WO2015137728A1 - Materiau d'electrode active contenant de l'oxyde de titane reduit et dispositif electrochimique utilisant un tel materiau - Google Patents

Materiau d'electrode active contenant de l'oxyde de titane reduit et dispositif electrochimique utilisant un tel materiau Download PDF

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WO2015137728A1
WO2015137728A1 PCT/KR2015/002366 KR2015002366W WO2015137728A1 WO 2015137728 A1 WO2015137728 A1 WO 2015137728A1 KR 2015002366 W KR2015002366 W KR 2015002366W WO 2015137728 A1 WO2015137728 A1 WO 2015137728A1
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active material
electrode active
lithium
tio
positive electrode
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PCT/KR2015/002366
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English (en)
Korean (ko)
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정연욱
이동훈
박동규
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경북대학교 산학협력단
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Publication of WO2015137728A1 publication Critical patent/WO2015137728A1/fr

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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • 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

Definitions

  • the present invention provides an electrode active material containing a lithium composite oxide capable of inserting and releasing lithium and TiO x (1 ⁇ x ⁇ 2); An electrode containing the electrode active material; And it relates to an electrochemical device containing the electrode active material in the positive electrode.
  • the lithium secondary battery commercially available is lithium-cobalt-based metal oxide as a positive electrode active material, carbon is used as a negative electrode active material.
  • the lithium-cobalt-based metal oxides are relatively easy to synthesize, and have excellent stability and cycle characteristics, but are limited in application to high capacity technology of batteries.
  • lithium-manganese-based metal oxides Due to these problems, recently, lithium-manganese-based metal oxides, lithium-nickel-based metal oxides, and the like have attracted attention as positive electrode active materials.
  • lithium-manganese-based metal oxides having a layered structure have advantages over lithium-cobalt-based metal oxides in terms of capacity but are known to have poor cycle characteristics due to unstable structure.
  • spinel lithium-manganese-based metal oxides have excellent thermal stability, but have a disadvantage in that they are lower than lithium-cobalt-based metal oxides in terms of capacity.
  • lithium-nickel-based metal oxides may exhibit high capacity, cycle characteristics are not good, and manufacturing methods have complicated problems.
  • the present inventors have made intensive efforts to improve the performance of the positive electrode active material, and confirmed that the performance of the positive electrode active material is improved when TiO x (1 ⁇ x ⁇ 2) is added or coated on the positive electrode active material, thereby completing the present invention.
  • An object of the present invention is to provide a method for reforming an electrode active material that can improve the output and cycle characteristics by increasing the electronic conductivity of the electrode active material of an electrochemical device such as a lithium secondary battery.
  • a first aspect of the present invention provides an electrode active material containing a lithium composite oxide capable of inserting and releasing lithium and TiO x (1 ⁇ x ⁇ 2).
  • the second aspect of the present invention provides an electrode containing the electrode active material, the conductive agent and the binder according to the first aspect of the present invention.
  • a third aspect of the invention provides an electrochemical device comprising an anode, a cathode and an electrolyte, wherein the cathode contains an electrode active material according to the first aspect of the invention.
  • the lithium secondary battery is a battery that generates electricity while lithium ions existing in an ionic state move from the positive electrode to the negative electrode when discharged, and move from the negative electrode to the positive electrode when charged.
  • the performance of a lithium secondary battery depends on the lithium ion activation ability of the positive electrode material and the presence of sufficient space to insert lithium ions in the negative electrode material. In particular, since lithium is included in the positive electrode active material, the positive electrode active material substantially influences the performance of the lithium secondary battery.
  • the positive electrode active material is generally composed of a transition metal oxide, since a change in the number of oxides to satisfy the charge neutral state is essential when lithium is de-inserted. Characteristics required for the positive electrode active material, high operating voltage, small polarization during charging and discharging, high capacity and efficiency, life characteristics, stability with the electrolyte should be considered.
  • TiO 2 is an insulator.
