JP6685542B2 - 多重保護層を含む負極及びこれを含むリチウム二次電池 - Google Patents
多重保護層を含む負極及びこれを含むリチウム二次電池 Download PDFInfo
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- JP6685542B2 JP6685542B2 JP2018544515A JP2018544515A JP6685542B2 JP 6685542 B2 JP6685542 B2 JP 6685542B2 JP 2018544515 A JP2018544515 A JP 2018544515A JP 2018544515 A JP2018544515 A JP 2018544515A JP 6685542 B2 JP6685542 B2 JP 6685542B2
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- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- QKBJDEGZZJWPJA-UHFFFAOYSA-N ethyl propyl carbonate Chemical compound [CH2]COC(=O)OCCC QKBJDEGZZJWPJA-UHFFFAOYSA-N 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229920005570 flexible polymer Polymers 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- SMBGWMJTOOLQHN-UHFFFAOYSA-N lead;sulfuric acid Chemical compound [Pb].OS(O)(=O)=O SMBGWMJTOOLQHN-UHFFFAOYSA-N 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 229920000092 linear low density polyethylene Polymers 0.000 description 1
- 239000004707 linear low-density polyethylene Substances 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNKYTQGIUYNRMY-UHFFFAOYSA-N methoxypropane Chemical compound CCCOC VNKYTQGIUYNRMY-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- KKQAVHGECIBFRQ-UHFFFAOYSA-N methyl propyl carbonate Chemical compound CCCOC(=O)OC KKQAVHGECIBFRQ-UHFFFAOYSA-N 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000131 polyvinylidene Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 238000007764 slot die coating Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000011787 zinc oxide Substances 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
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- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- 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
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- H—ELECTRICITY
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- H01M4/00—Electrodes
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- 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
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/46—Separators, membranes or diaphragms characterised by their combination with electrodes
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- 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
Description
本発明は、リチウム金属層;及び
前記リチウム金属層上に形成された多層構造の保護層;を備え、
前記保護層は、炭素ナノチューブ−イオン伝導性高分子の複合材料を含む第1保護層;及び
炭素ナノチューブ−電気伝導性高分子の複合材料を含む第2保護層;を含むことを特徴とする、リチウム二次電池用負極を提供する。
前記リチウム金属層上に形成された臨時保護金属層;及び
前記臨時保護金属層上に形成された多層構造の保護層;を備え、
前記臨時保護金属は、リチウム金属と合金を形成することができるか、またはリチウム金属に拡散することができるし、
前記保護層は、炭素ナノチューブ−イオン伝導性高分子の複合材料を含む第1保護層;及び
炭素ナノチューブ−電気伝導性高分子の複合材料を含む第2保護層;を含むことを特徴とする、リチウム二次電池用負極を提供する。
前記リチウム金属層110上に形成された多層構造の保護層;を備え、
前記保護層は、炭素ナノチューブ−イオン伝導性高分子の複合材料を含む第1保護層120;及び
炭素ナノチューブ−電気伝導性高分子の複合材料を含む第2保護層130;を含むことを特徴とする、リチウム二次電池用負極100を提供する。
前記リチウム金属層110上に形成された臨時保護金属層140;及び
前記臨時保護金属層140上に形成された多層構造の保護層;を備え、
前記臨時保護金属は、リチウム金属と合金を形成できたり、またはリチウム金属に拡散されることができるし、
前記保護層は、炭素ナノチューブ−イオン伝導性高分子の複合材料を含む第1保護層120;及び
