JP2021535545A - 電気化学素子用の分離膜及びそれを含む電気化学素子 - Google Patents
電気化学素子用の分離膜及びそれを含む電気化学素子 Download PDFInfo
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- 229940050176 methyl chloride Drugs 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical class OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
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- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
Description
a)高分子樹脂を溶融/押出して成膜した多孔性フィルム
b)前記a)の多孔性フィルムが二層以上積層された多層膜
c)高分子樹脂を溶融/紡糸して得たフィラメントを集積して製造された不織布ウェブ
d)前記c)の不織布ウェブが二層以上積層された多層膜
e)前記a)〜d)のうち二つ以上を含む多層構造の多孔性複合膜
本発明の一実施様態において、前記PVDF系高分子は、前記樹脂組成物100wt%に対して60wt%〜95wt%の範囲で含まれ得る。後述するように、前記耐熱コーティング層は、加湿条件で耐熱コーティング層形成用の高分子溶液が固化する間にPVDF系バインダーの相分離を誘導して気孔を形成し得る。この際、前記樹脂組成物においてPVDF系バインダー樹脂の含量が少ない場合には、相分離可能なバインダー樹脂成分が十分ではなく、気孔の大きさ及び気孔度の面で所望する水準に気孔が形成されない。
本発明において、前記ポリビニルピロリドン(polyvinylpyrrolidone,PVP)系高分子は、単量体としてN−ビニルピロリドンを含む高分子重合体を意味する。前記ポリビニルピロリドン系高分子は、N−ビニルピロリドンの単一共重合体、N−ビニルピロリドンとフリーラジカル共重合可能な追加の共単量体との共重合体またはこれらの一種以上を含み得る。
[数1]
PVP高分子の密度(g/m3)=(耐熱コーティング層中のPVP含量)×{(分離膜の単位面積当たりの重量−多孔性高分子基材の単位面積当たりの重量)/(分離膜の厚さ−多孔性高分子基材の厚さ)}
分離膜の製造
下記表1の組成によって樹脂組成物を準備した。アセトンとイソプロピルアルコール(IPA)とを混合して分散媒を準備し、ここに各実施例及び比較例のPVP及びPVDF−HFPを含む樹脂組成物を投入することで高分子溶液を製造した。前記PVDF−HFPは、分子量(Mw)が30万であり、置換率は15wt%であった。多孔性高分子基材(厚さ9μm、気孔度32vol%、分子量50万のポリエチレン)の上にディップコーティング(dip coating)方法で前記高分子溶液をコーティングし、相対湿度(RH)60%水準及び常温条件で加湿相分離を誘導した。このような方法で分離膜を製造した。
1)ロード量
多孔性高分子基材の両面にコーティングされた耐熱コーティング層に含まれた樹脂組成物の単位面積当たりの重量を示す。
通気度測定機(製造社:Asahi Seiko,製品名:EG01−55−1MR)を用いて一定の圧力(0.05MPa)で100ccの空気が分離膜を通過するのにかかる時間(sec)を測定した。サンプルの左/中/右の各1点ずつ総3点測定して平均を記録した。
各実施例及び比較例で製造された分離膜を5cm×5cmの大きさで裁断した後、150℃で30分間維持した後、収縮した程度をTD、MD方向へ各々計算した。
熱収縮率(%)=[(収縮前の長さ−収縮後の長さ)/収縮前の長さ]×100
各実施例及び比較例で製造された分離膜を100mm(長さ)×25mm(幅)で切断し、60℃、6.5MPa、1sの条件で、ホットプレスで負極にラミネートした後、UTM装備(Instron社)を用いて300mm/minの速度で180°角度で剥離し、この際の強度を測定した。50g/25mm以上確保されることが望ましい。
Claims (12)
- 多孔性高分子基材と、前記多孔性高分子基材の少なくとも一面に形成された耐熱コーティング層と、を含み、前記耐熱コーティング層は、PVDF系高分子及びポリビニルピロリドン(PVP)系高分子を含む樹脂組成物を含み、前記樹脂組成物100wt%に対し、PVP系高分子の含量が5wt%〜40wt%の割合で含まれ、前記PVP系高分子は分子量(Mw)が900,000g/mol以上であり、前記樹脂組成物は多孔性高分子基材の表面に対するローディング量が1g/cm2以上であり、通気度が900s/100cc以下である、電気化学素子用の分離膜。
- 前記耐熱コーティング層は、厚さが0.5μm〜5.0μmである、請求項1に記載の電気化学素子用の分離膜。
- 前記耐熱コーティング層は、PVDF系高分子及びポリビニルピロリドン系高分子を含む樹脂組成物を含み、耐熱コーティング層中に前記樹脂組成物が90wt%以上、望ましくは99wt%以上含まれる、請求項1に記載の電気化学素子用の分離膜。
- 前記PVDF系高分子は、フッ化ビニリデン単独重合体(PVDF)、PVDF−HFP、PVDF−CTFEまたはこれらの二種以上を含む混合物を含む、請求項1に記載の電気化学素子用の分離膜。
- 前記PVP系高分子は、N−ビニルピロリドンの単一共重合体、N−ビニルピロリドンとフリーラジカル共重合可能な追加の共単量体との共重合体またはこれら一種以上を含み、前記共重合体がN−ビニルピロリドンの含量の60wt%以上である、請求項1に記載の電気化学素子用の分離膜。
- 前記共単量体が、アクリルアミド、アクリルアミドの誘導体、アクリル酸エステル、アクリル酸エステルの誘導体またはこれらの二種以上を含む、請求項5に記載の電気化学素子用の分離膜。
- 前記PVDF系高分子がPVDF−HFPを含み、その分子量(Mw)が1万〜100万である、請求項1に記載の電気化学素子用の分離膜。
- 前記PVDF系高分子がPVDF−HFPを含み、ここで、HFPの置換率が0.1wt%〜25wt%である、請求項1に記載の電気化学素子用の分離膜。
- PVP系高分子の密度が0.1g/m3〜0.6g/m3である、請求項1に記載の電気化学素子用の分離膜。
- PVP系高分子の密度が0.2g/m3〜0.5g/m3である、請求項9に記載の電気化学素子用の分離膜。
- 請求項1に記載の分離膜の製造方法であって、前記方法がPVDF系高分子及びPVP系高分子を含む樹脂組成物と、分散媒と、を含む高分子溶液を準備し、前記高分子溶液を多孔性高分子基材の表面に塗布した後、加湿条件で乾燥し、前記分散媒が樹脂組成物に対する溶媒及び非溶媒を含み、前記高分子溶液中に樹脂組成物が20wt%未満の濃度で含まれる、電気化学素子用の分離膜の製造方法。
- 前記分散媒は、分散媒100mol%に対して非溶媒が20mol%以下に含まれる、請求項11に記載の分離膜の製造方法。
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