JP5650738B2 - 電池用セパレータおよび電池 - Google Patents
電池用セパレータおよび電池 Download PDFInfo
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- JP5650738B2 JP5650738B2 JP2012523530A JP2012523530A JP5650738B2 JP 5650738 B2 JP5650738 B2 JP 5650738B2 JP 2012523530 A JP2012523530 A JP 2012523530A JP 2012523530 A JP2012523530 A JP 2012523530A JP 5650738 B2 JP5650738 B2 JP 5650738B2
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- resin
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- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- 229910052749 magnesium Inorganic materials 0.000 description 1
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- KXKVLQRXCPHEJC-UHFFFAOYSA-N methyl acetate Chemical compound COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
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- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- ILCQQHAOOOVHQJ-UHFFFAOYSA-N n-ethenylprop-2-enamide Chemical compound C=CNC(=O)C=C ILCQQHAOOOVHQJ-UHFFFAOYSA-N 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
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- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Description
直径16mmの2枚のステンレス鋼板に直径25mmとした前記電池用セパレータを挟んだ積層体を挿入し、更にエチレンカーボネートとメチルエチルカーボネートとを体積比1:2で混合した溶媒にLiPF6を1.0mol/lの濃度で溶解した電解液を注入して密閉したセルを、恒温槽に入れ、槽内の温度を1℃/minの割合で昇温し、その間に前記積層体に係る2枚のステンレス鋼板の間の抵抗値を測定し続け、前記抵抗値が40Ωになった温度を、セパレータのシャットダウン温度とする。
前記シャットダウン温度測定後に、槽内の昇温と、前記積層体に係る2枚のステンレス鋼板の間の抵抗値の測定とを継続し、前記シャットダウン温度の前後それぞれ10Ω、計20Ωの間の前記抵抗値の変化から、下記(1)式を用いてセパレータのシャットダウン速度を算出する。
[前記(1)式中、VSD:シャットダウン速度(Ω/min・cm2)、t50:抵抗値が50Ωに達するまでの経過時間(分)、t30:抵抗値が30Ωに達するまでの経過時間(分)、S:ステンレス鋼板の面積(cm2)である。]
RSD = Rf/S (2)
ここで、前記(2)式中、RSD:シャットダウン後のセパレータの抵抗値(Ω/cm2)、Rf:シャットダウン後の最高到達抵抗値(Ω)、S:ステンレス鋼板の面積(cm2)である。
d = (K4γcosθ)/P (3)
ここで、前記(3)式中、d:バブルポイント細孔径(μm)、γ:表面張力(mN/m)、θ:接触角(°)、K:キャピラリー定数、である。
C = {1−(m/t)/(Σai・ρi)}×100 (4)
ここで、前記(4)式中、ai:全体の質量を1としたときの成分iの比率、ρi:成分iの密度(g/cm3)、m:セパレータの単位面積あたりの質量(g/cm2)、t:セパレータの厚み(cm)である。
4cm×4cmに切り出した各セパレータの試験片を、クリップで固定した2枚のステンレス鋼板で挟みこみ、これらを150℃の恒温槽内に30分放置した後に取り出し、各試験片の長さを測定し、試験前の長さと比較して長さの減少割合を熱収縮率とした。
16mmφのステンレス鋼板で、25mmφに切ったセパレータを挟み込み、電解液(エチレンカーボネートとメチルエチルカーボネートとを体積比1:2で混合し、LiPF6を1.0mol/lの濃度で溶解した溶液)を注入して密閉したセルを作製した。このセルを恒温槽中で、1℃/minの割合で150℃まで昇温し、HIOKI製「3560型ミリオームハイテスター」で1KHzでの抵抗値を測定した。また、熱電対をセル表面に配置して、セル表面の温度を同時に読み取った。前記の測定で、抵抗値が40Ωとなった温度をシャットダウン温度とした。また、シャットダウン温度の前後それぞれ10Ω、計20Ωの抵抗値の変化から、前記(1)式を用いてシャットダウン速度を計算した。
耐熱性微粒子として板状ベーマイト(平均粒径1μm、アスペクト比10)1000gを水1000gに分散させ、更に有機バインダとしてSBRラテックス(固形分比率40質量%)120gを加えて均一に分散させて、耐熱多孔質層(II)形成用組成物を調製した。
耐熱性微粒子として二次粒子状ベーマイト(平均粒径0.6μm)を用いた以外は実施例1と同様にしてセパレータを作製した。このセパレータは、耐熱多孔質層(II)の空孔率が59%であり、耐熱多孔質層(II)における耐熱性微粒子の体積割合は89%であった。また、このセパレータは、熱収縮率が3%で、シャットダウン温度、シャットダウン速度およびシャットダウン後の抵抗値は、実施例1とほぼ同じであった。
