JP2017179677A - 多孔性シート - Google Patents
多孔性シート Download PDFInfo
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- JP2017179677A JP2017179677A JP2016072964A JP2016072964A JP2017179677A JP 2017179677 A JP2017179677 A JP 2017179677A JP 2016072964 A JP2016072964 A JP 2016072964A JP 2016072964 A JP2016072964 A JP 2016072964A JP 2017179677 A JP2017179677 A JP 2017179677A
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- porous sheet
- fiber
- weight
- fibers
- cellulose
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Abstract
【解決手段】20〜500nmの平均繊維径を有するセルロース繊維、1.5〜20μmの平均繊維径を有するカットファイバー、及び、親水性高分子バインダーを含み、前記カットファイバーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を基準として1重量%以上80重量%以下であり、前記親水性高分子バインダーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を100重量部として5重量部以上30重量部以下である多孔性シート。
【選択図】なし
Description
1)電解液に対して化学的に安定であり、セパレータにより致命的な欠陥を起こさない。
2)セパレータの厚みを自由に設計することができるため、様々な要求に対応したセパレータの提供が可能である。
3)細孔径のサイズを小さく設計することができるため、リチウム遮断特性が優れ、リチウムデンドライトによる短絡が発生し難い。
4)リチウムイオン二次電池が熱暴走を起こした際に、ポリプロピレンやポリエチレンが溶融することで細孔が狭くなり初期の熱暴走を抑制することが可能である。
といった点である。
20〜500nmの平均繊維径を有するセルロース繊維、
1.5〜20μmの平均繊維径を有するカットファイバー、及び、
親水性高分子バインダー
を含み、
前記カットファイバーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を基準として1重量%以上80重量%以下であり、
前記親水性高分子バインダーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を100重量部として5重量部以上30重量部以下である
多孔性シートである。なお、ここでの「平均繊維径」とは、多孔性シートの表面の複数箇所を電子顕微鏡によって拡大観察し、各電子顕微鏡画像中から所定数の繊維を無作為に選別し、選別された当該繊維の径を測定し平均して得られた平均繊維径を意味する。選別される繊維の数は100以上であり、150以上が好ましく、200以上がより好ましく、300以上が更により好ましい。
本発明の多孔性シートは、
20〜500nmの平均繊維径を有するセルロース繊維、及び、
1.5〜20μmの平均繊維径を有するカットファイバー
親水性高分子バインダー
を含み、
前記カットファイバーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を基準として1重量%以上80重量%以下であり、
前記親水性高分子バインダーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を100重量部として5重量部以上30重量部以下である。
空孔率(%)=100×(吸液後のシート重量−吸液前のシート重量)/吸液させた溶媒の密度×5×5×厚み(cm)
本発明の多孔性シートは、20〜500nmの平均繊維径(太さ)のセルロース繊維を含むものであり、20nm未満の平均繊維径のセルロース繊維を一部含んでもよいが、セルロース繊維の全重量を基準として、その配合量は20重量%未満が好ましく、10重量%未満がより好ましく、5重量%未満が更により好ましい。なお、前記多孔性シートは500nm超の平均繊維径のセルロース繊維を一部含んでもよいが、セルロース繊維の全重量を基準として、その配合量は30重量%未満が好ましく、20重量%未満がより好ましく、10重量%未満が更により好ましい。セルロース繊維の平均繊維径としては、50〜450nmが好ましく、100〜400nmがより好ましく、150〜380nmが更により好ましく、200〜360nmが更により好ましい。
