JP5065233B2 - リチウム2次電池用負極活物質、その製造方法、及びこれを含むリチウム2次電池 - Google Patents
リチウム2次電池用負極活物質、その製造方法、及びこれを含むリチウム2次電池 Download PDFInfo
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- JP5065233B2 JP5065233B2 JP2008301611A JP2008301611A JP5065233B2 JP 5065233 B2 JP5065233 B2 JP 5065233B2 JP 2008301611 A JP2008301611 A JP 2008301611A JP 2008301611 A JP2008301611 A JP 2008301611A JP 5065233 B2 JP5065233 B2 JP 5065233B2
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- active material
- negative electrode
- secondary battery
- lithium secondary
- electrode active
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- 239000007773 negative electrode material Substances 0.000 title claims description 77
- 229910052744 lithium Inorganic materials 0.000 title claims description 71
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 67
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 239000000126 substance Substances 0.000 claims description 49
- 239000000463 material Substances 0.000 claims description 32
- 239000011148 porous material Substances 0.000 claims description 27
- -1 polytetrafluoroethylene Polymers 0.000 claims description 21
- 229920005596 polymer binder Polymers 0.000 claims description 18
- 239000002491 polymer binding agent Substances 0.000 claims description 18
- 239000011230 binding agent Substances 0.000 claims description 17
- 239000004642 Polyimide Substances 0.000 claims description 15
- 229920001721 polyimide Polymers 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 239000000956 alloy Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 7
- 239000011149 active material Substances 0.000 claims description 7
- 229910001416 lithium ion Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
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- 239000007774 positive electrode material Substances 0.000 claims description 5
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- 150000005676 cyclic carbonates Chemical class 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
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- CYEDOLFRAIXARV-UHFFFAOYSA-N ethyl propyl carbonate Chemical compound CCCOC(=O)OCC CYEDOLFRAIXARV-UHFFFAOYSA-N 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
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- KKQAVHGECIBFRQ-UHFFFAOYSA-N methyl propyl carbonate Chemical compound CCCOC(=O)OC KKQAVHGECIBFRQ-UHFFFAOYSA-N 0.000 description 2
