WO2010084701A1 - 非水系二次電池用活物質および非水系二次電池 - Google Patents

非水系二次電池用活物質および非水系二次電池 Download PDF

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WO2010084701A1
WO2010084701A1 PCT/JP2010/000049 JP2010000049W WO2010084701A1 WO 2010084701 A1 WO2010084701 A1 WO 2010084701A1 JP 2010000049 W JP2010000049 W JP 2010000049W WO 2010084701 A1 WO2010084701 A1 WO 2010084701A1
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active material
alkali metal
secondary battery
aqueous secondary
transition metal
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French (fr)
Japanese (ja)
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丹羽淳一
村瀬仁俊
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Toyota Industries Corp
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Toyota Industries Corp
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Priority to US13/145,056 priority Critical patent/US20110285353A1/en
Priority to KR1020117015249A priority patent/KR101354085B1/ko
Priority to EP10733309A priority patent/EP2383821A4/en
Priority to CN201080003846.0A priority patent/CN102272989A/zh
Publication of WO2010084701A1 publication Critical patent/WO2010084701A1/ja
Anticipated expiration legal-status Critical
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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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/582—Halogenides
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/388—Halogens
    • 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
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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 relates to non-aqueous secondary batteries such as lithium ion secondary batteries, and more particularly to an active material for non-aqueous secondary batteries.
  • a lithium ion secondary battery has an active material capable of inserting and removing lithium (Li) on a positive electrode and a negative electrode, respectively. Then, it operates by moving Li ions in the electrolyte provided between both electrodes.
  • Patent Document 1 discloses a positive electrode active material represented by Li a M 2 O 4-b F b containing a transition metal (M). Also, recently, as disclosed in Patent Document 2 and Patent Document 3, a secondary battery using a transition metal halide such as FeF 3 as a positive electrode active material is also attracting attention.
  • Patent Document 2 and Patent Document 3 as a voltage range of charge and discharge, charge and discharge is performed only in a voltage range (a range of 4.5 V to 2 V in the case of a lithium ion secondary battery) which does not advance reaction to the conversion region I did not let In charge and discharge in this voltage range, FeF 3 inserts and desorbs Li, and FeF 3 + yLi ⁇ Li y FeF 3 and Li y FeF 3 ⁇ FeF 3 + yLi (all 0 ⁇ y ⁇ 1) Reaction is performed, and the bond between Fe and F is maintained. That is, reduction from Fe 3+ to Fe 2+ is performed at the time of discharge, and oxidation from Fe 2+ to Fe 3+ is performed at the time of charge.
  • a voltage range a range of 4.5 V to 2 V in the case of a lithium ion secondary battery
  • FeF 3 is electrolytically reduced from Fe 3 + to Fe 0 by decomposition when it is reacted to the conversion region, significant increase in capacity of the secondary battery as will be described later is expected.
  • FeF 3 is easily decomposed and the decomposed FeF 3 is reversibly regenerated, and from the viewpoint of battery performance, the reaction to the conversion region has rather been avoided.
  • FeF 3 exhibits high capacity by using up to the conversion region, it does not contain lithium in the active material, so it is necessary to use metallic lithium for the counter electrode or to dope lithium in the active material in advance. .
  • An object of the present invention is to provide a non-aqueous secondary battery active material comprising a combination of novel materials in view of the above problems. Furthermore, it aims at providing the non-aqueous secondary battery which used this active material as a positive electrode active material.
  • the present inventors have conceived of combining LiF and Fe present in the conversion region, that is, an alkali metal salt and a transition metal, to constitute a novel non-aqueous secondary battery active material. So far, there has been no finding that a combination of a salt and a metal can provide an active material of a non-aqueous secondary battery. However, when the mixture of the alkali metal salt and the transition metal is brought to a high potential state, the transition metal is oxidized (electrons are taken), anion exchange occurs, and a compound is formed from the mixture. Furthermore, it was newly found that the alkali metal ions (cations) contained in the alkali metal salt move to extract electricity from the produced compound.