本発明の多孔性シートは、1.5〜20μmの平均繊維径(太さ)のカットファイバーを含むものであり、1.5μm未満の平均繊維径のカットファイバーを一部含んでもよいが、カットファイバーの全重量を基準として、その配合量は20重量%未満が好ましく、10重量%未満がより好ましく、5重量%未満が更により好ましい。なお、本発明の多孔性シートは20μm超の平均繊維径のカットファイバーを一部含んでもよいが、カットファイバーの全重量を基準として、その配合量は30重量%未満が好ましく、20重量%未満がより好ましく、10重量%未満が更により好ましい。カットファイバーの平均繊維径としては、1.5〜18μmが好ましく、2〜16μmがより好ましく、2.5〜14μmが更により好ましく、3.0〜12μmが更により好ましく、3.5〜10μmが特に好ましい。
本発明の多孔性シートは、少なくとも1種の親水性高分子バインダーを含む。本発明で使用される親水性高分子バインダーは、繊維間を繋ぐための接着剤として使用されるものであるが、接着剤としての機能以外に、繊維の分散性を向上させる機能を発揮することができる。均一な細孔分布を得るためには、多孔性シートの製造に使用されるスラリー中に繊維が均一に分散する必要があるが、バインダーは繊維の表面に定着することで保護コロイドに似た役割を果たすため分散性が向上する。
本発明の多孔性シートと多孔性基材の積層体は、多孔性基材、及び、上記多孔性シートを備える。
前記多孔性基材の形状は特に限定されるものではないがシート状が好ましい。したがって、前記多孔性基材としては上記の多孔性シートとは異なる多孔性シートでもよく、上記の多孔性シートと同一の多孔性シートでもよい。上記の多孔性シートとは異なる多孔性シートであることが好ましい。
本発明の多孔性シートの少なくとも一方の表面には無機フィラーからなる層(無機フィラー層)を更に備えることができる。無機フィラー層を設けることで、本発明の多孔性シートを例えば電池用セパレータとして使用する場合に、電極と多孔性シートとが直接接触することを防ぐことができる。電池の充電圧が高くなると、電極表面の酸化/還元力が高くなるため、直接接触している有機物(例えば多孔性シート)をおかす可能性があるが、多孔性シートの表面に無機フィラー層を設けることによって、多孔性シートの劣化を抑制することができる。
本発明の多孔性シートは、例えば、20〜500nmの平均繊維径を有するセルロース繊維、1.5〜20μmの平均繊維径を有するカットファイバー、及び、親水性高分子バインダーを含み、前記カットファイバーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を基準として1〜80重量%であり、前記親水性高分子バインダーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を100重量部として5〜30重量部であるスラリーを基材上に塗布し、乾燥することで製造することができる。スラリー中の繊維の濃度は限定されるものではないが、例えば、1〜40重量%とすることができ、5〜30重量%が好ましく、10〜20重量%が更により好ましい。
(1)既述のとおり多孔性シートを調製する。
(2)前記多孔性シートを多孔性基材上に積層する。
(1)20〜500nmの平均繊維径を有するセルロース繊維、1.5〜20μmの平均繊維径を有するカットファイバー、親水性高分子バインダーを含み、前記カットファイバーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を基準として1〜80重量%であり、前記親水性高分子バインダーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を100重量部として5〜30重量部であるスラリーを多孔性基材上に塗布する。スラリー中の繊維の濃度は限定されるものではないが、例えば、1〜40重量%とすることができ、5〜30重量%が好ましく、10〜20重量%が更により好ましい。
(2)前記スラリーを乾燥させて前記多孔性基材上に多孔性シートを形成する。
本発明の多孔性シート又は積層体は、電気化学素子用セパレータの一構成要素として又はそのまま電気化学素子用セパレータとして使用することができる。
電子顕微鏡(日立製作所製)で倍率5000倍の画像を5箇所撮影し、それぞれの視野から任意で20本の繊維を選択して繊維径を測定することで、(数)平均繊維径を測定した。
(2)比引裂強度の測定
