JP4656102B2 - 固体型電池 - Google Patents
固体型電池 Download PDFInfo
- Publication number
- JP4656102B2 JP4656102B2 JP2007195469A JP2007195469A JP4656102B2 JP 4656102 B2 JP4656102 B2 JP 4656102B2 JP 2007195469 A JP2007195469 A JP 2007195469A JP 2007195469 A JP2007195469 A JP 2007195469A JP 4656102 B2 JP4656102 B2 JP 4656102B2
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- JP
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- Prior art keywords
- power generation
- battery case
- solid
- battery
- generation element
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- 239000007787 solid Substances 0.000 title claims description 53
- 239000000565 sealant Substances 0.000 claims abstract description 75
- 238000010248 power generation Methods 0.000 claims abstract description 71
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 46
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000012528 membrane Substances 0.000 claims abstract description 43
- 239000012530 fluid Substances 0.000 claims description 80
- 238000007789 sealing Methods 0.000 claims description 25
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 230000002209 hydrophobic effect Effects 0.000 claims description 10
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- 239000000463 material Substances 0.000 description 9
- 229930195734 saturated hydrocarbon Natural products 0.000 description 9
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 8
- 230000006866 deterioration Effects 0.000 description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 8
- 239000011834 metal-based active material Substances 0.000 description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007774 positive electrode material Substances 0.000 description 6
- 229910018130 Li 2 S-P 2 S 5 Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000005192 partition Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000007773 negative electrode material Substances 0.000 description 4
- 239000002203 sulfidic glass Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000002388 carbon-based active material Substances 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 3
- 239000012024 dehydrating agents Substances 0.000 description 3
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 150000001924 cycloalkanes Chemical class 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002931 mesocarbon microbead Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- ZBMRKNMTMPPMMK-UHFFFAOYSA-N 2-amino-4-[hydroxy(methyl)phosphoryl]butanoic acid;azane Chemical compound [NH4+].CP(O)(=O)CCC(N)C([O-])=O ZBMRKNMTMPPMMK-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229910018091 Li 2 S Inorganic materials 0.000 description 1
- 229910018133 Li 2 S-SiS 2 Inorganic materials 0.000 description 1
