JP2017191777A - 多孔性耐熱層組成物、多孔性耐熱層を含む分離膜、および該分離膜を用いた電気化学電池 - Google Patents
多孔性耐熱層組成物、多孔性耐熱層を含む分離膜、および該分離膜を用いた電気化学電池 Download PDFInfo
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- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229910021473 hassium Inorganic materials 0.000 description 1
- 125000001072 heteroaryl group Chemical group 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 125000004366 heterocycloalkenyl group Chemical group 0.000 description 1
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- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-M isovalerate Chemical compound CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 1
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- 239000008274 jelly Substances 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
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- WGJJZRVGLPOKQT-UHFFFAOYSA-K lanthanum(3+);trifluoromethanesulfonate Chemical compound [La+3].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F WGJJZRVGLPOKQT-UHFFFAOYSA-K 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
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- 238000000691 measurement method Methods 0.000 description 1
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- 229940017219 methyl propionate Drugs 0.000 description 1
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- 230000000116 mitigating effect Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
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- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- SRSFOMHQIATOFV-UHFFFAOYSA-N octanoyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(=O)CCCCCCC SRSFOMHQIATOFV-UHFFFAOYSA-N 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- GHZRKQCHJFHJPX-UHFFFAOYSA-N oxacycloundecan-2-one Chemical compound O=C1CCCCCCCCCO1 GHZRKQCHJFHJPX-UHFFFAOYSA-N 0.000 description 1
- 125000003566 oxetanyl group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- 229920006260 polyaryletherketone Polymers 0.000 description 1
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- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
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- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 229920000973 polyvinylchloride carboxylated Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- RGBXDEHYFWDBKD-UHFFFAOYSA-N propan-2-yl propan-2-yloxy carbonate Chemical compound CC(C)OOC(=O)OC(C)C RGBXDEHYFWDBKD-UHFFFAOYSA-N 0.000 description 1