  • the active material for non-aqueous secondary batteries of the present invention comprises a mixture of an alkali metal salt and a transition metal, and the alkali metal is removed from the compound formed by the reaction of the alkali metal salt with the transition metal by charge and discharge. They are characterized in that they are separated and subjected to reversible oxidation-reduction to regenerate the alkali metal salt and the transition metal from the compound into which the alkali metal is inserted.
  • the non-aqueous secondary battery of the present invention comprises a positive electrode comprising the positive electrode active material comprising the active material for non-aqueous secondary battery of the present invention, and a negative electrode active material comprising a material capable of inserting and removing alkali metal. And a negative electrode.
  • FeF 3 is a perovskite type fluoride and has cation vacancies in its structure. Up to 1 mol of an alkali metal ion such as Li + can be inserted in 1 mol of FeF 3 in the cation vacancies, resulting in LiFeF 3 . At this time, the theoretical capacity exceeds 230 mAh / g. Furthermore, LiFeF 3 reacts with Li ions and is eventually decomposed into LiF and Fe. That is, the reaction proceeds to the conversion region, and at this time theoretically shows a capacity of 700 mAh / g or more.
  • This reaction is considered to be the same even when 'Fe' is another transition metal element, 'F' is a transition metal element and another element having a perovskite structure, and 'Li' is another alkali metal element.
  • the structure is not limited to the perovskite structure, but may be a spinel structure, as long as it is a structure that can insert and release alkali metal ions. Therefore, by using the active material for a non-aqueous secondary battery of the present invention, which is a mixture of an alkali metal salt and a transition metal, the capacity of the non-aqueous secondary battery can be increased.
  • the active material for non-aqueous secondary batteries of this invention contains the alkali metal which contributes to charging / discharging
  • the active material used for a counter electrode is not limited.
  • safety is improved because it is not necessary to use an electrode containing metallic lithium.
  • the crystal structure of the perovskite type fluoride FeF 3 is shown. It is an X-ray diffraction pattern of the mixed powder which consists of LiF powder and Fe powder.
  • the charge-discharge curve of the lithium ion secondary battery which made the active material for non-aqueous secondary batteries of this invention a positive electrode active material is shown.
  • the active material for non-aqueous secondary batteries of the present invention comprises a mixture of an alkali metal salt and a transition metal.
  • alkali metals are six elements of lithium (Li), sodium (Na), potassium (K), rubidium (Ru), cesium (Cs), and francium (Fr).
  • Li and Na are preferable, and exhibit high capacity and reversible charge and discharge characteristics.
  • the active material of the present invention forms a structure capable of inserting and removing alkali metal ions by charge and discharge.
  • a perovskite structure, a spinel structure and the like can be mentioned.
  • the element X bonded to the transition metal element in the above range is preferably at least one selected from elements of Groups 15 to 17 of the periodic table, and particularly preferably halogen (fluorine (F), chlorine (Cl), bromine (Br) And iodine (I), astatine (At)), oxygen, sulfur and nitrogen, and one or more of these may be used.
  • halogen fluorine (F), chlorine (Cl), bromine (Br) And iodine (I), astatine (At)
  • oxygen, sulfur and nitrogen and one or more of these may be used.
  • LiF, NaF, Li 2 O , Na 2 O, Li 2 S, Na 2 S, Li 3 N and the like two or more may be used one of these singly You may mix and use.
  • the alkali metal salt may be represented by AX.
  • X may be any element having an anion radius that fits the tolerance factor in which the perovskite structure can stably exist.
  • Specific examples of X include a halogen element, an oxygen element, a sulfur element, and a nitrogen element, and one or more of them is preferable. That is, for the alkali metal salt AX, in addition to halides such as fluoride and chloride, oxides can be suitably used. Specifically, LiF, NaF, etc. may be mentioned, and one of them may be used alone, or two or more may be mixed and used.
  • transition metal there is no particular limitation on the transition metal, and for example, one or more of the first transition elements (3d transition elements: Sc to Zn), especially iron (Fe), nickel (Ni), manganese (Mn), cobalt (Co), may be mentioned.