- 229910011281 LiCoPO 4 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910014397 LiNi1/3Co1/3Mn1/3 Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910003289 NiMn Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- WJTCGQSWYFHTAC-UHFFFAOYSA-N cyclooctane Chemical compound C1CCCCCCC1 WJTCGQSWYFHTAC-UHFFFAOYSA-N 0.000 description 1
- 239000004914 cyclooctane Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000008279 sol Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
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- 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
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- 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
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- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
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- Sealing Battery Cases Or Jackets (AREA)
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- Primary Cells (AREA)
Description
以下、本発明の固体型電池について、固体型電池の部材と、固体型電池の構成とに分けて説明する。
本発明の固体型電池の部材について説明する。本発明の固体型電池は、少なくとも、発電要素、電池ケースおよび流動性封止剤を有し、さらに通常は、電気を取り出すための取り出し電極を有する。
まず、本発明に用いられる流動性封止剤について説明する。本発明に用いられる流動性封止剤は、電池ケース内で発電要素を封止し、硫化物系固体電解質膜と反応しない性質を有するものである。本発明において「硫化物固体電解質膜と反応しない」とは、硫化物固体電解質膜との反応で硫化水素等が発生せず、硫化物固体電解質膜の機能を実質的に劣化させないことをいう。また、本発明に用いられる流動性封止剤は流動性を有するものである。「流動性を有する」とは、固体または気体ではないことをいい、充放電等に伴う発電要素の体積変化に柔軟に追従できることをいう。従って、本発明における流動性封止剤には、通常の液体(有機溶媒)の他に、ゾル、ゲル、エマルジョン等の分散系も含まれる。また、本発明における流動性封止剤には、通常、絶縁性に優れた材料が用いられる。
以下、本発明に用いられる流動性封止剤について、電池ケースが開放型である場合と、電池ケースが密閉型である場合とに分けて説明する。
電池ケースが開放型である場合、上述した図1に示すように、流動性封止剤は大気(空気)と接することになる。そのため、流動性封止剤の疎水性は高いことが好ましい。より具体的には、流動性封止剤が疎水性液体であることが好ましい。空気中の水分が、硫化物系固体電解質膜と接触することを抑制することができるからである。
また、上記無極性液体としては、例えばベンゼン、トルエン、ジエチルエーテル、クロロホルム、酢酸エチル、テトラヒドロフランおよび塩化メチル等を挙げることができる。
なお、本発明においては、ゾル、ゲル、エマルジョン等の分散系の流動性封止剤を使用することもできる。
電池ケースが密閉型である場合、上述した図2に示すように、流動性封止剤は基本的には大気(空気)と接しない。そのため、流動性封止剤の種類は、硫化物系固体電解質膜と反応しない性質を有するものであれば特に限定されるものではない。中でも、本発明においては、流動性封止剤の疎水性が高いことが好ましく、より具体的には、流動性封止剤が疎水性液体であることが好ましい。例えば正極層等に空気が残存している場合であっても、容易に除去することができ、水分が硫化物系固体電解質膜と接触することを抑制することができるからである。なお、疎水性液体の種類等については、上述した内容と同様であるので、ここでの説明は省略する。
次に、本発明に用いられる発電要素について説明する。本発明に用いられる発電要素は、正極層、硫化物系固体電解質膜および負極層がこの順に積層されたものである。さらに通常は、正極層および負極層の集電を行う正極集電体および負極集電体が配置される。
次に、本発明に用いられる電池ケースについて説明する。本発明に用いられる電池ケースは、発電要素および流動性封止剤を収納するものである。本発明に用いられる電池ケースは、大気と流動性封止剤とが接触可能な開放型電池ケースであっても良く、接触不可能な密閉型電池ケースであっても良い。
本発明の固体型電池は、上述した部材の他に、通常、集電体に接続された取り出し電極を有する。取り出し電極の形状は、例えば箔状およびリード状等を挙げることができる。また、後述するように、本発明の固体型電池は、中間集電体、撹拌手段、温度調整手段、ガイド手段等を有していても良い。
次に、本発明の固体型電池の構成について説明する。本発明においては、電池ケースの内部に発電要素を配置し、発電要素が浸漬するように、流動性封止剤で封止を行う。これにより、硫化物系固体電解質膜が大気中の空気等と接触することを防止することができる。
[実施例1]
不活性ガス雰囲気中で、発電要素を作製した。まず、正極活物質としてLiCoO2、負極活物質としてIn箔(厚さ100μm)を用意した。次に、Li2S(日本化学工業製)およびP2S5(アルドリッチ製)を遊星型ボールミルで粉砕混合することにより、硫化物系固体電解質としてのLi2S−P2S5を形成した。次に、プレス機を用意し、負極活物質(In箔)を置き0.6t/cm2でプレスし、その上に硫化物系固体電解質(Li2S−P2S5)を添加し1.2t/cm2でプレスし、その上に正極活物質(LiCoO2)を添加し5t/cm2でプレスし、負極層/硫化物系固体電解質膜/正極層の積層体を得た。さらに、この積層体の両面を、集電体(SUS、厚さ10mm)で挟持し、発電要素を得た。
