JP5545650B2 - 非水電解質電池用セパレータおよび非水電解質電池 - Google Patents
非水電解質電池用セパレータおよび非水電解質電池 Download PDFInfo
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- JP5545650B2 JP5545650B2 JP2010151535A JP2010151535A JP5545650B2 JP 5545650 B2 JP5545650 B2 JP 5545650B2 JP 2010151535 A JP2010151535 A JP 2010151535A JP 2010151535 A JP2010151535 A JP 2010151535A JP 5545650 B2 JP5545650 B2 JP 5545650B2
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 150000005676 cyclic carbonates Chemical class 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 239000005042 ethylene-ethyl acrylate Substances 0.000 description 1
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical group OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 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
- 150000002576 ketones Chemical class 0.000 description 1
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N methyl acetate Chemical compound COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- DTIFFOYIBPJUET-UHFFFAOYSA-N n'-(3-trimethylsilylpropyl)ethane-1,2-diamine Chemical compound C[Si](C)(C)CCCNCCN DTIFFOYIBPJUET-UHFFFAOYSA-N 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 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
- 239000012169 petroleum derived wax Substances 0.000 description 1
- 235000019381 petroleum wax Nutrition 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920003050 poly-cycloolefin Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Cell Separators (AREA)
- Secondary Cells (AREA)
Description
[前記一般式(1)中、nは正の整数であり、RはHまたは炭素数1〜10のアルキル基である。]
BR = (V0/Vi)−1 (2)
[前記式中、V0は、非水電解液中に25℃で24時間浸漬後の熱膨潤性微粒子の体積(cm3)、Viは、非水電解液に浸漬する前の熱膨潤性微粒子の体積(cm3)をそれぞれ表す。]
BT = (V1/V0)−1 (3)
[前記式中、V0は、非水電解液中に25℃で24時間浸漬後の熱膨潤性微粒子の体積(cm3)、V1は、非水電解液中に25℃で24時間浸漬後、非水電解液を120℃に昇温させ、120℃で1時間経過後における熱膨潤性微粒子の体積(cm3)をそれぞれ表す。]
VB = (M0−Mi)/PB (5)
VC = M1/PC−M0/PB (6)
VV = Mi×(1−W)/PV (7)
V0 = Vi+VB−VV×(BB+1) (8)
VD = VV×(BB+1) (9)
BT = {V0+VC−VD×(BC+1)}/V0−1 (10)
ここで、前記式(4)〜(10)中、
Vi:非水電解液に浸漬する前の熱膨潤性微粒子の体積(cm3)、
V0:非水電解液中に25℃で24時間浸漬後の熱膨潤性微粒子の体積(cm3)、
VB:非水電解液中に常温で24時間浸漬後に、フィルムに吸収された非水電解液の体積(cm3)、
Vc:非水電解液中に常温に24時間浸漬した時点から、非水電解液を120℃まで昇温させ、更に120℃で1時間経過するまでの間に、フィルムに吸収された非水電解液の体積(cm3)、
VV:非水電解液に浸漬する前のバインダ樹脂の体積(cm3)、
VD:非水電解液中に常温で24時間浸漬後のバインダ樹脂の体積(cm3)、
Mi:非水電解液に浸漬する前のフィルムの質量(g)、
M0:非水電解液中に常温で24時間浸漬後のフィルムの質量(g)、
Ml:非水電解液中に常温で24時間浸漬した後、非水電解液を120℃まで昇温させ、更に120℃で1時間経過した後におけるフィルムの質量(g)、
W:非水電解液に浸漬する前のフィルム中の熱膨潤性微粒子の質量比率、
PA:非水電解液に浸漬する前の熱膨潤性微粒子の比重(g/cm3)、
PB:常温における非水電解液の比重(g/cm3)、
PC:所定温度での非水電解液の比重(g/cm3)、
PV:非水電解液に浸漬する前のバインダ樹脂の比重(g/cm3)、
BB:非水電解液中に常温で24時間浸漬後のバインダ樹脂の膨潤度、
BC:前記(3)式で定義される昇温時のバインダ樹脂の膨潤度
である。
P ={1−(m/t)/(Σai・ρi)}×100 (11)
ここで、前記式中、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。
前記式(13)中、D:バブルポイント法による細孔径(m)、γ:液体の表面張力(N/m)、Px:バブルポイントでの圧力(Pa)である。
製造例1
シランカップリング剤である(3−Trimethoxysilylpropyl)diethylenetriamine:10gを、0.5質量%濃度の酢酸水溶液500g中に入れて攪拌し、均一に溶解させてシランカップリング剤溶液を調製した。
シランカップリング剤を(Aminoethylaminomethyl)phenethyltrimethoxysilaneに変更し、無機微粒子を二次粒子状のベーマイト(平均粒子径0.6μm)に変更した以外は、製造例1と同様にしてポリアミン基含有無機微粒子(A−2)を製造した。