炭素ナノチューブ−電気伝導性高分子の複合材料を含む第2保護層130;を含むことを特徴とする、リチウム二次電池用負極100を提供する。
実施例1〜8。本発明のリチウム二次電池用負極の製造(二重層)
NMP溶液に下記表1の組成の含量でポリアニリン(PANI)単量体及び炭素ナノチューブ(CNT)を溶解させ、超音波分散を利用して均一に分散させた。また、アセトニトリル溶液に下記表1の組成のような含量で炭素ナノチューブ及びポリエチレンオキシド(PEO)が溶解された溶液を超音波分散を利用して均一に混合し、電解液をポリマー重さの2倍の重さで投入した後、2時間撹拌した。前記二つの高分子溶液をリチウム金属表面にスピンコッターを利用して順にコーティングし、この時、水分と大気中の活性気体による影響を最小化するために、工程は常温のドライルームの中で進めた。リチウム金属表面に前記高分子溶液を少量落とした後、2000rpmの速度で10秒間、そして2500rpmの速度で20秒間連続コーティングした。次に、NMPとアセトニトリル溶媒を取り除いて、リチウム金属とその表面に形成される保護膜の接着性を高めるために、110℃の真空オーブンで1〜2分間乾燥させることで2層の保護層を形成した。それぞれの保護層は10μmの厚さで製造された。
前記実施例1〜8の製造方法でPEOの代わりにポリ塩化ビニリデン−ヘキサフルオロプロピレン(PVdF−HFP)共重合体を使用したことを除いて、同一な方法で下記表2の組成によって負極を製造し、保護層を形成した。
前記実施例1〜8の製造方法でCNTとPANIまたはPEOが溶解された溶液の代わりに下記表3に示された混合物を使用したことを除いて、同一に負極を製造して一層の保護層を形成した。
前記実施例1〜8及び比較例1〜7のリチウム二次電池用負極、有機電解液、LiCoO2正極を用いてリチウム金属電池を製造した。正極を製造するためにバインダーとして使用されるポリ塩化ビニリデン(poly(vinylidene fluoride)、PVdF)をN−メチルピロリドンに溶かした後、この混合液に導電材であるSuper−P carbonとLiCoO2を定量して入れて撹拌した。この時、正極活物質、導電材、バインダーの重量比は85:7.5:7.5であった。完全な混合が行われたスラリー溶液をアルミニウム集電体に塗布して乾燥した後、ロールプレスを使ってラミネーション工程を施した。これは活物質/導電材/バインダーの相互結合力を向上させ、電流集電体にこれら物質を効果的に結着させるためである。圧搾工程後、切断過程を経て適当な大きさの電極を製造し、110℃の真空オーブンで24時間以上乾燥させた。負極としては、前記実施例1〜8及び比較例1〜7の保護層が形成されたリチウム金属層をそれぞれ銅ホイルにラミネーションして使用した。分離膜としては、Celgard 3501を使用した。全ての電極の準備は、ドライルームで行われ、電池の製作はアルゴン雰囲気が維持されるグローブボックス内で行われた。
1。表面特性評価
前記実施例1〜8及び比較例1〜7で製造された負極を含むリチウム二次電池の製作後、0.5mAの条件で10回充放電を行った。次いで、リチウムデンドライトの形成を確認するために、電池からリチウム金属(負極)を分離した。
実施例1〜8または比較例1〜7の保護層が形成されたリチウム金属の負極の界面抵抗を測定し、結果を下記表4に示した。
前記実施例2、3及び比較例2で製造された負極を含むリチウム二次電池を0.1Cで3回充放電した後、0.3Cを印加して充放電テストを行い、その結果を図8に示した。
110:リチウム金属層
120:第1保護層
130:第2保護層
140:臨時保護金属層
Claims (7)
- リチウム金属層;及び
前記リチウム金属層上に形成された多層構造の保護層;を備え、
前記保護層は、炭素ナノチューブ−イオン伝導性高分子の複合材料を含む第1保護層;及び
炭素ナノチューブ−電気伝導性高分子の複合材料を含む第2保護層;を含み、
前記炭素ナノチューブ−イオン伝導性高分子の複合材料は、イオン伝導性高分子100重量部に対して炭素ナノチューブ0.5〜20重量部を含み、
前記炭素ナノチューブ−電気伝導性高分子の複合材料は、電気伝導性高分子100重量部に対して炭素ナノチューブ0.5〜20重量部を含むことを特徴とする、リチウム二次電池用負極。 - 前記保護層は、第1保護層と第2保護層が交互に積層された2層以上の層を有することを特徴とする、請求項1に記載のリチウム二次電池用負極。
- 前記第1保護層は、厚さが0.01〜10μmであることを特徴とする、請求項1に記載のリチウム二次電池用負極。
- 前記第2保護層は、厚さが0.01〜10μmであることを特徴とする、請求項1に記載のリチウム二次電池用負極。
- 前記イオン伝導性高分子は、ポリエチレンオキシド、ポリエチレングリコール、ポリプロピレングリコール、ポリプロピレンオキシド、ポリエチレンサクシネート、アジピン酸ポリエチレン、ポリエチレンイミン、ポリエピクロロヒドリン、ポリβ−プロピオラクトン、ポリN−プロピルアジリジン、ポリエチレングリコールジアクリレート、ポリプロピレングリコールジアクリレート、ポリエチレングリコールジメタクリレート及びポリプロピレングリコールジメタクリレートからなる群から選択された一つ以上を含むことを特徴とする、請求項1に記載のリチウム二次電池用負極。
- 前記電気伝導性高分子は、ポリアニリン、ポリエチレンジオキシチオフェン、ポリフェニレンビニレン、ポリアセンチレン、ポリ(p−フェニレン)、ポリチオフェン、ポリ(3−アルキルチオフェン)、ポリ(3−アルコキシチオフェン)、ポリ(クラウンエーテルチオフェン)、ポリピロール、ポリ(ジアルキル−2,2’−ビピリジン)、ポリピリジン、ポリアルキルピリジン、ポリ(2,2’−ビピリジン)、ポリ(ジアルキル−2,2’−ビピリジン)、ポリピリミジン、ポリジヒドロフェナントレン、ポリキノリン、ポリイソキノリン、ポリ(1,2,3−ベンゾチアジアゾル)、ポリ(ベンズイミダゾール)、ポリ(キノキサリン)、ポリ(2,3−ジアリルキノキサリン)、ポリ(1,5−ナフチリジン)、ポリ(1,3−シクロヘキサジエン)、ポリ(アントラキノン)、ポリ(Z−メチルアントラキノン)、ポリ(フェロセン)、ポリ(6,6’−ビキノリン)、ポリフェニレンスルフィド、ポリフェニレンビニレン、ポリインドール、ポリピレン、ポリカルバゾール、ポリアズレン、ポリアゼピン、ポリフルオレン、ポリナフタレン及びポリ3,4−エチレンジオキシチオフェン−ポリスチレンスルホネートからなる群から選択された一つ以上を含むことを特徴とする、請求項1に記載のリチウム二次電池用負極。
- 請求項1〜6のいずれか一項に記載の負極を含む、リチウム二次電池。
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