JP6041343B2 - リチウム二次電池およびその製造方法 - Google Patents
リチウム二次電池およびその製造方法 Download PDFInfo
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- JP6041343B2 JP6041343B2 JP2012195246A JP2012195246A JP6041343B2 JP 6041343 B2 JP6041343 B2 JP 6041343B2 JP 2012195246 A JP2012195246 A JP 2012195246A JP 2012195246 A JP2012195246 A JP 2012195246A JP 6041343 B2 JP6041343 B2 JP 6041343B2
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- cyclic siloxane
- negative electrode
- side chain
- secondary battery
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- 238000004519 manufacturing process Methods 0.000 title claims description 17
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- 239000011255 nonaqueous electrolyte Substances 0.000 claims description 33
- 125000004432 carbon atom Chemical group C* 0.000 claims description 15
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- 239000007795 chemical reaction product Substances 0.000 claims description 14
- 125000000962 organic group Chemical group 0.000 claims description 8
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- 238000000034 method Methods 0.000 description 21
- 125000000217 alkyl group Chemical group 0.000 description 20
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- RDYLAVUUPAFWGX-UHFFFAOYSA-N dimethyl-[[4,6,8-tris(dimethylsilyloxy)-2,4,6,8-tetrakis(2-methylpropyl)-1,3,5,7,2,4,6,8-tetraoxatetrasilocan-2-yl]oxy]silane Chemical compound C(C(C)C)[Si]1(O[Si](O[Si](O[Si](O1)(O[SiH](C)C)CC(C)C)(O[SiH](C)C)CC(C)C)(O[SiH](C)C)CC(C)C)O[SiH](C)C RDYLAVUUPAFWGX-UHFFFAOYSA-N 0.000 description 1
- TYSWRMLLCVSLGQ-UHFFFAOYSA-N dimethyl-[[4,6,8-tris(dimethylsilyloxy)-2,4-diethyl-6,8-dimethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocan-2-yl]oxy]silane Chemical compound C[Si]1(O[Si](O[Si](O[Si](O1)(O[SiH](C)C)C)(O[SiH](C)C)CC)(O[SiH](C)C)CC)O[SiH](C)C TYSWRMLLCVSLGQ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000011254 layer-forming composition Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- DEUISMFZZMAAOJ-UHFFFAOYSA-N lithium dihydrogen borate oxalic acid Chemical compound B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] DEUISMFZZMAAOJ-UHFFFAOYSA-N 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- IGILRSKEFZLPKG-UHFFFAOYSA-M lithium;difluorophosphinate Chemical compound [Li+].