多孔性シートを50mm×25mmの短冊にカットした。図1に示すように、短冊の長辺の中央より、片方の辺は上下5mmの位置に、もう片方の辺は上下10mmの位置に印をつけ、上と下それぞれの点を線で結び、短冊に2つの斜線を入れた。図1に示すように、短冊の5mmの線をつけた側の長辺の中央に長さ1mmの切込みを入れ、試験片とした。これを、チャック間距離10mmに設定したテンシロン万能引張り試験機(RTG−1210、エー・アンド・デイ製)に、上述の斜線がテンシロンの2つのチャックの下辺に沿うように、上下10mmの位置に印をつけた側の長辺がたるむようにセットした。チャックの移動速度は5mm/分として、チャックの移動距離が11mmとなるまで逆方向に移動させ、試験片の引っ張りを行い、引裂強度の数値を測定した。さらに、その値を坪量で除することで比引裂強度を算出した。比引裂強度は、15.0mN・m2/g以上を優(◎)とし、10.0mN・m2/g超を合格(○)とし、10.0mN・m2/g以下を不合格(×)として評価した。
(3)比引張強度の測定
多孔性シートを、MD方向を長辺として15mm×150mmの短冊状にカットし、試験片とした。これを、チャック間距離10mmに設定したテンシロン万能引張り試験機(RTG−1210、エー・アンド・デイ製)に、セットし、チャックの移動速度を5mm/分として、定速で引張を行い、シートが破断した際の強度を測定して引張強度とした。さらに、その値を坪量で除することで比引張強度を算出した。比引張強度は、3.0N/15mm超を優(◎)とし、2.0N/15mm以上を合格(○)とし、2.0N/15mm未満を不合格(×)として評価した。
(4)透気抵抗度の測定
JIS P8117に従い、ガーレー式透気度計(東洋精機(株)製)にて透気抵抗度を測定し、その値を厚さ10μmあたりに換算した。
NBKPをイオン交換水中に3重量%濃度になるように分散させ、ダブルディスクリファイナーを用いて数平均繊維長1.0mm以下となるような条件までサイクリングにて叩解した。数平均繊維長が1.0mm以下となったセルロース繊維分散液を高圧ホモジナイザー(LAB−1000)で800barの条件で10回処理することにより微細化セルロース繊維原料を得た。この原料を脱水装置を使って処理することにより約10重量%まで濃縮した。セルロース繊維の原料を等量のトリエチレングリコールブチルメチルエーテルと混合し、120℃のオーブンで乾燥して溶媒を除去したうえで電子顕微鏡を用いて平均繊維径を測定したところ、280nmであった。
カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の30重量%となるように、スラリー1とスラリー2の混合重量比(繊維ベース)を70:30とした以外は実施例1と同様の方法で、塗料を調製し、PETフィルム上にWET膜厚が0.30mmとなるようアプリケーターを用いて塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより坪量5.2g/m2、膜厚17μmのセルロース系微多孔膜の形態の多孔性シートを得た。
カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の70重量%となるように、スラリー1とスラリー2の混合重量比(繊維ベース)を30:70とした以外は実施例1と同様の方法で、塗料を調製し、PETフィルム上にWET膜厚が0.30mmとなるようアプリケーターを用いて塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより坪量5.0/m2、膜厚18μmの不織布の形態の多孔性シートを得た。
カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の5重量%となるように、スラリー1とスラリー2の混合重量比(繊維ベース)を95:5とした以外は実施例1と同様の方法で、塗料を調製し、PETフィルム上にWET膜厚が0.30mmとなるようアプリケーターを用いて塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより坪量5.0g/m2、膜厚17μmのセルロース系微多孔膜の形態の不織布を得た。
カットファイバーとして平均繊維径8μm、繊維長3mmのポリエチレンテレフタレート繊維(TA04N、帝人ファイバー製)を使用して、実施例1と同様の方法にてポリエステル繊維の分散液を調製し、スラリー3とした。カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の30重量%となるように、スラリー1とスラリー3の混合重量比を70:30とし、PETフィルム上にWET膜厚が0.40mmとなるようアプリケーターを用いて塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより坪量5.8g/m2、膜厚21.1μmのセルロース系微多孔膜の形態の多孔性シートを得た。