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- 229940057061 mevalonolactone Drugs 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- GHZRKQCHJFHJPX-UHFFFAOYSA-N oxacycloundecan-2-one Chemical compound O=C1CCCCCCCCCO1 GHZRKQCHJFHJPX-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 239000011871 silicon-based negative electrode active material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 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
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Description
LiaA1−bBbD2
(前記式で、0.95≦a≦1.1、0≦b≦0.5である)
LiaE1−bBbO2−cFc
(前記式で、0.95≦a≦1.1、0≦b≦0.5、0≦c≦0.05である)
LiE2−bBbO4−cFc
(前記式で、0≦b≦0.5、0≦c≦0.05である)
LiaNi1−b−cCobBcDα
(前記式で、0.95≦a≦1.1、0≦b、≦0.5、0≦c≦0.05、0<α≦2である)
LiaNi1−b−cCobBcO2−αFα
(前記式で、0.95≦a≦1.1、0≦b≦0.5、0≦c≦0.05、0<α<2である)
LiaNi1−b−cCobBcO2−αF2
(前記式で、0.95≦a≦1.1、0≦b≦0.5、0≦c≦0.05、0<α<2である)
LiaNi1−b−cMnbBcDα
(前記式で、0.95≦a≦1.1、0≦b≦0.5、0≦c≦0.05、0<α≦2である)
LiaNi1−b−cMnbBcO2−αFα
(前記式で、0.95≦a≦1.1、0≦b≦0.5、0≦c≦0.05、0<α<2である)
LiaNi1−b−cMnbBcO2−αF2
(前記式で、0.95≦a≦1.1、0≦b≦0.5、0≦c≦0.05、0<α<2である)
LiaNibEcGdO2
(前記式で、0.90≦a≦1.1、0≦b≦0.9、0≦c≦0.5、0.001≦d≦0.1である)
LiaNibCocMndGeO2
(前記式で、0.90≦a≦1.1、0≦b≦0.9、0≦c≦0.5、0≦d≦0.5、0.001≦e≦0.1である)
LiaNiGbO2
(前記式で、0.90≦a≦1.1、0.001≦b≦0.1である)
LiaCoGbO2
(前記式で、0.90≦a≦1.1、0.001≦b≦0.1である)
LiaMnGbO2
(前記式で、0.90≦a≦1.1、0.001≦b≦0.1である)
LiaMn2GbO4
(前記式で、0.90≦a≦1.1、0.001≦b≦0.1である)
QO2
QS2
LiQS2
V2O5
LiV2O5
LiIO2
LiNiVO4
Li(3−f)J2(PO4)3(0≦f≦3)
Li(3−f)Fe2(PO4)3(0≦f≦2)
Si系合金をアーク溶解法で溶解して溶融放射した後、4000rpmの速度で急冷凝固して、平均の厚さが5umであり、縦横比が2であるリボンタイプの薄片を製造した。製造したリボンタイプの薄片及びポリメチルメタクリレートを85:15の重量比で混合した。この混合物を窒素雰囲気で400℃で焼成して、気孔の大きさが0.1μm以上であり、気孔度が65%である負極活物質を製造した。
リボンタイプの薄片、ポリメチルメタクリレート、及び結合バインダーであるポリイミドを85:7.5:7.5の重量比で混合したことを除いては、実施例1と同一に実施して、負極活物質を製造した。
ポリメチルメタクリレートをポリブタヂエンラバーに変更したことを除いては、実施例1と同一に実施して、負極活物質を製造した。
ポリイミドをカルボキシメチルセルロースに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをジアセチルセルロースに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをヒドロキシプロピルセルロースに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをポリ塩化ビニルに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをポリビニルピロリドンで変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをポリテトラフルオロエチレンに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをポリフッ化ビニリデンに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
ポリイミドをポリエチレンに変更したことを除いては、実施例2と同一に実施して、負極活物質を製造した。
Si系合金粉末を負極活物質として使用した。
前記実施例1乃至11によって製造された負極活物質のSEM写真(×5,000)を撮影し、このうちの実施例1のSEM写真(×5,000)を図4に示した。図4を参照すると、負極活物質は、平均の粒径が約10umである球状の組立体からなり、組立体の内部には粒径が0.1um以上である気孔が形成された。
実施例1乃至11及び比較例1によって製造された負極活物質を利用してコインセルを製造した後、電池の特性を評価し、このうちの実施例1乃至4及び比較例1の結果を下記の表1に示した。電池の特性は、実施例1乃至11及び比較例1の負極活物質を利用して製造された各々のコインセルを0.1Cで1回充放電し、化成工程を実施した後、0.5Cで1回充放電した後の放電容量対比の100回充放電した後の放電容量維持率(%)で示した。