[O-]P(F)(F)=O IGILRSKEFZLPKG-UHFFFAOYSA-M 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000005593 norbornanyl group Chemical group 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 125000005702 oxyalkylene group Chemical group 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002568 propynyl group Chemical group [*]C#CC([H])([H])[H] 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 239000003115 supporting electrolyte Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 125000004665 trialkylsilyl group Chemical group 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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Description
上記シロキシ側鎖含有環状シロキサンとしては、例えば、上記式(1)で表される化合物を好ましく採用し得る。
リチウム二次電池の正極(典型的には正極シート)を構成する正極集電体としては、導電性の良好な金属からなる導電性部材が好ましく用いられる。そのような導電性部材としては、例えば、アルミニウムまたはアルミニウムを主成分とする合金を用いることができる。正極集電体の形状は、電池の形状等に応じて異なり得るため、特に制限はなく、棒状、板状、シート状、箔状、メッシュ状等の種々の形態であり得る。正極集電体の厚さも特に限定されず、例えば5μm〜30μmとすることができる。正極活物質層は、正極活物質の他、必要に応じて導電材、結着剤(バインダ)等の添加剤を含有し得る。
(2)次の一般式(B1):Li1+αMn2−xMxO4;で表される、典型的にはスピネル構造のリチウム遷移金属酸化物。ここで、xは0≦x<2であり、典型的には0≦x≦1である。xが0より大きい場合、Mは、Mn以外の任意の金属元素または非金属元素であり得る。Mが遷移金属元素の少なくとも1種を含む組成のものが好ましい。具体例としては、LiMn2O4,LiNi0.5Mn1.5O4,LiCrMnO4等が挙げられる。
(3)次の一般式(C1):Li2+αMO3;で表されるリチウム遷移金属酸化物。ここで、Mは、Mn,Fe,Co等の遷移金属元素の少なくとも1種を含み、他の金属元素または非金属元素をさらに含み得る。具体例としては、Li2MnO3,Li2PtO3等が挙げられる。
(4)次の一般式(D1):Li1+αMPO4;で表されるリチウム遷移金属化合物(リン酸塩)。ここで、Mは、Mn,Fe,Ni,Co等の遷移金属元素の少なくとも1種を含み、他の金属元素または非金属元素をさらに含み得る。具体例としては、LiMnPO4,LiFePO4等が挙げられる。
(5)次の一般式(E1):Li2+αMPO4F;で表されるリチウム遷移金属化合物(リン酸塩)。ここで、Mは、Mn,Ni,Co等の遷移金属元素の少なくとも1種を含み、他の金属元素または非金属元素をさらに含み得る。具体例としては、LiMnPO4F等が挙げられる。
(6)Li1+αMO2とLi2+αMO3との固溶体。ここで、Li1+αMO2は上記(1)に記載の一般式(A1)で表される組成を指し、Li2+αMO3は上記(3)に記載の一般式(C1)で表される組成を指す。具体例としては、0.5LiNiMnCoO2−0.5Li2MnO3で表される固溶体が挙げられる。
なお、上記(1)〜(6)中の各組成式におけるαは、0≦α≦0.5であり、典型的には0≦α≦0.3(例えば0≦α≦0.2)が適当である。
上記一般式(B1)で表される化合物の好適例として、該一般式(B1)におけるMが少なくともNiを含む化合物、例えば、次の一般式(B2):LiNipM1 qMn2−p−qO4;で表されるスピネル構造のリチウム遷移金属酸化物が挙げられる。ここで、0<pであり、0≦qであり、p+q<2(典型的にはp+q≦1)である。好ましい一態様では、q=0であり、0.2≦p≦0.6である。上記の含有割合(上記一般式(B2)のpで示す割合)のNiを含有させることによって、スピネル構造のLiNiMn複合酸化物(例えばLiNi0.5Mn1.5O4)の充電終止時の正極電位を高電位化(典型的には4.5V(対Li/Li+)以上に高電位化)させることができ、5V級のリチウム二次電池を構築することが可能になる。上記一般式(B2)において、0<qである場合、M1は、Ni,Mn以外の任意の金属元素または非金属元素(例えば、Fe,Co,Cu,Cr,ZnおよびAlから選択される1種または2種以上)であり得る。M1が3価のFeおよびCoの少なくとも一方を含むことが好ましい。また、0<q≦0.3であり、1≦2p+qであることが好ましい。
1つのシロキシ側鎖に含まれるシロキシ基の数は、2以上(例えば2〜5程度)であってもよいが、通常は1であることが好ましい。