耐熱性微粒子として粒状アルミナ(平均粒径0.4μm)を用いた以外は実施例1と同様にしてセパレータを作製した。このセパレータは、耐熱多孔質層(II)の空孔率が50%であり、耐熱多孔質層(II)における耐熱性微粒子の体積割合は86%であった。また、このセパレータは、熱収縮率が7%で、シャットダウン温度、シャットダウン速度、およびシャットダウン後の抵抗値は、実施例1とほぼ同じであった。
樹脂多孔質膜(I)として、PE製微多孔膜(厚み16μm、空孔率39%、PEの融点137℃)を用いた以外は実施例1と同様にしてセパレータを作製した。このセパレータは、熱収縮率が5%、シャットダウン温度は134℃、シャットダウン速度は9.2Ω/min・cm2であった。また、シャットダウン後の抵抗値は139Ω/cm2であった。
実施例1で用いた樹脂多孔質膜(I)に耐熱多孔質層(II)を形成せずにセパレータとした。このセパレータは、熱収縮率が49%、シャットダウン温度は130℃、シャットダウン速度は79Ω/min・cm2、シャットダウン後の抵抗値は>1.5kΩ/cm2であった。
負極活物質である黒鉛:95質量部と、バインダであるPVDF:5質量部とを、NMPを溶剤として均一になるように混合して負極合剤含有ペーストを調製した。この負極合剤含有ペーストを、銅箔からなる厚さ10μmの集電体の両面に、塗布長が表面790mm、裏面810mmになるように間欠塗布し、乾燥した後、カレンダー処理を行って全厚が80μmになるように負極合剤層の厚みを調整し、幅56mmになるように切断して、長さ920mm、幅56mmの負極を作製した。更にこの負極の銅箔の露出部にタブを溶接してリード部を形成した。
正極活物質であるLiNi0.6Co0.2Mn0.2O2:85質量部、導電助剤であるアセチレンブラック:10質量部、およびバインダであるPVDF:5質量部を、NMPを溶剤として均一になるように混合して、正極合剤含有ペーストを調製した。このペーストを、集電体となる厚さ20μmのアルミニウム箔の両面に、塗布長が表面795mm、裏面805mmになるように間欠塗布し、乾燥した後、カレンダー処理を行って、全厚が95μmになるように正極合剤層の厚みを調整し、幅54mmになるように切断して、長さ910mm、幅54mmの正極を作製した。更にこの正極のアルミニウム箔の露出部にタブを溶接してリード部を形成した。
製造例1で作製した負極と製造例2で作製した正極との間に、実施例1のセパレータを、耐熱多孔質層(II)が正極側となるように介在させ、渦巻状に巻回して電極巻回体を作製した。この電極巻回体を直径18mm、長さ650mmの円筒状鉄製外装缶に入れ、有機電解液(エチレンカーボネートとメチルエチルカーボネートを体積比1:2に混合した溶媒にLiPF6を濃度1.2mol/lで溶解した溶液)を注入した後に封止を行ってリチウム二次電池を作製した。
実施例1のセパレータに代えて、それぞれ実施例2〜3、比較例1〜2のセパレータを用いた以外は実施例4と同様にしてリチウム二次電池を作製した。
Claims (7)
- 樹脂多孔質膜(I)と、耐熱性微粒子を主体として含む耐熱多孔質層(II)とを少なくとも有する多層多孔質膜からなり、
樹脂多孔質膜(I)は、融点が80〜150℃の樹脂(A)を主体とする層の両側に、融点が150℃よりも高い樹脂(B)を主体とする層をそれぞれ有する積層膜であり、
前記樹脂(B)の融点は、前記樹脂(A)の融点よりも25℃以上高く、
前記融点が150℃よりも高い樹脂(B)を主体とする層の厚みが2μm以上7μm以下であり、
シャットダウン温度が100〜150℃であり、かつシャットダウン速度が50Ω/min・cm2以上であることを特徴とする電池用セパレータ。 - シャットダウン後の抵抗値が500Ω/cm2以上である請求項1に記載の電池用セパレータ。
- 樹脂多孔質膜(I)は、ポリエチレンを主体とする層の両側に、ポリプロピレンを主体とする層をそれぞれ有している請求項1または2に記載の電池用セパレータ。
- 耐熱多孔質層(II)に含まれる耐熱性微粒子が、アルミナ、シリカおよびベーマイトよりなる群から選択される少なくとも1種の微粒子である請求項1〜3のいずれかに記載の電池用セパレータ。
- 耐熱多孔質層(II)に含まれる耐熱性微粒子の少なくとも一部が、板状粒子である請求項1〜4のいずれかに記載の電池用セパレータ。
- 耐熱多孔質層(II)に含まれる耐熱性微粒子の少なくとも一部が、一次粒子が凝集した二次粒子構造を有する微粒子である請求項1〜5のいずれかに記載の電池用セパレータ。
- Liイオンを吸蔵放出可能な活物質を有する正極と、Liイオンを吸蔵放出可能な活物質を有する負極と、有機電解液と、請求項1〜6のいずれかに記載の電池用セパレータとを有することを特徴とする電池。
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WO2015022862A1 (ja) * | 2013-08-13 | 2015-02-19 | 日立マクセル株式会社 | 電気化学素子用セパレータおよび電気化学素子 |
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CN104868156A (zh) * | 2014-12-22 | 2015-08-26 | 上海恩捷新材料科技股份有限公司 | 锂离子电池 |
JP6380307B2 (ja) * | 2015-09-09 | 2018-08-29 | トヨタ自動車株式会社 | 電池用セパレータ |
KR101874159B1 (ko) * | 2015-09-21 | 2018-07-03 | 주식회사 엘지화학 | 리튬 이차전지용 전극의 제조방법 및 이로부터 제조된 리튬 이차전지용 전극 |
CN105576173A (zh) * | 2015-12-16 | 2016-05-11 | 安徽壹石通材料科技股份有限公司 | 一种陶瓷涂层材料的制备方法及其应用 |
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CN109891633B (zh) * | 2016-11-18 | 2022-09-16 | 株式会社Lg新能源 | 隔板和包括该隔板的电化学装置 |
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