カットファイバーとして平均繊維径17μm、繊維長5mmのポリエチレンテレフタレート繊維(TA04N、帝人ファイバー製)を使用して、実施例1と同様の方法にてポリエステル繊維の分散液を調製し、スラリー4とした。カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の10重量%となるように、スラリー1とスラリー4の混合重量比(繊維ベース)を90:10とし、PETフィルム上にWET膜厚が0.40mmとなるようアプリケーターを用いて塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより坪量5.5g/m2、膜厚25.5μmのセルロース系微多孔膜の形態の多孔性シートを得た。
カットファイバーとして平均繊維径7.0μm、繊維長3mmのビニロン繊維(VPB041、株式会社クラレ製)を使用して、実施例1と同様の方法にてカットファイバーの分散液を調製し、スラリー5とした。カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の10重量%となるように、スラリー1とスラリー5の混合重量比(繊維ベース)を90:10とし、PETフィルム上にWET膜厚が0.40mmとなるようアプリケーターを用いて塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより坪量6.1g/m2、膜厚23μmのセルロース系微多孔膜の形態の多孔性シートを得た。
セルロース繊維の原料を100重量部とし、これに対してグリコールエーテル系開孔剤(商品名:ハイソルブDB 東邦化学製)を350重量部、親水性高分子バインダーとして1重量%濃度でイオン交換水に溶解したカルボキシメチルセルロース(商品名:サンローズMAC−500LC 日本製紙ケミカル製)を25重量部添加し、最終的に固形分濃度が2重量%となるように水を加えた塗料をホモミキサー(株式会社アズワン製)で均一に混ざるまで分散を行い、スラリー6とした。また、カットファイバーとして平均繊維径3.5μm、繊維長3mmのポリエチレンテレフタレート繊維(TA04PN、帝人ファイバー製)を100重量部、これに対しに親水性高分子バインダーとして1重量%濃度でイオン交換水に溶解したカルボキシメチルセルロース(商品名:サンローズMAC−500LC 日本製紙ケミカル製)を25重量部添加し、最終的に固形分濃度が2重量%となるように水を加え、ホモミキサーで均一に混ざるまで分散を行い、スラリー7とした。カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の50重量%となるように、スラリー6とスラリー7を50:50の重量比率(繊維ベース)で混合し、スターラーにて300rpmで均一になるまで撹拌することで塗料を調合した後、実施例1と同様の方法で塗布、乾燥を行い、坪量4.9g/m2、膜厚16μmの多孔性シートを得た。
無機フィラーとしてアルミナの粉体(商品名:AKP−3000 住友化学製)を100重量部、バインダー樹脂としてポリイミド樹脂(商品名:HPC−1000−28 日立化成工業製)を10重量部、およびイオン交換水に溶解したカルボキシメチルセルロース(商品名:サンローズMAC−500LC 日本製紙ケミカル製)を5重量部の割合で混合し、固形分濃度が2%となるように水に分散を行い、スラリー8とした。スラリー8をPETフィルム上に乾燥後の厚さが4μmとなるようにワイヤーバーで塗布し、120℃で乾燥して無機フィラー層を設けた後、無機フィラー層の上にWET膜厚が0.30mmとなるようアプリケーターを用いて実施例1と同一の塗料を塗布し、120℃の熱風及び赤外線ヒーターを用いて12分間乾燥した。得られた塗工膜をトルエン中でPETフィルムから剥離してトルエンを揮発させることにより、坪量5.6g/m2、膜厚19μmの多孔性シートを得た。
カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の0%となるように、スラリー1とスラリー2の混合重量比(繊維ベース)を100:0とした以外は、実施例1と同様にしてセルロース微多孔膜の形態の多孔性シートを得た。
カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の90%となるように、スラリー1とスラリー2の混合重量比(繊維ベース)を10:90とした以外は、実施例1と同様にして不織布の形態の多孔性シートを得た。