流動パラフィンを用いなかった以外は、実施例1と同様にして固体型電池を得た。
(1)硫化水素濃度の時間依存性
実施例1および比較例1で得られた固体型電池について、デシケーターのコックを閉じた状態で放置し、デシケーター内の硫化水素濃度の時間依存性を評価した。硫化水素濃度の測定には、ガスバスターライト(GBL−HS、アズワン社製)を用い、デシケーター内を大気雰囲気に置換した時から、10分後、1日後、2日後、10日後に測定を行った。その結果を表1に示す。
実施例1および比較例1で得られた固体型電池について、内部抵抗の変化を評価した。内部抵抗には交流インピーダンス法を用い、以下の条件で測定を行った。
周波数範囲:10MHz〜0.1Hz
電圧振幅 :5mV
装置 :Solartron社製、1260型インピーダンスアナライザー
なお、ここでは、デシケーター内を大気雰囲気に置換する前の段階での抵抗(初期抵抗)と、置換から2日経過した後の段階での抵抗(大気暴露2日後の抵抗)とを測定した。その結果を図8および表2に示す。
実施例1で得られた固体型電池の充放電容量を測定した。充放電の条件を以下に示す。
電流密度:127μA/cm2
充放電の切替条件
(1)充電:3.59Vにて充電終止
(2)放電:2Vにて放電終止
その結果を図9に示す。図9に示されているように、実施例1で得られた固体型電池は、LiCoO2に対して、100mAh/gの以上の充放電容量を有することが確認された。
このことから、発電要素を流動性封止剤(流動パラフィン)に浸漬した状態であっても、二次電池として機能することが確認された。
2 … 硫化物系固体電解質膜
3 … 負極層
4 … 集電体
5 … 発電要素
6 … 電池ケース
7 … 流動性封止剤
8 … 取り出し電極
Claims (10)
- 正極層、硫化物系固体電解質膜および負極層がこの順に積層された発電要素と、前記発電要素を収納する電池ケースと、前記電池ケース内で前記発電要素を浸漬させ、前記発電要素に接触し、かつ、前記硫化物系固体電解質膜と反応しない性質を有する流動性封止剤と、を有することを特徴とする固体型電池。
- 前記流動性封止剤が、疎水性液体であることを特徴とする請求項1に記載の固体型電池。
- 前記疎水性液体が、流動パラフィンであることを特徴とする請求項2に記載の固体型電池。
- 前記発電要素が、中間集電体を介して複数積層されていることを特徴とする請求項1から請求項3までのいずれかの請求項に記載の固体型電池。
- 前記電池ケースが、開放型電池ケースであることを特徴とする請求項1から請求項4までのいずれかの請求項に記載の固体型電池。
- 前記電池ケースが、密閉型電池ケースであることを特徴とする請求項1から請求項4までのいずれかの請求項に記載の固体型電池。
- 前記流動性封止剤を撹拌する撹拌手段を有することを特徴とする請求項1から請求項6までのいずれかの請求項に記載の固体型電池。
- 前記撹拌手段が、前記流動性封止剤を、前記電池ケースに連結された外部経路を通じて循環させる手段であることを特徴とする請求項7に記載の固体型電池。
- 前記流動性封止剤を加熱または冷却する温度調整手段を有することを特徴とする請求項1から請求項8までのいずれかの請求項に記載の固体型電池。
- 前記発電要素が、前記電池ケースの底面側に、気泡を逃すガイド手段を有することを特徴とする請求項1から請求項9までのいずれかの請求項に記載の固体型電池。
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JP2007195469A JP4656102B2 (ja) | 2007-07-27 | 2007-07-27 | 固体型電池 |
DE602008005024T DE602008005024D1 (de) | 2007-07-27 | 2008-07-28 | Feststoffbatterie |
AT08826826T ATE498914T1 (de) | 2007-07-27 | 2008-07-28 | Feststoffbatterie |
KR1020107001662A KR101095173B1 (ko) | 2007-07-27 | 2008-07-28 | 고체형 전지 |
US12/663,553 US8481204B2 (en) | 2007-07-27 | 2008-07-28 | Solid-state battery |
EP08826826A EP2171777B1 (en) | 2007-07-27 | 2008-07-28 | Solid-state battery |
CN2008800156690A CN101730950B (zh) | 2007-07-27 | 2008-07-28 | 固态电池 |
CA2673955A CA2673955C (en) | 2007-07-27 | 2008-07-28 | Solid-state battery |
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Also Published As
Publication number | Publication date |
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EP2171777B1 (en) | 2011-02-16 |
CN101730950B (zh) | 2012-10-10 |
EP2171777A2 (en) | 2010-04-07 |
CA2673955A1 (en) | 2009-02-05 |
CN101730950A (zh) | 2010-06-09 |
JP2009032539A (ja) | 2009-02-12 |
US20100178554A1 (en) | 2010-07-15 |
WO2009016510A2 (en) | 2009-02-05 |
DE602008005024D1 (de) | 2011-03-31 |
ATE498914T1 (de) | 2011-03-15 |
KR101095173B1 (ko) | 2011-12-16 |
WO2009016510A3 (en) | 2009-06-04 |
US8481204B2 (en) | 2013-07-09 |
KR20100032436A (ko) | 2010-03-25 |
CA2673955C (en) | 2011-02-22 |
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