2 板状の物質
3 空間部
4 低温焼成高分子バインダー
10 球状の組立体
12 板状の物質
13 気孔
100 リチウム2次電池
110 電極群
112 正極
113 負極
114 セパレータ
120 ケース
140 キャップ組立体
Claims (18)
- リチウムのドープ及び脱ドープが可能な板状の物質が結合して形成された球状の組立体を含み、
前記組立体の内部には気孔が形成され、
前記板状の物質は、Si系、Sn系、Al系、Ge系、これらの合金、及びこれらの組み合わせからなる群より選択される、リチウム2次電池用負極活物質。 - 前記板状の物質は、平均の厚さが1乃至30umである、請求項1に記載のリチウム2次電池用負極活物質。
- 前記板状の物質は、縦横比が1乃至3である、請求項1に記載のリチウム2次電池用負極活物質。
- 前記気孔は、前記板状の物質と板状の物質とが接触して形成された空間部である、請求項1に記載のリチウム2次電池用負極活物質。
- 前記気孔は、平均の粒径が0.1乃至5umである、請求項1に記載のリチウム2次電池用負極活物質。
- 前記気孔は、平均の粒径が0.5乃至2umである、請求項5に記載のリチウム2次電池用負極活物質。
- 前記組立体は、気孔度が20乃至80%である、請求項1に記載のリチウム2次電池用負極活物質。
- 前記組立体は、気孔度が30乃至70%である、請求項7に記載のリチウム2次電池用負極活物質。
- 前記負極活物質は、ポリイミド、ポリビニルアルコール、カルボキシメチルセルロース、ヒドロキシプロピルセルロース、ジアセチルセルロース、ポリ塩化ビニル、ポリビニルピロリドン、ポリテトラフルオロエチレン、ポリフッ化ビニリデン、ポリエチレン、ポリプロピレン、及びこれらの組み合わせからなる群より選択される結合バインダーをさらに含む、請求項1に記載のリチウム2次電池用負極活物質。
- リチウムのドープ及び脱ドープが可能な板状の物質を製造する段階;
前記板状の物質及び低温焼成高分子バインダーを混合して混合物を製造する段階;及び
前記混合物を低温焼成して、内部に気孔が形成された球状の組立体を含む負極活物質を製造する段階;を含み、
前記板状の物質は、Si系、Sn系、Al系、Ge系、これらの合金、及びこれらの組み合わせからなる群より選択される、リチウム2次電池用負極活物質の製造方法。 - 前記混合物の製造時に結合バインダーをさらに添加する、請求項10に記載のリチウム2次電池用負極活物質の製造方法。
- 前記低温焼成高分子バインダーは400℃以下で除去される、請求項10に記載のリチウム2次電池用負極活物質の製造方法。
- 前記低温焼成高分子バインダーは150乃至400℃で除去される、請求項12に記載のリチウム2次電池用負極活物質の製造方法。
- 前記低温焼成高分子バインダーは、アクリレート系ポリマー、ブタジエンラバー系ポリマー、及びこれらの組み合わせからなる群より選択される、請求項10に記載のリチウム2次電池用負極活物質の製造方法。
- 前記結合バインダーは、ポリイミド、ポリビニルアルコール、カルボキシメチルセルロース、ヒドロキシプロピルセルロース、ジアセチルセルロース、ポリ塩化ビニル、ポリビニルピロリドン、ポリテトラフルオロエチレン、ポリフッ化ビニリデン、ポリエチレン、ポリプロピレン、及びこれらの組み合わせからなる群より選択される、請求項11に記載のリチウム2次電池用負極活物質の製造方法。
- 前記リチウムのドープ及び脱ドープが可能な板状の物質及び低温焼成高分子バインダーは、95:5乃至50:50の重量比で混合される、請求項10に記載のリチウム2次電池用負極活物質の製造方法。
- 前記焼成段階は400℃以下の温度で実施される、請求項10に記載のリチウム2次電池用負極活物質の製造方法。
- 請求項1乃至請求項9のいずれか一項によるリチウム2次電池用負極活物質を含む負極;
リチウムイオンを可逆的に挿入及び脱離することができる正極活物質を含む正極;及び
電解液;を含む、リチウム2次電池。
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US8257864B2 (en) * | 2009-06-29 | 2012-09-04 | 3M Innovative Properties Company | Method of making tin-based alloys for negative electrode compositions |
US9077029B2 (en) * | 2010-02-23 | 2015-07-07 | Samsung Sdi Co., Ltd. | Negative active material for rechargeable lithium battery and rechargeable lithium battery including the same |
CN102195038B (zh) * | 2010-03-05 | 2015-04-15 | 宁波杉杉新材料科技有限公司 | 一种锂离子电池及其负极材料和制备方法 |
JP5617457B2 (ja) * | 2010-09-08 | 2014-11-05 | 株式会社豊田中央研究所 | 蓄電デバイス用電極材料、蓄電デバイス用電極、蓄電デバイスおよび蓄電デバイス用電極材料の製造方法 |
JP5844048B2 (ja) * | 2011-02-01 | 2016-01-13 | 三洋電機株式会社 | 非水電解質二次電池 |
JP5617744B2 (ja) * | 2011-03-31 | 2014-11-05 | Tdk株式会社 | 活物質粒子、活物質、電極及びリチウムイオン二次電池 |
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