  • TiO x (1 ⁇ x ⁇ 2) in which some or all of TiO 2 was reduced has TiO x (1 ⁇ x ⁇ 2) added to a lithium compound oxide capable of inserting and releasing lithium, taking advantage of its extremely high electrical conductivity.
  • the heat-treated electrode active material for the positive electrode of the lithium secondary battery not only the output and cycle characteristics were improved, but also the high output characteristics were found to be good.
  • the present invention is based on this.
  • TiO x (1 ⁇ x ⁇ 2) can be prepared by reducing some or all of TiO 2 in a reducing atmosphere such as hydrogen gas containing atmosphere.
  • the electrode active material according to the present invention may be prepared by mixing lithium compound oxide capable of inserting and releasing lithium and TiO x (1 ⁇ x ⁇ 2), followed by drying and heat treatment.
  • the heat treatment temperature is preferably 100 °C to 500 °C.
  • the reduced titanium oxide (TiO x , 1 ⁇ x ⁇ 2) may be in the form of a homogeneous mixture with the lithium composite oxide, or may be in the form of coating lithium composite oxide particles.
  • the lithium composite oxide is LiCoO 2 , LiNiO 2 , Li 1 + x Mn 2-x O 4 (0 ⁇ x ⁇ 0.33), Li 2 CuO 2 , LiV 3 O 8 , LiFe 3 O 4 , LiNi 1-x M x O 2 (M is Co, Mn, Al, Cu, Fe, Mg, B or Ga; 0.01 ⁇ x ⁇ 0.3), LiMn 2-x M x O 2 (M is Co, Ni, Fe, Cr, Zn or Ta; 0.01 ⁇ x ⁇ 0.1), Li 2 Mn 3 MO 8 (M is Fe, Co, Ni, Cu, or Zn), Li (Ni 1-xy Co x M y ) O 2 (0 ⁇ x ⁇ 0.33, 0 ⁇ y ⁇ 0.33, M may be Mn, Al, Mg or Fe) or mixtures thereof.
  • the reduced titanium oxide is preferably contained in 0.1 to 10 parts by weight, preferably 5 to 10 parts by weight with respect to 100 parts by weight of the electrode active material. If it is less than 0.1% by weight, the effect of the reduced titanium oxide is insignificant, and if it exceeds 10% by weight, there is a problem of excessively coating the lithium composite oxide.
  • the size of the titanium oxide (TiO x , 1 ⁇ x ⁇ 2) particles is preferably 1 ⁇ m or less.
  • the electrode according to the invention contains the electrode active material, the conductive agent and the binder according to the invention.
  • Non-limiting examples of the conductive agent include acetylene black or carbon blacks.
  • the content of the conductive agent used in the electrode is preferably 0.5 to 10% by weight for the positive electrode, 10% by weight or less for the negative electrode.
  • Non-limiting examples of binders used in the present invention include polytetrafluoroethylene, polyvinylidene fluoride, polyvinyl fluoride, polyacrylonitrile, nitrile rubber, polybutadiene, polystyrene, styrene butadiene rubber, polysulfide rubber, butyl rubber, It is preferable to select at least 1 type from the group which consists of hydrogenated styrene butadiene rubber, nitro cellulose, and carboxymethyl cellulose.
  • the content of the binder is preferably 0.1 to 15% by weight.
  • the electrochemical device according to the present invention includes a positive electrode, a negative electrode and an electrolyte containing the electrode active material according to the present invention.
  • the electrode active material according to the present invention exhibits its effects well in a lithium secondary battery among electrochemical devices.
  • a lithium secondary battery includes a positive electrode capable of absorbing and releasing lithium ions, a negative electrode capable of absorbing and releasing lithium ions, a nonaqueous electrolyte, and a separator.
  • the positive electrode may be configured in a form in which the positive electrode active material according to the present invention is bound to a positive electrode current collector, that is, a foil manufactured by aluminum, nickel, or a combination thereof.
  • the content of the cathode active material is preferably 80 to 99% by weight.
  • the negative electrode active material for constituting the negative electrode is lithium metal or lithium adsorption such as lithium alloy and carbon, petroleum coke, activated carbon, graphite, or various other carbons.
  • the substance can be used as the main component.
  • the negative electrode is configured in a form in which the negative electrode active material is bound to a negative electrode current collector, that is, a foil manufactured by copper, gold, nickel, or a copper alloy or a combination thereof.
  • the content of the negative electrode active material is preferably 80 to 99% by weight.
  • the separator is a polyethylene (polyethylene), a polypropylene (polypropylene) having a microporous structure, or a multilayer film produced by a combination of these films, or polyvinylidene fluoride (polyvinylidene fluoride), polyethylene oxide (polyethylene oxide) And polymer films for solid polymer electrolytes or gel polymer electrolytes such as polyacrylonitrile or polyvinylidene fluoride hexafluoropropylene copolymers.
  • the electrolyte is A + B - and may be a salt of such a structure,
  • a + is Li +, Na +,, and comprising an alkali metal cation or an ion composed of a combination thereof, such as K + B - is PF 6 - , BF 4 -, Cl -, Br -, I -, ClO 4 -, ASF 6 -, CH 3 CO 2 -, CF 3 SO 3 -, N (CF 3 SO 2) 2 -, C (CF 2 SO 2 ) 3 - and means a salt containing the same anion, ion consisting of a combination thereof.
