JP5269692B2 - 正極の形成方法 - Google Patents
正極の形成方法 Download PDFInfo
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- JP5269692B2 JP5269692B2 JP2009115433A JP2009115433A JP5269692B2 JP 5269692 B2 JP5269692 B2 JP 5269692B2 JP 2009115433 A JP2009115433 A JP 2009115433A JP 2009115433 A JP2009115433 A JP 2009115433A JP 5269692 B2 JP5269692 B2 JP 5269692B2
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 229910000733 Li alloy Inorganic materials 0.000 claims abstract description 35
- 239000001989 lithium alloy Substances 0.000 claims abstract description 34
- 238000009832 plasma treatment Methods 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 10
- -1 polyparaphenylene benzobisoxazole Polymers 0.000 claims description 9
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 5
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- 229910052751 metal Inorganic materials 0.000 claims description 4
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- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910012851 LiCoO 2 Inorganic materials 0.000 claims description 3
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 3
- 229910013716 LiNi Inorganic materials 0.000 claims description 3
- 229910013290 LiNiO 2 Inorganic materials 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 229910021450 lithium metal oxide Inorganic materials 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 claims description 2
- 229910010586 LiFeO 2 Inorganic materials 0.000 claims description 2
- 229910016087 LiMn0.5Ni0.5O2 Inorganic materials 0.000 claims description 2
- 229910014071 LiMn1/3Co1/3Ni1/3O2 Inorganic materials 0.000 claims description 2
- 229910014689 LiMnO Inorganic materials 0.000 claims description 2
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- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- ICXAPFWGVRTEKV-UHFFFAOYSA-N 2-[4-(1,3-benzoxazol-2-yl)phenyl]-1,3-benzoxazole Chemical compound C1=CC=C2OC(C3=CC=C(C=C3)C=3OC4=CC=CC=C4N=3)=NC2=C1 ICXAPFWGVRTEKV-UHFFFAOYSA-N 0.000 claims 2
- 239000012300 argon atmosphere Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000007740 vapor deposition Methods 0.000 claims 1
- 229910052744 lithium Inorganic materials 0.000 abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 12
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- 238000001237 Raman spectrum Methods 0.000 description 7
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 7
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 6
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910013870 LiPF 6 Inorganic materials 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 5
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- 238000010884 ion-beam technique Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 2
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 2
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- 238000005240 physical vapour deposition Methods 0.000 description 2
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- 229940090181 propyl acetate Drugs 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 238000001552 radio frequency sputter deposition Methods 0.000 description 2
- 238000001289 rapid thermal chemical vapour deposition Methods 0.000 description 2
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- 238000004544 sputter deposition Methods 0.000 description 2
