JP2023518499A - 電気化学素子用の分離膜及びその製造方法 - Google Patents
電気化学素子用の分離膜及びその製造方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 description 1
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical compound C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- PVADDRMAFCOOPC-UHFFFAOYSA-N germanium monoxide Inorganic materials [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
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- 229910052745 lead Inorganic materials 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910000664 lithium aluminum titanium phosphates (LATP) Inorganic materials 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910000659 lithium lanthanum titanates (LLT) Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- 229910021450 lithium metal oxide Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001485 poly(butyl acrylate) polymer Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
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- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
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- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
Description
前記多孔性コーティング層は、無機物粒子とバインダー樹脂を、重量比を基準にして約50:50~99:1の割合で含み、
前記バインダー樹脂は、第1バインダー樹脂及び第2バインダー樹脂を含み、
前記第1バインダー樹脂は、ガラス転移温度(Tg)が30~60℃であり、極性基を有するエチレン系高分子樹脂であり、
第2バインダー樹脂は、ガラス転移温度(Tg)が80~120℃であるアクリル系バインダー樹脂である。
前記バインダー樹脂は、第1、第2及び第3バインダー樹脂を含み、
前記第1バインダー樹脂は、ガラス転移温度(Tg)が30~60℃であり、ポリビニルアセテート(PVAc)を含み、
前記第2バインダー樹脂は、ガラス転移温度(Tg)が80~120℃であり、ポリメチルメタクリレート(PMMA)を含み、
前記第3バインダー樹脂は、ポリアクリロニトリル(PAN)を含む。
(1)分離膜の製造
実施例1
Al2O3(D50:500nm)、PVAc(Mw:15万、Tg:40℃)、PMMA(Mw:13万、Tg:116℃)及び分散剤(タンニン酸)をアセトンに投入して第1スラリーを準備した。一方、PAN(Mw:15万、Tg:85℃、Tm:320℃)をDMFに溶解して高分子溶液を準備した。次に、前記第1スラリーと前記高分子溶液を混合して多孔性コーティング層形成用のスラリー(第2スラリー)を準備した。前記第2スラリー濃度は18wt%であり、前記第2スラリー中のAl2O3、PVAc、PMMA、PAN及び分散剤(タンニン酸)の含量は、80:16:2:1:1の割合(wt%)にした。前記スラリー分離膜(ポリエチレン、気孔度45%、厚さ16μm、通気度、100sec/100cc)の上に、分離膜の面積に対して13.5g/m2のロード量で塗布した後、乾燥した。前記乾燥は、温度23℃、相対湿度45%の加湿条件下で行われた。その後、これを60mm(長さ)×25mm(幅)で切断して分離膜を得た。なお、得られた分離膜の厚さは25μmであった。
PANは使用せず、Al2O3、PVAc、PMMA及び分散剤(タンニン酸)をwt%で80:17:2:1の割合でアセトンに投入して多孔性コーティング層形成用のスラリーを得たことを除いては、実施例1と同様の方法で分離膜を得た。なお、得られた分離膜の表面のSEMイメージを図4aに示した。
PANは使用せず、Al2O3、PVAc、PMMA及び分散剤(タンニン酸)をwt%で80:15:4:1の割合でアセトンに投入して多孔性コーティング層形成用のスラリーを得たことを除いては、実施例1と同様の方法で分離膜を得た。なお、得られた分離膜の表面のSEMイメージを図4bに示した。
PANは使用せず、Al2O3、PVAc、PMMA及び分散剤(タンニン酸)をwt%で80:9.5:9.5:1の割合でアセトンに投入して多孔性コーティング層形成用のスラリーを得たことを除いては、実施例1と同様の方法で分離膜を得た。なお、得られた分離膜の表面のSEMイメージを図4cに示した。
Al2O3、PVdF-HFP(Mw:40万、Tm:145℃)、PVDF-CTFE(Mw:40万、Tm:160℃)及び分散剤(タンニン酸)をwt%を基準にして80:10:9:1の割合でアセトンに投入して多孔性コーティング層形成用のスラリーを得た。前記スラリー分離膜(ポリエチレン、気孔度45%、厚さ16μm)の上に、分離膜の面積に対して13.5g/m2のロード量で塗布した後、乾燥した。前記乾燥は、温度23℃、相対湿度45%の加湿条件下で行われた。次に、これを60mm(長さ)×25mm(幅)で切断して分離膜を得た。得られた分離膜の厚さは25μmであった。