  • lithium salt examples include propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC) and dipropyl carbonate (dipropyl).
  • carbonate, DPC dimethyl sulfoxide, acetonitrile, dimethoxyethane, diethoxyethane, tetrahydrofuran, N-methyl-2-pyrrolidone ( N-methyl-2-pyrrolidone (NMP), ethyl methyl carbonate (ethyl methyl carbonate, EMC), gamma butyrolactone ( ⁇ -butyrolactone) or dissolved in an organic solvent consisting of a mixture thereof is dissociated.
  • PC propylene carbonate
  • EC ethylene carbonate
  • DEC diethyl carbonate
  • DMC dimethyl carbonate
  • dipropyl carbonate dipropyl
  • carbonate, DPC dimethyl sulfoxide
  • acetonitrile dimethoxye
  • Non-limiting examples of the method for producing an electrochemical device according to the present invention include a) i) electrode active material particles; ii) conductive particles; And iii) preparing a slurry in which the binder is dispersed in a solvent; b) coating the slurry on a current collector, drying and pressing to prepare an electrode; And c) assembling an electrochemical device having the electrode and injecting a nonaqueous electrolyte.
  • the solvent used in the slurry is not particularly limited, and in general, N-methyl-2-pyrrolidone (NMP) may be used for both the positive electrode and the negative electrode, and distilled water may be used for the aqueous negative electrode.
  • NMP N-methyl-2-pyrrolidone
  • the conductive particles are arranged to connect the spaced apart electrode active material particles after electrode coating if the electrode is well dispersed by mixing during electrode production.
  • the electrode may be heat treated to evaporate the solvent.
  • the electrode active material according to the present invention When the electrode active material according to the present invention is used as a positive electrode active material of a lithium secondary battery, improved output and excellent cycle characteristics can be imparted to the lithium secondary battery.
  • FIG. 1 shows a scanning electron micrograph of a positive electrode active material according to Example 1.
  • FIG. 2 shows a scanning electron micrograph of the positive electrode active material according to Example 2.
  • FIG. 3 shows the results of XRD analysis of the positive electrode active materials according to Examples 1 and 2.
  • FIG. 4 shows the results of evaluation of output characteristics of a lithium secondary battery according to one embodiment of the present invention.
  • Uncoated composite oxide particles having a composition of LiNi 0.6 Mn 0.2 Co 0.2 O 2 were used as comparative examples.
  • a coin cell containing the positive electrode active material prepared in Example 1 was prepared.
  • the positive electrode active material prepared in Example 1 polyvinylidene fluoride (PVDF) as a binder, and carbon black (manufacturer: Timcal) as a conductive agent are mixed at a weight ratio of 95: 2: 3, and coated on an aluminum current collector. After that, it was dried and roll pressed to prepare a positive electrode.
  • a coin cell including a lithium metal and an electrolyte (1M LiPF 6 EC / DMC) was prepared as the positive electrode and the negative electrode prepared as described above.
  • the particle surface was observed using a scanning electron microscope (manufactured by JEOL), and the results are shown in FIGS. 1 and 2, respectively. It can be seen from the figure that the TiO x (1 ⁇ x ⁇ 2) particles are partially coated on the surface of the lithium composite oxide particles.
  • XRD analysis (manufacturer: PANalytical, model name: X'Pert pro MPD) of each of the cathode active materials prepared in Examples 1 and 2 and Comparative Example 1 was performed, and the results are shown in FIG. 3.
  • the X-ray diffraction analysis test was carried out using Cu-K ⁇ rays under the condition that the sampling width is 0.01 °, scan rate 4 ° / min in the 2 ⁇ value range from 10 ° to 80 °.
  • Preparation Example 1 including a positive electrode active material coated with 3% by weight of TiO x (1 ⁇ x ⁇ 2)
  • Preparation Example 2 8% by weight of TiO x (1 ⁇ x on the surface
  • the coin cell of the positive electrode active material coated with ⁇ 2) was compared to the coin cell of Preparation Example 3 (including the positive electrode active material not coated with TiO x (1 ⁇ x ⁇ 2) on the surface), and the capacity retention rate and C-rate were higher. It was confirmed that other output characteristics improved by or equal to or more.
  • the coin cells prepared in Preparation Examples 1 to 3 were charged and discharged at a rate of C / 5 once in the range of 3.0 V to 4.5 V, respectively, and then charged and discharged at a rate of 1 C to improve cycle characteristics. It evaluated, and the result is shown in FIG.
  • the coin cell of Preparation Example 2 (including the positive electrode active material coated with 8 wt% of TiO x (1 ⁇ x ⁇ 2)) was prepared in Preparation Example 1 (3 wt% of TiO x (on the surface) It can be seen that the life characteristics are improved compared to the coin cells of the positive electrode active material coated with 1 ⁇ x ⁇ 2) and Preparation Example 3 (including the positive electrode active material not coated with TiO x (1 ⁇ x ⁇ 2) on the surface). there was.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