  • the first transition elements 3d transition elements: Sc to Zn
  • a transition metal taking trivalent Specifically, Fe, Ni, Mn, Co and the like can be mentioned.
  • a transition metal one of these may be used alone, or two or more may be mixed and used.
  • LiF and Fe, LiF and Ni, LiF and Mn, LiF and Co, etc. may be mentioned as a particularly preferred combination of alkali metal salt and transition metal among the above-mentioned alkali metal salts and transition metals.
  • the active material of the present invention is a mixture of an alkali metal salt and a transition metal.
  • the alkali metal salt and the transition metal are preferably in powder form. If it is a powder of a transition metal, a powder obtained by pulverizing an ingot or pulverizing a molten metal can be used. For example, atomized powder is commercially available and easily available.
  • the alkali metal salt powder is also obtained by pulverization or the like, but it is also possible to convert the precursor by heating the solution containing the alkali metal salt precursor or the like to obtain a fine powder.
  • the average particle diameter of the alkali metal salt powder and the transition metal powder is not particularly limited, but the reaction between the alkali metal salt and the transition metal can be expected to occur in fine domains, so 10 ⁇ m or less is preferable.
  • the mixed powder obtained by milling the alkali metal salt powder and the transition metal powder is such that the particles are uniformly mixed and the particles are further finely divided by the milling, so the decomposition reaction to the conversion region and the conversion region As a result, the formation of a compound consisting of the anion of the alkali metal salt and the transition metal easily occurs reversibly.
  • the reversible reaction is better as the average particle size of the mixed powder is smaller.
  • the milling speed may be 100 rpm or more. If less than 100 rpm, the powder is difficult to be finely divided even if milling is performed for a long time.
  • the milling time may be 10 to 24 hours. If it is less than 10 hours, the refining effect is scarce, and even if milling is performed for more than 24 hours, there is no significant improvement in the refining effect.
  • the compounding ratio of the active material of the present invention may be determined according to the type of the compound produced by charge and discharge, and the molar ratio of the transition metal to the alkali metal salt may be 1: 1 to 1: 3. If the compound generated by charge and discharge has a perovskite structure (ABX 3 ), the transition will theoretically be 3AX + B ⁇ BX 3 + 3A due to the insertion and desorption of the electrolyte ion (alkali metal ion: A + ). This is because it is presumed that the metal B: alkali metal salt AX is preferably about 1: 3 in molar ratio.
  • the electrode comprises the active material of the present invention, a conductive support, and a binder for binding the active material and the conductive support.
  • the active material is a mixture of the above-mentioned alkali metal salt and transition metal.
  • the alkali metal salt and the transition metal can be variously combined as described above, one type can be used alone, or two or more types can be mixed and used.
  • the conductive additive a material generally used in the electrode of the non-aqueous secondary battery may be used.
  • a conductive carbon material such as carbon black, acetylene black, ketjen black, carbon fiber and the like. It is good to use 1 type of these individually or in mixture of 2 or more types.
  • the conductive support is preferably milled together with the above-mentioned active material to further improve the conductivity.
  • the binding agent is not particularly limited, and any known binding agent may be used.
  • a resin which does not decompose even at high potential such as a fluorine-containing resin such as polytetrafluoroethylene or polyvinylidene fluoride can be used.
  • the active material of the present invention is generally used in a state of being pressure-bonded to a current collector as an active material layer in an electrode.
  • a current collector metal mesh or metal foil can be used. If the active material of the present invention is used for the positive electrode, it is preferable to use a current collector such as aluminum or aluminum alloy which is difficult to dissolve at high potential, and for the negative electrode a current collector such as copper.
  • the manufacturing method of an electrode there is no limitation in particular in the manufacturing method of an electrode, and it may follow the manufacturing method of the electrode for non-aqueous secondary batteries generally implemented.
  • the conductive auxiliary material and the binding agent are mixed with the active material, and an appropriate amount of organic solvent is added as necessary to obtain a paste-like electrode mixture.