Al2O3、PVAc及び分散剤を80:19:1の割合(wt%)でアセトンに投入して多孔性コーティング層形成用のスラリーを得た。前記スラリー分離膜(ポリエチレン、気孔度45%、厚さ16μm)の上に、分離膜の面積に対して13.5g/m2のロード量で塗布した後、乾燥した。前記乾燥は、温度23℃、相対湿度45%の加湿条件下で行われた。その後、それを60mm(長さ)×25mm(幅)で切断して分離膜を得た。
Al2O3、PMMA及び分散剤を80:19:1の割合(wt%)でアセトンに投入して多孔性コーティング層形成用のスラリーを得た。前記スラリー分離膜(ポリエチレン、気孔度45%、厚さ16μm)の上に、分離膜の面積に対して13.5g/m2のローディング量で塗布した後、乾燥した。前記乾燥は、温度23℃、相対湿度45%の加湿条件下で行われた。次に、これを60mm(長さ)×25mm(幅)で切断して分離膜を得た。
Al2O3、PVAc、PMMA及び分散剤を80:6:13:1の割合(wt%)でアセトンに投入して多孔性コーティング層形成用のスラリーを得た。前記スラリー分離膜(ポリエチレン、気孔度45%、厚さ16μm)の上に、分離膜面積に対して3.5g/m2のロード量で塗布した後、乾燥した。前記乾燥は、温度23℃、相対湿度45%の加湿条件下で行われた。次に、それを60mm(長さ)×25mm(幅)で切断して分離膜を得た。また、得られた分離膜の表面のSEMイメージを図4dに示した。
Al2O3(D50:500nm)、PVAc(Mw:80万、Tg:40℃)、PMMA(Mw:13万、Tg:116℃)及び分散剤(タンニン酸)をアセトンに投入して第1スラリー準備した。一方、PAN(Mw:15万、Tg:85℃、Tm:320℃)をDMFに溶解して高分子溶液を準備した。次に、前記第1スラリーと前記高分子溶液を混合して多孔性コーティング層形成用のスラリー(第2スラリー)を準備した。前記第2スラリーの濃度は18wt%であり、前記第2スラリー中のAl2O3、PVAc、PMMA、PAN及び分散剤(タンニン酸)の含量は、80:16:2:1:1の割合(wt%)にした。前記スラリー分離膜(ポリエチレン、気孔度45%、厚さ16μm、通気度100秒/100cc)の上に、分離膜の面積に対して13.5g/m2のロード量で塗布した後、乾燥した。前記乾燥は、温度23℃、相対湿度45%の加湿条件下で行われた。次に、これを60mm(長さ)×25mm(幅)で切断して分離膜を得た。得られた分離膜の厚さは25μmであった。
天然黒鉛、SBR及びCMC(重量比で90:9:1)を水に入れて負極スラリーを得た。前記負極スラリーを銅薄膜(厚さ10μm)の上に125mg/cm2のロード量で塗布した後、乾燥した。次に、それを90μmの厚さになるように圧延して50mm(長さ)×25mm(幅)で切断して負極を得た。
前記各実施例または比較例から得た分離膜を60mm(長さ)×25mm(幅)で切断して準備した負極と分離膜を、プレスを用いて60℃、6.5MPaの条件でラミネートして試片を製作した。準備した試片を両面テープを用いてガラス板に付着して固定し、この際、負極がガラス板に対面するように配置した。試片の分離膜部分を25℃で300mm/分の速度で180゜の角度に剥離し、この際の強度を測定した。前記分離膜と負極との接着力については、下記の表1及び図1にその結果を整理して示した。一方、比較例2で同様の製造方法によって得られた分離膜試片5個を準備し、25℃で300mm/分の速度で180゜の角度に剥離し、距離による剥離強度を測定した。その結果を下記の表2及び図2に示した。
各実施例及び比較例から得られた分離膜を130℃の温度条件下で0.5時間維持した後、分離膜の収縮率を測定した。収縮率は、分離膜に任意の二つの点を標示し、これら間の距離(標点距離)の増減率を下記の式1によって計算した。図2は、実施例1及び2の分離膜の収縮率の測定前と後の様子を示す写真である。これによると、実施例1及び2の分離膜は、収縮率が1%以内であって、収縮率特性が非常に高いことが確認された。
Claims (11)
- 多孔性分離膜基材及び前記基材の表面に形成された多孔性コーティング層を含む電気化学素子用の分離膜であって、
前記多孔性コーティング層が、無機物粒子とバインダー樹脂を、重量比を基準にして50:50~99:1の割合で含み、
前記バインダー樹脂は、第1バインダー樹脂及び第2バインダー樹脂を含み、
前記第1バインダー樹脂は、ガラス転移温度(Tg)が30~60℃であり、極性基を有するエチレン系高分子樹脂であり、
第2バインダー樹脂は、ガラス転移温度(Tg)が80~120℃であるアクリル系バインダー樹脂である、電気化学素子用の分離膜。 - 前記バインダー樹脂は、第3バインダー樹脂をさらに含み、前記第3バインダー樹脂は、分子量(Mw)が50万以下であり、主鎖にシアノ基が結合したビニル系高分子である、請求項1に記載の電気化学素子用の分離膜。
- 前記第1バインダー樹脂は、前記バインダー樹脂100wt%に対して50~90wt%の含量で含まれ、前記第2バインダー樹脂は、前記バインダー樹脂100wt%に対して10~50wt%の含量で含まれる、請求項1または2に記載の電気化学素子用の分離膜。
- 前記第3バインダー樹脂は、前記バインダー樹脂100wt%に対して6wt%以下の含量で含まれる、請求項2に記載の電気化学素子用の分離膜。
- 前記第3バインダー樹脂が、ポリアクリロニトリル(PAN)を含む、請求項2に記載の電気化学素子用の分離膜。
- 多孔性分離膜基材及び前記基材の表面に形成された多孔性コーティング層を含む電気化学素子用の分離膜であって、
前記多孔性コーティング層は、無機物粒子とバインダー樹脂を重量比を基準にして50:50~99:1の割合で含み、
前記バインダー樹脂は、第1、第2及び第3バインダー樹脂を含み、
前記第1バインダー樹脂は、ガラス転移温度(Tg)が30~60℃であり、ポリビニルアセテート(PVAc)を含み、
前記第2バインダー樹脂は、ガラス転移温度(Tg)が80~120℃であり、ポリメチルメタクリレート(PMMA)を含み、
前記第3バインダー樹脂は、ポリビニルアセテート(PVAc)を含む、電気化学素子用の分離膜。 - 正極、負極及び前記正極と負極との間に介在された分離膜を含み、前記分離膜は、請求項1から8のいずれか一項に記載のものである、電気化学素子。
- 請求項10に記載の電気化学素子を含む、リチウムイオン二次電池。
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