JP6698174B2 - 電気化学素子用分離膜及び該分離膜を含む電気化学素子 - Google Patents
電気化学素子用分離膜及び該分離膜を含む電気化学素子 Download PDFInfo
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- JP6698174B2 JP6698174B2 JP2018554303A JP2018554303A JP6698174B2 JP 6698174 B2 JP6698174 B2 JP 6698174B2 JP 2018554303 A JP2018554303 A JP 2018554303A JP 2018554303 A JP2018554303 A JP 2018554303A JP 6698174 B2 JP6698174 B2 JP 6698174B2
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Description
実施例1
まず、ポリエチレン多孔性高分子基材を用意した(ポリエチレン、厚さ7μm、空隙率32%)。次に、第1及び第2スラリーを用意した。前記第1スラリーは、溶媒(蒸留水:エタノールを95:5重量比で混合)にアルミナ(Al2O3、D50:0.5μm)粒子、ポリアクリレート及び増粘剤であるCMC(カルボキシメチルセルロース )を98:1:1の比率で混合したものである。前記アルミナ粒子は縦横比が1〜1.5のものを使用した。また、第2スラリーは、前記溶媒にMg(OH)2(D50:1.1μm、)、ポリアクリレート及び増粘剤であるCMCを98:1:1の比率で混合したものである。前記Mg(OH)2は縦横比が約3.1〜5のものを使用した。それぞれのスラリーで固形分の含量は5%にした。前記第1及び第2スラリーには、無機物粒子の凝集を防止するため、無機物粒子と同量のビーズを投入し、前記ビーズ及び溶媒の接触角を減少させるための湿潤剤(陰イオン性化合物、硫酸ナトリウム<1%)を添加して、ペイントシェーカー装置を用いて50分ずつ2回混合した。
まず、ポリエチレン多孔性高分子基材を用意した(ポリエチレン、厚さ7μm、気孔度32%)。次に、第1及び第2スラリーを用意した。前記第1スラリーは、溶媒(蒸留水:エタノールを95:5重量比で混合)にアルミナ(Al2O3、D50:0.5μm)粒子、ポリアクリレート及び増粘剤であるCMCを98:1:1の比率で混合したものである。前記アルミナ粒子は縦横比が1〜1.5のものを使用した。また、第2スラリーは、前記溶媒にMg(OH)2(D50:1.1μm)、ポリアクリレート及び増粘剤であるCMCを98:1:1の比率で混合したものである。それぞれのスラリーで固形分の含量は5%にした。一方、前記Mg(OH)2は縦横比が約3.1〜5のものを使用した。
ポリエチレン多孔性高分子基材を用意した(ポリエチレン、厚さ7μm、気孔度32%)。次に、多孔性コーティング層用スラリーを用意した。前記スラリーは、溶媒(アセトン)にアルミナ(Al2O3、D50:0.5μm)粒子、PVDF−HFP及びシアノ系のバインダー(シアノエチル化ポリビニルアルコール)を9:1:2の比率で混合した。前記アルミナ粒子は縦横比が1〜1.5のものを使用した。前記スラリーは固形分の含量が18%であった。前記スラリーは、無機物粒子の凝集を防止するため、無機物粒子と同量のビーズを投入し、ペイントシェーカー装置を用いて50分ずつ2回混合した。前記スラリーに前記高分子基材を浸して、ディップコティング法で多孔性コーティング層が形成された分離膜を収得した。
1)穿孔強度実験
穿孔強度は、直径1mm(0.5mmR)の針を用いて速度120mm/minで各実施例及び比較例の分離膜を刺したときの最大荷重値を測定した。実施例、比較例1及び比較例2の分離膜に対し、それぞれ3ヶ所に対して穿孔を行い、その平均値を示した。
実施例、比較例1及び比較例2で収得した分離膜からそれぞれ試片(10cm×10cm)を3つずつを用意した。これを150℃のオーブンに30分間放置した。その後、オーブンから試片を取り出して寸法を確認し、最初分離膜の寸法と対比して各分離膜の収縮率を確認した。その結果を下記表2に示した。
Claims (12)
- 電気化学素子用分離膜であって、
高分子樹脂を含む多孔性高分子基材;及び