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- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- GEWWCWZGHNIUBW-UHFFFAOYSA-N 1-(4-nitrophenyl)propan-2-one Chemical compound CC(=O)CC1=CC=C([N+]([O-])=O)C=C1 GEWWCWZGHNIUBW-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- 229910011939 Li2.6 Co0.4 N Inorganic materials 0.000 description 1
- 229910010199 LiAl Inorganic materials 0.000 description 1
- 229910010238 LiAlCl 4 Inorganic materials 0.000 description 1
- 229910015015 LiAsF 6 Inorganic materials 0.000 description 1
- 229910013063 LiBF 4 Inorganic materials 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- 229910013528 LiN(SO2 CF3)2 Inorganic materials 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 229910012424 LiSO 3 Inorganic materials 0.000 description 1
- 229910012513 LiSbF 6 Inorganic materials 0.000 description 1
- 229910013391 LizN Inorganic materials 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- MYWGVEGHKGKUMM-UHFFFAOYSA-N carbonic acid;ethene Chemical compound C=C.C=C.OC(O)=O MYWGVEGHKGKUMM-UHFFFAOYSA-N 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
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- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PVADDRMAFCOOPC-UHFFFAOYSA-N germanium monoxide Inorganic materials [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 150000002641 lithium Chemical class 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 125000005439 maleimidyl group Chemical class C1(C=CC(N1*)=O)=O 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 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
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002294 plasma sputter deposition Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 210000001578 tight junction Anatomy 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
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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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Description
比較例1
500nmの厚さのLiMn2O4層はステンレス基板上でマグネトロンスパッタリングされ、600℃でアニールされる。上述のLiMn2O4表面は、集束イオンビームにより切断されて、分析され、電子線回折スペクトルは図3Aで示され、ESCAスペクトルは図4で示され、RAMANスペクトルは図5で示され、上表面のSEMイメージは図6で示される。図6のように、付加的なプラズマ処理がないLiMn2O4表面は不均一で、粒子も粗く、大きい。
500nmの厚さのLiMn2O4層はステンレス基板上でマグネトロンスパッタリングされ、600℃でアニールされ、Rfプラズマにより処理される。Rfプラズマに用いられる電力は30Wで、大気処理はアルゴンで、処理温度は100℃以下で、処理期間は30分である。プラズマ処理後のLiMn2O4層は、図4で示されるESCAスペクトル、図5で示されるRAMANスペクトルを有する。
実施例2は実施例1と同様で、異なるのは、プラズマ処理に用いられる電力が、実施例2では50Wであることである。プラズマ処理後のLiMn2O4表面層は、集束イオンビームにより切断されて、分析され、電子線回折スペクトルは図3Bで示され、ESCAスペクトルは図4で示され、RAMANスペクトルは図5で示され、上表面のSEMイメージは図7Aで示される。図7Aのように、付加的なプラズマ処理後のLiMn2O4表面は均一、緻密で、平坦である。極細で、緊密な接合のナノ粒子が上表面上に形成されるので、SEMにより効果的に粒子を分析することが困難である。図7Bは、図3Bと同じ表面部分の明視野像を示し、ナノ粒子の緊密な接合構造を示す。
実施例3は実施例1と同様で、異なるのは、プラズマ処理に用いられる電力が、実施例3では80Wであることである。プラズマ処理後のLiMn2O4表面層は、図4で示されるESCAスペクトル、図5で示されるRAMANスペクトルを有する。
比較例1の電極は、EC/EMCの1M LiPF6電解質に入れられる。電極は、室温(25℃)で、順方向電流と逆電流(0.3mA/mg) 、および、電圧(1.5 〜 4.5 V vs. Li/Li+)により充電/放電されて、その容量(mAh/g)を測定する。図8で示されるように、第1回目の充電/放電曲線 (最も右側の曲線) は140mAh/gの容量を有する。充電/放電周期の増加に伴い、曲線は左側にシフトする。20回の充電/放電で、その容量は僅か115mAh/gである。
実施例2の電極は、EC/EMCの1M LiPF6電解質に入れられる。電極は、室温(25℃)で、順方向電流と逆電流(0.3mA/mg)、および、電圧(2.0〜4.5 V vs. Li/Li+)により充電/放電されて、その容量(mAh/g)を測定する。図10で示されるように、第1〜20回の充電/放電曲線は、ほぼ重畳し、140mAh/gを維持する。
2 容置領域
3 負極
5 隔離膜
6 封止構造
7 上電極
8 アノードシールド
9 閉磁場
10 下電極
Claims (6)
- 正極の形成方法であって、
基板を提供するステップと、
リチウム合金酸化層を前記基板上に形成するステップと、
アルゴン雰囲気下、150℃以下の温度で、プラズマ処理を実行して、前記リチウム合金酸化層を改質するステップと、からなり、