セルロース繊維の原料を100重量部とし、これに対してグリコールエーテル系開孔剤(商品名:ハイソルブDB 東邦化学製)を250重量部添加し、最終的に固形分濃度が2重量%となるように水を加えた塗料をホモミキサー(株式会社アズワン製)で均一に混ざるまで分散を行い、スラリー9とした。また、カットファイバーとして平均繊維径8.0μm、繊維長3mmのポリエチレンテレフタレート繊維(TA04N、帝人ファイバー製)を100重量部添加し、最終的に固形分濃度が2重量%となるように水を加え、ホモミキサーで均一に混ざるまで分散を行い、スラリー10とした。カットファイバーの配合率がセルロース繊維及びカットファイバーの合計量の50重量%となるように、スラリー9とスラリー10を50:50の重量比率(繊維ベース)で混合し、スターラーにて300rpmで均一になるまで撹拌することで塗料を調合した。その後、実施例1と同様の方法で塗布、乾燥を行い、坪量4.9g/m2、膜厚23μmの親水性高分子バインダーを添加していない多孔性シートを得た。
Claims (19)
- 20〜500nmの平均繊維径を有するセルロース繊維、
1.5〜20μmの平均繊維径を有するカットファイバー、及び、
親水性高分子バインダー
を含み、
前記カットファイバーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を基準として1重量%以上80重量%以下であり、
前記親水性高分子バインダーの含有量が前記セルロース繊維及び前記カットファイバーの合計重量を100重量部として5重量部以上30重量部以下である
多孔性シート。 - 比引裂強度が15.0mN・m2/g以上である、請求項1記載の多孔性シート。
- 比引張強度が3.0N/15mm超である、請求項1又は2記載の多孔性シート。
- 厚さ10μmあたりのガーレー透気抵抗度が10秒以上200秒以下である請求項1〜3のいずれかに記載の多孔性シート。
- 前記セルロース繊維に400nm以下の太さの繊維がセルロース繊維の全重量を基準として50重量%以上含まれている、請求項1〜4のいずれかに記載の多孔性シート。
- 前記セルロース繊維に1μm以上の太さの繊維がセルロース繊維の全重量を基準として5〜40重量%含まれている、請求項1〜5のいずれかに記載の多孔性シート。
- 前記カットファイバーの平均繊維長が10mm以下である、請求項1〜6のいずれかに記載の多孔性シート。
- 前記カットファイバーが、ポリエステル繊維、アラミド繊維、PPS樹脂繊維、再生セルロース繊維、ビニロン繊維、及び、これらの混合物からなる群から選択される、請求項1〜7のいずれかに記載の多孔性シート。
- 前記ポリエステル繊維が、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンナフタレート、及び、これらの組合せからなる群から選択されるポリエステルからなる、請求項8記載の多孔性シート。
- 空孔率が30〜70%である、請求項1〜9のいずれかに記載の多孔性シート。
- 3〜50μmの厚みを有する、請求項1〜10のいずれかに記載の多孔性シート。
- 少なくとも一方の表面に、無機フィラーからなる層を備える、請求項1〜11のいずれかに記載の多孔性シート。
- 多孔性基材、並びに、
請求項1〜12のいずれかに記載の多孔性シート
を備えた積層体。 - 前記多孔性基材が織布又は不織布からなる、請求項13記載の積層体。
- 前記多孔性基材がセルロース繊維からなる、請求項13又は14記載の積層体。
- 1mol/LiPF6/プロピレンカーボネート溶液を含浸させた状態において20kHzの交流を使用して決定した体積抵抗率が1500Ω・cm以下である、請求項1〜12のいずれかに記載の多孔性シート又は請求項13〜15のいずれかに記載の積層体。
- 請求項1〜12のいずれかに記載の多孔性シート又は請求項13〜16のいずれかに記載の積層体を備える電気化学素子用セパレータ。
- 請求項17記載の電気化学素子用セパレータを備える電気化学素子。
- 電池又はキャパシタである請求項18記載の電気化学素子。
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TWI644798B (zh) | 2018-12-21 |
SE1851139A1 (en) | 2018-09-25 |
US20190048528A1 (en) | 2019-02-14 |
SE545740C2 (en) | 2023-12-27 |
US11236468B2 (en) | 2022-02-01 |
WO2017169848A1 (ja) | 2017-10-05 |
KR20180131541A (ko) | 2018-12-10 |
KR20220151235A (ko) | 2022-11-14 |
TW201738077A (zh) | 2017-11-01 |
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