La présente invention concerne un matériau d'électrode active contenant du TiOx (1≤x< 2) et un complexe d'oxyde de lithium dans lequel du lithium peut être intercalé ou libéré. Lorsque le matériau d'électrode active est utilisé en tant que matériau actif de cathode pour une batterie secondaire au lithium, d'excellentes caractéristiques de cycle et de sortie améliorée peuvent être procurées à la batterie secondaire au lithium.
PCT/KR2015/002366 2014-03-11 2015-03-11 Materiau d'electrode active contenant de l'oxyde de titane reduit et dispositif electrochimique utilisant un tel materiau WO2015137728A1 (fr)

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KR10-2014-0028410 2014-03-11
KR1020140028410A KR20150106203A (ko) 2014-03-11 2014-03-11 환원된 티타늄 산화물 함유 전극 활물질 및 이를 이용한 전기화학소자

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107017385A (zh) * 2016-01-28 2017-08-04 株式会社Lg化学 阳极活性物质、其制造方法以及锂二次电池

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102659587B1 (ko) * 2020-02-28 2024-04-22 숙명여자대학교산학협력단 산소결핍 밸브 금속 산화물의 제조방법 및 산소결핍 밸브 금속 산화물

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09330719A (ja) * 1996-06-11 1997-12-22 Sanyo Electric Co Ltd リチウム二次電池
JP2003142101A (ja) * 2001-10-31 2003-05-16 Nec Corp 二次電池用正極およびそれを用いた二次電池
US20090117463A1 (en) * 2007-11-02 2009-05-07 Hideharu Takezawa Lithium ion secondary battery
KR20110027112A (ko) * 2009-09-09 2011-03-16 한국과학기술연구원 리튬전지용 양극 활물질의 제조방법
KR101264337B1 (ko) * 2010-08-13 2013-05-14 삼성에스디아이 주식회사 양극 활물질 및 이를 이용한 리튬 전지

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09330719A (ja) * 1996-06-11 1997-12-22 Sanyo Electric Co Ltd リチウム二次電池
JP2003142101A (ja) * 2001-10-31 2003-05-16 Nec Corp 二次電池用正極およびそれを用いた二次電池
US20090117463A1 (en) * 2007-11-02 2009-05-07 Hideharu Takezawa Lithium ion secondary battery
KR20110027112A (ko) * 2009-09-09 2011-03-16 한국과학기술연구원 리튬전지용 양극 활물질의 제조방법
KR101264337B1 (ko) * 2010-08-13 2013-05-14 삼성에스디아이 주식회사 양극 활물질 및 이를 이용한 리튬 전지

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107017385A (zh) * 2016-01-28 2017-08-04 株式会社Lg化学 阳极活性物质、其制造方法以及锂二次电池

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