- YPVDWEHVCUBACK-UHFFFAOYSA-N propoxycarbonyloxy propyl carbonate Chemical compound CCCOC(=O)OOC(=O)OCCC YPVDWEHVCUBACK-UHFFFAOYSA-N 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 230000003763 resistance to breakage Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910021481 rutherfordium Inorganic materials 0.000 description 1
- DDCWGUIPLGMBPO-UHFFFAOYSA-K samarium(3+);trifluoromethanesulfonate Chemical compound [Sm+3].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F DDCWGUIPLGMBPO-UHFFFAOYSA-K 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910021477 seaborgium Inorganic materials 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- DCVWZWOEQMSMLR-UHFFFAOYSA-N silylperoxysilane Chemical compound [SiH3]OO[SiH3] DCVWZWOEQMSMLR-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- XTXFUQOLBKQKJU-UHFFFAOYSA-N tert-butylperoxy(trimethyl)silane Chemical compound CC(C)(C)OO[Si](C)(C)C XTXFUQOLBKQKJU-UHFFFAOYSA-N 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000002733 tin-carbon composite material Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- AHZJKOKFZJYCLG-UHFFFAOYSA-K trifluoromethanesulfonate;ytterbium(3+) Chemical compound [Yb+3].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F AHZJKOKFZJYCLG-UHFFFAOYSA-K 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229940075420 xanthine Drugs 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
熱収縮率(%)=(A−B)/A×100・・・(式1)
ここで、Aは、オーブンに入れる前の長さであり、Bは、オーブンにて1時間放置した後の長さである。
平均粒径(D50)500nmの第1アルミナ(AES011、住友化学社製)をアセトン(大井化金社製)に25重量%添加後、25℃で3時間ビーズミル分散をして第1アルミナ分散液を製造した。また、平均粒径(D50)200nmの第2アルミナ(AKP53、住友化学社製)をメチルエチルケトンに30重量%添加後、25℃で3時間ビーズミル分散をして第2アルミナ分散液を製造し、第1アルミナと第2アルミナとの重量比が8.5:1.5となるように製造された第1アルミナ分散液に第2アルミナ分散液を添加して、無機粒子分散液を製造した。
前記実施例1における第1アルミナと第2アルミナとの重量比が8:2となるようにしたことを除けば、実施例1と同様の方法で分離膜を製造した。
前記実施例1における第1アルミナと第2アルミナとの重量比が7:3となるようにしたことを除けば、実施例1と同様の方法で分離膜を製造した。
前記実施例1における第1アルミナと第2アルミナとの重量比が9:1となるようにしたことを除けば、実施例1と同様の方法で分離膜を製造した。
前記実施例1における第1アルミナと第2アルミナとの重量比が10:0となるように第2アルミナを用いないことを除けば、実施例1と同様の方法で分離膜を製造した。
前記実施例1における第1アルミナと第2アルミナとの重量比が6:4となるようにしたことを除けば、実施例1と同様の方法で分離膜を製造した。
前記実施例1における第1アルミナの平均粒径を700nm、第2アルミナの平均粒径を50nmとし、第1アルミナと第2アルミナとの重量比が7:3となるようにしたことを除けば、実施例1と同様の方法で分離膜を製造した。
前記実施例1における第1アルミナの平均粒径を700nm、第2アルミナの平均粒径を500nmとし、第1アルミナと第2アルミナとの重量比が7:3となるようにしたこを除けば、実施例1と同様の方法で分離膜を製造した。
実施例1〜3および比較例1〜5で製造された分離膜に対して、以下に開示された測定方法で熱収縮率、破断耐熱度、弾性率、硬度および通気度を測定し、その結果を表1に示した。
実施例1〜3および比較例1〜5で製造された各分離膜を13cm×13cmの大きさに切断し、MD方向およびTD方向にそれぞれ10cmの間隔で2点をつけ、MD方向およびTD方向が垂直に交差する中央に点をつけてサンプルを準備し、このサンプルを150℃に加熱されたオーブン(LO−FS050、LK LAB KOREA)に入れて1時間加熱した後、MD方向およびTD方向の2点の間の距離を測定した。熱収縮率は次の式1で計算した。