[シロキシ側鎖含有環状シロキサン]
化合物(a1):下記式(2)におけるR11,R12,R13およびR14がいずれもイソブチル基(−CH 2 CH(CH3)2)である環状シロキサン(2,4,6,8−テトライソブチル−2,4,6,8−テトラ(ジメチルシロキシ)シクロテトラシロキサン)
化合物(a2):下記式(2)におけるR11,R12,R13およびR14がいずれもメチル基(−CH3)である環状シロキサン
化合物(a3):下記式(2)におけるR11,R12,R13およびR14がいずれもエチル基(−CH2CH3)である環状シロキサン
化合物(a4):下記式(2)におけるR11,R12,R13およびR14がいずれもn−ノニル基(−(CH2)8CH3)である環状シロキサン
化合物(a5):下記式(2)におけるR11,R12,R13およびR14がいずれもアリル基(−CH2CH=CH2)である環状シロキサン
化合物(a6):下記式(2)におけるR11,R12,R13およびR14がいずれもフェニル基(−C6H5)である環状シロキサン
化合物(a7):下記式(2)におけるR11,R12,R13およびR14がいずれもビニル基(−CH=CH2)である環状シロキサン
化合物(a8):下記式(2)におけるR11,R12,R13およびR14がいずれも水素原子(H)である環状シロキサン
化合物(a9):下記式(2)におけるR11,R12,R13およびR14のうち2つがメチル基であり、他の2つがエチル基である環状シロキサン
化合物(b1):ヘキサメチルシクロトリシロキサン
[鎖状シロキサン]
化合物(c1):ヘキサメチルジシロキサン
[コインセルの作製]
ステンレス鋼を作用極、金属リチウムを対極とし、これらをセパレータおよび非水電解液とともにステンレス製容器に組み込んで、直径20mm、厚さ3.2mm(2032型)のコインセル(性能評価用のハーフセル)A1〜A7を構築した。セパレータとしては多孔質ポリオレフィンシートを使用した。非水電解液としては、エチレンカーボネート(EC)とエチルメチルカーボネート(EMC)との3:7(質量比)混合溶媒中に支持塩として約1mol/LのLiPF6を含む基本組成の電解液に、シロキサン化合物としての化合物(a1)を配合して、該化合物(a1)の含有率がそれぞれ表1に示す値(質量%)となるように調製したものをそれぞれ使用した。例えば、セルA3の構築には、上記基本組成の電解液と化合物(a1)とを85:15の質量比で混合して調製した電解液(化合物(a1)の含有率が15質量%である電解液)を使用した。なお、セルA5の構築には上記基本組成の電解液をそのまま使用した。
セルA1〜A7に対して、温度60℃にて、0.5mA/cm2の電流密度で、カット電圧−2.0V〜1.5V(E/V vs.(Li+/Li))の範囲で50サイクルの充放電を行った。そして、1サイクル目の充電容量(リチウムイオンをステンレス鋼にLi金属として充電した充電容量)を100%として、50サイクル目の充電容量の維持率(%)を求めた。得られた結果を表1および図4に示す。
上記基本組成の電解液と化合物(a2)〜(a9)とをそれぞれ85:15の質量比で混合して調製した電解液(すなわち、各シロキサン化合物を15質量%の含有率で含む電解液)を用いた点以外は実験例1と同様にして、コインセルB1〜B8を構築した。また、上記基本組成の電解液と化合物(b1)および(c1)とをそれぞれ85:15の質量比で混合して調製した電解液を用いた点以外は実験例1と同様にして、コインセルB9およびB10を構築した。
10 電池ケース
12 開口部
14 蓋体
20 捲回電極体
25 非水電解質(非水電解液)
30 正極(正極シート)
32 正極集電体
34 正極活物質層
35 正極集電体積層部
36 正極活物質層非形成部
37 内部正極端子
38 外部正極端子
40 負極(負極シート)
42 負極集電体
44 負極活物質層
45 負極集電体積層部
46 負極活物質層非形成部
47 内部負極端子
48 外部負極端子
50A,50B セパレータ(セパレータシート)
100 リチウム二次電池
Claims (5)
- 正極と負極と非水電解質とを備えたリチウム二次電池であって、
前記負極の表面には、環状シロキサンおよび/またはその反応生成物が存在しており、
前記環状シロキサンは、少なくとも1つのジメチルシロキシ基を側鎖に有するシロキシ側鎖含有環状シロキサンであり、
前記環状シロキサンおよび/またはその反応生成物を前記非水電解質の0.01〜20質量%含む、リチウム二次電池。 - 正極と負極とを用意すること、および
少なくとも前記負極に環状シロキサンを供給すること、を包含し、
前記環状シロキサンは、少なくとも1つのジメチルシロキシ基を側鎖に有するシロキシ側鎖含有環状シロキサンであり、
前記環状シロキサンの供給は、
前記環状シロキサンを含む非水電解質を用意すること、および
その用意した非水電解質を前記負極に供給すること、を包含し、
前記非水電解質として、前記環状シロキサンを0.01〜20質量%含む非水電解質を用いる、リチウム二次電池製造方法。 - 請求項1または2に記載のリチウム二次電池を搭載した、車両。
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