前記多孔性高分子基材の両面のうち少なくとも一面に形成された多孔性コーティング層;を備えてなり、
前記多孔性コーティング層は、その厚さ方向にて、
多孔性高分子基材に近い下部から上部に至るまでa)無機物粒子の含量が段階的に増加し、
多孔性高分子基材に近い下部から上部に至るまでb)無機物粒子の含量が段階的に減少し、
前記a)無機物粒子は板状無機物粒子であり、前記b)無機物粒子は球状無機物粒子である、電気化学素子用分離膜。 - 前記多孔性コーティング層は、その厚さ方向にて、
多孔性高分子基材に近い下部から厚さ10%までの部分は無機物粒子のうちb)の含量が高く、
多孔性コーティング層の表面から厚さ10%までの部分は無機物粒子のうちa)の含量が高いものである、請求項1に記載の電気化学素子用分離膜。 - 前記多孔性コーティング層は、その厚さ方向にて、
多孔性高分子基材に近い下部から厚さ10%までの部分は、無機物粒子a)とb)との和100重量%に対してb)無機物粒子の含量が50重量%以上である、請求項1又は2に記載の電気化学素子用分離膜。 - 前記多孔性コーティング層は、その厚さ方向にて、
電極と対面する多孔性コーティング層の表面から厚さ10%までの部分は、無機物粒子a)とb)との和100重量%に対してa)無機物粒子の含量が50重量%以上である、請求項1又は2に記載の電気化学素子用分離膜。 - 前記a)板状無機物粒子は縦横比が3超過100以下である、請求項1に記載の電気化学素子用分離膜。
- 前記a)板状無機物粒子はベーマイトである、請求項5に記載の電気化学素子用分離膜。
- 前記b)球状無機物粒子は縦横比が1〜3である、請求項1に記載の電気化学素子用分離膜。
- 前記多孔性コーティング層は、a)板状無機物粒子とb)球状無機物粒子とバインダー樹脂との混合物を備えてなり、前記多孔性コーティング層のうちバインダー樹脂の含量が3〜10重量%である、請求項1に記載の電気化学素子用分離膜。
- 前記分離膜は穿孔強度が0.26kgf以上である、請求項1に記載の電気化学素子用分離膜。
- 電気化学素子であって、
正極、負極、及び前記正極と前記負極との間に介在された分離膜を備えてなり、
前記負極はリチウム金属であり、
前記分離膜は請求項1〜9の何れか一項に記載の分離膜である、電気化学素子。 - 電気化学素子用分離膜であって、
高分子樹脂を含む多孔性高分子基材;及び
前記多孔性高分子基材の両面のうち少なくとも一面に形成された多孔性コーティング層;を備えてなり、
前記多孔性コーティング層はa)板状無機物粒子及びb)球状無機物粒子を備えてなり、
前記多孔性コーティング層は、その厚さ方向にて、
多孔性高分子基材に近い下部から厚さ10%までの部分は無機物粒子a)より無機物粒子b)の含量が多く、
電極と対面する多孔性コーティング層の表面から厚さ10%までの部分は無機物粒子a)とb)との和100重量%に対してa)無機物粒子の含量が50重量%以上であり、
多孔性高分子基材に近い下部から上部に至るまでa)無機物粒子の含量が段階的に増加し、
多孔性高分子基材に近い下部から上部に至るまでb)無機物粒子の含量が段階的に減少する、電気化学素子用分離膜。 - 電気化学素子用分離膜であって、
熱可塑性樹脂を含む多孔性高分子基材;及び
前記多孔性高分子基材の両面のうち少なくとも一面に形成された多孔性コーティング層;を備えてなり、
前記多孔性コーティング層は無機物粒子及びバインダー樹脂を備えてなり、
前記無機物粒子がバインダー樹脂を媒介にして点結着及び/または面結着して集積されたものであり、
前記多孔性コーティング層はa)縦横比が3超過20以下の板状無機物粒子及びb)縦横比が1〜3の球状無機物粒子を備えてなり、
前記多孔性コーティング層は、その厚さ方向にて、
多孔性高分子基材に近い下部から厚さ10%までの部分は無機物粒子a)より無機物粒子b)の含量が多く、
電極と対面する多孔性コーティング層の表面から厚さ10%までの部分は無機物粒子a)とb)との和100重量%に対してa)無機物粒子の含量が50重量%以上であり、
前記縦横比は[長軸方向の長さ/長軸方向と直交する方向の幅]で定義され、
多孔性高分子基材に近い下部から上部に至るまでa)無機物粒子の含量が段階的に増加し、
多孔性高分子基材に近い下部から上部に至るまでb)無機物粒子の含量が段階的に減少する、電気化学素子用分離膜。
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