熱収縮率(%)=(A−B)/A×100・・・(式1)
ここで、Aは、オーブンに入れる前の長さであり、Bは、オーブンにて1時間放置した後の長さである。
実施例1〜3および比較例1〜5で製造された分離膜をMD方向およびTD方向に6cm×6cmの大きさに切り出した。中央に5cm×5cmの穴をあけたメタルフレーム上にポリイミドフイルムで分離膜を固定させた後、オーブン(LO−FS050、LK LAB KOREA)に入れて、230℃、240℃および250℃で10分間加熱した後、破断の有無を確認して、分離膜の破断が発生した場合に不良(NG)、破断が発生しなかった場合に合格(OK)と判断した。
実施例1〜3および比較例1〜5で製造された各分離膜を10cm×5cmの大きさに切断した。弾性率および硬度は、microindentation装備(FISCHERSCOPE HM2000 Microindenter)を用いて、圧子を分離膜に押込(load:10mN、load rate:1sec/mN)み連続的に測定した荷重/押込深さの結果から、測定した。
実施例1〜3および比較例1〜5で製造したセパレータそれぞれを直径1インチの円が入れるほどの大きさに、互いに異なる10個の地点で裁断した10個の試料を作製した後、通気度測定装置(旭精工社製)を用いて、前記各試料で空気100ccが通過する時間を測定した。前記時間をそれぞれ5回ずつ測定した後、平均値を計算して、これを通気度とした。
20 負極
30 分離膜
40 電極アセンブリ
50 ケース
100 リチウム二次電池
Claims (16)
- 架橋性官能基を1つ以上含む、モノマー、オリゴマー、およびポリマーからなる群より選択された一つまたはこれらの混合物と、
溶媒と、
開始剤と、
平均粒径(D50)をXとすると、300nm〜700nmの範囲内のXを有する第1無機粒子と、
0.1X〜0.4Xの範囲内の平均粒径(D50)を有する第2無機粒子と、
を含み、
前記第1無機粒子と前記第2無機粒子との重量比が7:3〜8.5:1.5である、分離膜の多孔性耐熱層組成物。 - 前記第2無機粒子の平均粒径(D50)は、50nm以上である、請求項1に記載の分離膜の多孔性耐熱層組成物。
- 前記架橋性官能基を1つ以上含む、モノマー、オリゴマー、およびポリマーが、下記化学式1で表わされるモノマー、オリゴマー、およびポリマーである、請求項1に記載の分離膜の多孔性耐熱層組成物。
- 非架橋型バインダーをさらに含む、請求項1に記載の分離膜の多孔性耐熱層組成物。
- 前記非架橋型バインダーは、PVdF系ポリマー、ポリメチルメタクリレート、ポリアクリロニトリル、ポリビニルピロリドン、ポリビニルアセテート、ポリエチレンオキシド、セルロースアセテート、セルロースアセテートブチレート、セルロースアセテートプロピオネート、シアノエチルプルラン、シアノエチルポリビニルアルコール、シアノエチルセルロース、シアノエチルスクロース、プルラン、カルボキシルメチルセルロース、およびアクリロニトリル−ブタジエン−スチレン重合体からなる群より選択された一つまたはこれらの混合物である、請求項4に記載の分離膜の多孔性耐熱層組成物。
- 前記架橋性官能基を1つ以上含むモノマー、オリゴマー、およびポリマーからなる群より選択された一つまたはこれらの混合物と、前記非架橋型バインダーとの重量比は、2:8〜5:5である、請求項4に記載の分離膜の多孔性耐熱層組成物。
- 多孔性基材と、
前記多孔性基材の一面あるいは両面に、請求項1〜6のいずれか1項に記載の多孔性耐熱層組成物から形成された多孔性耐熱層と、
を含む、分離膜。 - 前記多孔性耐熱層が、下記の化学式1で表わされるモノマー、オリゴマー、およびポリマーからなる群より選択された一つまたはこれらの混合物から形成された架橋構造のバインダーを含む、請求項7に記載の分離膜。
- 多孔性基材と、
前記多孔性基材の一面あるいは両面に形成された多孔性耐熱層と、
を含み、
前記多孔性耐熱層は、
架橋型バインダーと、
非架橋型バインダーと、
平均粒径(D50)をXとすると、300〜700nmの範囲内のXを有する第1無機粒子と、
0.1X〜0.4Xの範囲内の平均粒径(D50)を有する第2無機粒子と、を含む、
分離膜。 - 前記第2無機粒子の平均粒径(D50)は、50nm以上である、請求項9に記載の分離膜。
- 前記架橋型バインダーは、下記化学式1で表わされるモノマー、オリゴマー、およびポリマーからなる群より選択された一つまたはこれらの混合物から形成されたものである、請求項9に記載の分離膜。
- 前記非架橋型バインダーは、PVdF系ポリマー、ポリメチルメタクリレート、ポリアクリロニトリル、ポリビニルピロリドン、ポリビニルアセテート、ポリエチレンオキシド、セルロースアセテート、セルロースアセテートブチレート、セルロースアセテートプロピオネート、シアノエチルプルラン、シアノエチルポリビニルアルコール、シアノエチルセルロース、シアノエチルスクロース、プルラン、カルボキシルメチルセルロース、およびアクリロニトリル−ブタジエン−スチレン重合体からなる群より選択された一つまたはこれらの混合物である、請求項11に記載の分離膜。
- 前記第1無機粒子と前記第2無機粒子との重量比が7:3〜8.5:1.5の範囲内である、請求項9に記載の分離膜。
- 弾性率が500MPa以上700MPa以下であり、硬度が25N/mm2以上35N/mm2以下である、請求項9乃至13のいずれか一項に記載の分離膜。
- 正極、負極、分離膜、および電解質を含む電気化学電池であって、前記分離膜は、請求項1乃至14のいずれか1項に記載の分離膜である、電気化学電池。
- 前記電気化学電池は、リチウム二次電池である、請求項15に記載の電気化学電池。
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