架橋性基を有するフッ素含有共重合体と該架橋性基と反応する硬化剤とにより形成されたフッ素系樹脂層を有する二次電池。
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US8440756B2 (en) | 2009-09-14 | 2013-05-14 | Mitsubishi Gas Chemical Company, Inc. | Flame-retardant polyamide resin composition |
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CN101087687A (zh) | 2007-12-12 |
CN101087687B (zh) | 2011-11-16 |
WO2006046615A1 (ja) | 2006-05-04 |
KR101237693B1 (ko) | 2013-02-26 |
KR20070088652A (ko) | 2007-08-29 |
JPWO2006046615A1 (ja) | 2008-05-22 |
US20060093906A1 (en) | 2006-05-04 |
US7745045B2 (en) | 2010-06-29 |
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