前記プラズマ処理は、出力密度が0.8W/cm 2 〜 5W/cm 2 、濃度が10 11 〜 10 13 cm -3 で、電子温度は1〜2eVで行い、
前記リチウム合金酸化層の上表面は、均一、緻密、緊密に接合したナノ粒子を形成し、内部/下方は、そのまま大きい粒子を維持しており、前記リチウム合金酸化層の上表面と、内部/下方とは、同一の化学成分および結晶構造であることを特徴とする正極の形成方法。 - 前記基板は、ステンレス、ポリアミド、アクリロニトリル・ブタジエン・スチレン(ABS)、 雲母(mica)、ガラス(glass)、ポリ(エチレンテフタレート)(poly(ethyleneterephthalate、PET)、ポリパラフェニレンベンゾビスオキサゾール(poly-p-phenylene-benzobisoxazole、PBO)、或いは、エポキシ樹脂(epoxy resin)であることを特徴とする請求項1に記載の正極の形成方法。
- 前記リチウム金属酸化物は、LiMnO2、LiMn2O4、LiCoO2、LiCr2O7、Li2CrO4、LiNiO2、LiFeO2、LiNixCo1-xO2、LiFePO4、LiMn0.5Ni0.5O2、LiMn1/3Co1/3Ni1/3O2、LiMc0.5Mn1.5O4、或いは、それらの組み合せで、0<x<1、且つ、Mcは二価金属であることを特徴とする請求項1または2に記載の正極の形成方法。
- 前記基板上にリチウム合金酸化層を形成するステップは、粉末プレス、気相蒸着、或いは、化学溶液合成蒸着であることを特徴とする請求項1〜3のいずれかに記載の正極の形成方法。
- 前記プラズマ処理は、プラズマチャンバを用いて、高密度、低エネルギーのプラズマを提供するステップを含み、前記プラズマチャンバは、アノードシールド、誘導結合されたコイルを有し、かつ、前記プラズマチャンバは、閉磁界を形成可能であることを特徴とする請求項1〜4のいずれかに記載の正極の形成方法。
- 前記プラズマ処理は、RFプラズマ、或いは、マイクロ波プラズマであることを特徴とする請求項1〜5のいずれかに記載の正極の形成方法。
Applications Claiming Priority (2)
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TW097138181A TWI365562B (en) | 2008-10-03 | 2008-10-03 | Positive electrode and method for manufacturing the same and lithium battery utilizing the same |
TW097138181 | 2008-10-03 |
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JP2010092835A JP2010092835A (ja) | 2010-04-22 |
JP5269692B2 true JP5269692B2 (ja) | 2013-08-21 |
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US (2) | US8178240B2 (ja) |
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TW (1) | TWI365562B (ja) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11152601B2 (en) | 2017-07-26 | 2021-10-19 | Lg Chem, Ltd. | Method for manufacturing lithium electrode |
US11430977B2 (en) | 2017-10-16 | 2022-08-30 | Lg Energy Solution, Ltd. | Lithium electrode and lithium secondary battery comprising same |
US11942629B2 (en) | 2019-01-11 | 2024-03-26 | Lg Energy Solution, Ltd. | Lithium electrode and lithium secondary battery comprising same |
Families Citing this family (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2009084966A1 (en) * | 2007-12-28 | 2009-07-09 | Universitetet I Oslo | Formation of a lithium comprising structure on a substrate by ald |
US20110287189A1 (en) * | 2010-05-12 | 2011-11-24 | Enerize Corporation | Method of the electrode production |
TWI418076B (zh) * | 2010-05-24 | 2013-12-01 | Hon Hai Prec Ind Co Ltd | 鋰離子動力電池 |
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TWI453971B (zh) | 2011-02-22 | 2014-09-21 | Univ Nat Taiwan Science Tech | 鋰電池及其製造方法 |
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- 2009-05-12 JP JP2009115433A patent/JP5269692B2/ja active Active
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US11152601B2 (en) | 2017-07-26 | 2021-10-19 | Lg Chem, Ltd. | Method for manufacturing lithium electrode |
US11430977B2 (en) | 2017-10-16 | 2022-08-30 | Lg Energy Solution, Ltd. | Lithium electrode and lithium secondary battery comprising same |
US11942629B2 (en) | 2019-01-11 | 2024-03-26 | Lg Energy Solution, Ltd. | Lithium electrode and lithium secondary battery comprising same |
Also Published As
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JP2010092835A (ja) | 2010-04-22 |
TW201015767A (en) | 2010-04-16 |
TWI365562B (en) | 2012-06-01 |
US20120129051A1 (en) | 2012-05-24 |
US8178240B2 (en) | 2012-05-15 |
US20100086851A1 (en) | 2010-04-08 |
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