シランカップリング剤をN−(2−Aminoethyl)−3−aminopropyltrimethoxysilaneに変更し、無機微粒子を板状ベーマイト(平均粒子径1μm、アスペクト比10)1000gに変更した以外は、製造例1と同様にしてポリアミン基含有無機微粒子(A−3)を製造した。
有機微粒子であるクロロメチルスチレン−ジビニルベンゼン共重合体粒子(平均粒子径0.8μm)10gを、メタノール10gおよびイオン交換水80gにトリエチレンテトラミン15gを溶解した溶液中に入れ、60℃で5時間反応させた。その後反応物を濾別し、イオン交換水で洗浄し、乾燥させてポリアミン基含有有機微粒子(B−1)を得た。
有機微粒子を、グリシジルメタクリレートと、メチルメタクリレートと、トリメチロールプロパンジメタクリレートとの共重合体粒子(平均粒子径0.4μm)に変更した以外は、製造例4と同様にしてポリアミン基含有有機微粒子(B−2)を製造した。
<負極の作製>
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、N−メチル−2−ピロリドン(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320mm、裏面260mm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142μmになるように負極合剤層の厚みを調整し、幅45mmになるように切断して、長さ330mm、幅45mm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LiMn1.5Ni0.5O4:85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15μmのアルミニウム箔の両面に、塗布長が表面320mm、裏面260mm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150μmになるように正極合剤層の厚みを調整し、幅43mmになるように切断して、長さ330mm、幅43mm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で製造したポリアミン基含有無機微粒子(A−1)1000gを1000gの水中に分散させ、更にバインダとして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セパレータ形成用スラリーを調製した。
前記の負極と前記の正極とを、前記のセパレータを介在させつつ重ね合わせ、渦巻状に巻回して巻回電極体を作製した。この巻回電極体を押し潰して扁平状にし、電池容器内に装填して、非水電解液(エチレンカーボネートとエチルメチルカーボネートを体積比1:2で混合した溶媒にLiPF6を1.2mol/lの濃度で溶解させた溶液)を電池容器内に注入した後、封止を行って、リチウム二次電池とした。
ポリアミン基含有無機微粒子(A−1)に代えて、製造例2で製造したポリアミン基含有無機微粒子(A−2)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、このセパレータを用いた以外は、実施例1と同様にしてリチウム二次電池を作製した。なお、前記セパレータの、ポリアミン基含有無機微粒子(A−2)を含有する層におけるポリアミン基含有無機微粒子(A−2)の体積割合は、この層の構成成分の全体積中、87体積%である。また、前記セパレータ中のポリアミン基の量は、NH基の量で、0.3mmol/m2であった。
ポリアミン基含有無機微粒子(A−1)に代えて、製造例3で製造したポリアミン基含有無機微粒子(A−3)を用いた以外は、実施例1と同様にしてセパレータ形成用スラリーを調製した。
製造例4で製造したポリアミン基含有有機微粒子(B−1)500gおよび二次粒子状ベーマイト(平均粒子径0.6μm)100gを1000gの水中に分散させ、更にバインダとして自己架橋性のアクリル樹脂エマルジョン(固形分比率45質量%)100gを加えて均一に分散させてセパレータ形成用スラリーを調製した。
ポリアミン基含有有機微粒子(B−1)に代えて、製造例5で製造したポリアミン基含有有機微粒子(B−2)を用いた以外は、実施例4と同様にしてセパレータを作製し、このセパレータを用いた以外は、実施例1と同様にしてリチウム二次電池を作製した。なお、前記セパレータの、ポリアミン基含有有機微粒子(B−2)を含有する層におけるポリアミン基含有有機微粒子(B−2)の体積割合は、この層の構成成分の全体積中、53体積%である。また、前記セパレータ中のポリアミン基の量は、NH基の量で、8.0mmol/m2であった。
セパレータに、PE製微多孔膜(厚み25μm、空孔率45%)を用いた以外は、実施例1と同様にしてリチウム二次電池を作製した。
ポリアミン基含有無機微粒子(B−2)に代えて、二次粒子状ベーマイト(平均粒子径0.6μm)を用いた以外は、実施例2と同様にしてリチウム二次電池を作製した。
実施例および比較例のリチウム二次電池について、以下の条件で初期化を実施した後、充放電試験を実施した。
実施例および比較例のリチウム二次電池について、以下の条件で高温貯蔵特性を評価した。
実施例および比較例のリチウム電池を恒温槽に入れ、30℃から150℃まで毎分1℃の割合で温度上昇させて加熱し、電池の内部抵抗の温度変化を求めた。そして、抵抗値が30℃での値の5倍以上に上昇したときの温度を、シャットダウン温度とした。また、150℃に昇温後30分保持して、各電池の状態の変化を調べた。
Claims (4)
- 非水電解質電池に用いられるセパレータであって、
ポリオレフィンを主体とする多孔質膜と、下記一般式(1)で表されるポリアミン基を含有しかつ平均粒子径が0.01〜15μmの微粒子を含む多孔質層とを少なくとも有する多層多孔質膜により構成されていることを特徴とする非水電解質電池用セパレータ。
−NH(CH2CH2NH)nR (1)
[前記一般式(1)中、nは正の整数であり、RはHまたは炭素数1〜10のアルキル基である。] - 前記微粒子は、無機微粒子および有機微粒子より選択される少なくとも1種である請求項1に記載の非水電解質電池用セパレータ。
- 80〜150℃の温度範囲で孔が閉塞するシャットダウン特性を有している請求項1または2に記載の非水電解質電池用セパレータ。
- 正極、負極、セパレータおよび非水電解液を有する非水電解質電池であって、
前記セパレータが、請求項1〜3のいずれかに記載の非水電解質電池用セパレータであることを特徴とする非水電解質電池。
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