  • the electrode mixture is applied to the surface of a current collector, dried, and pressed if necessary by pressing or the like.
  • the manufactured electrode is a sheet-like electrode.
  • the sheet-like electrode may be cut into dimensions according to the specifications of the non-aqueous secondary battery to be produced.
  • the active material of the present invention can be used as an active material of a positive electrode of a non-aqueous secondary battery or as an active material of a negative electrode.
  • the active material of the present invention contains an alkali metal that becomes an electrolyte ion in a battery reaction, so the active material used for the counter electrode is not limited.
  • a lithium-containing oxide such as LiCoO 2 or Li 2 MnO 3 or a lithium-free compound such as MoS or sulfur is used.
  • the non-aqueous secondary battery may be configured by using an electrode serving as an active material as a positive electrode. The case where the active material of the present invention is used as a positive electrode active material of a non-aqueous secondary battery will be described below.
  • Non-aqueous secondary battery of the present invention comprises a positive electrode comprising the positive electrode active material comprising the active material of the present invention, and a negative electrode comprising the negative electrode active material comprising a material capable of inserting and removing alkali metal.
  • the configuration and manufacturing method of the positive electrode are as described above.
  • the negative electrode may be, for example, an alkali metal such as Li or Na, an alloy of an alkali metal, a carbon material such as graphite, coke, hard carbon, a metal such as tin forming an alloy with the alkali metal, or a silicon or a compound containing them. It is preferable that it is an electrode used as a substance.
  • the negative electrode may be manufactured by a general manufacturing method according to the above-described method of manufacturing an electrode.
  • the non-aqueous secondary battery using the electrode of the present invention includes a separator and a non-aqueous electrolyte in addition to the positive electrode and the negative electrode, as well as the general secondary battery, in addition to the positive electrode and the negative electrode.
  • the separator separates the positive electrode and the negative electrode and holds the electrolytic solution, and a thin microporous film such as polyethylene or polypropylene can be used.
  • the non-aqueous electrolytic solution is obtained by dissolving an alkali metal salt which is an electrolyte in an organic solvent, and as the organic solvent, an aprotic organic solvent such as ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, diethyl carbonate, ethyl methyl carbonate And mixtures of two or more of these, such as imidazole-based ionic liquids.
  • an alkali metal salt which is an electrolyte in an organic solvent
  • an aprotic organic solvent such as ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, diethyl carbonate, ethyl methyl carbonate And mixtures of two or more of these, such as imidazole-based ionic liquids.
  • Alkali metal salts soluble in organic solvents such as NaPF 6 , NaBF 4 , NaAsF 6 and the like can be used.
  • a polymer such as polyethylene oxide (PEO) containing a supporting salt instead of a non-aqueous electrolytic solution, a gel electrolyte in which the electrolytic solution is confined with PVdF, an inorganic compound having lithium ion conductivity including Li 2 S, glass And other solid electrolytes can also be used.
  • the shape of the non-aqueous secondary battery is not particularly limited, and various shapes such as a cylindrical shape, a laminated shape, and a coin shape can be adopted.
  • the separator is interposed between the positive electrode and the negative electrode to form an electrode body, and the distance from the positive electrode current collector and the negative electrode current collector to the positive electrode terminal and the negative electrode terminal leading to the outside is for current collection After connection using a lead or the like, the electrode body is sealed in a battery case together with the non-aqueous electrolyte to form a battery.
  • BX 3 is generated from the alkali metal salt (AX) and the transition metal (B) through Ay BX 3 (0 ⁇ y ⁇ 1) by charging, and is discharged from BX 3 by discharging.
  • a reversible oxidation-reduction is carried out to regenerate AX and B via A y BX 3 (0 ⁇ y ⁇ 1).
  • the active material of the present invention is in the conversion region consisting of an alkali metal salt and a transition metal, it is desirable to sweep the discharge end voltage to a lower level than before.
  • charge and discharge are usually performed at a voltage range of 4.5 V to 2.0 V, but the active material of the present invention is used as a positive electrode active material
  • the discharge end voltage may be 4.5 V to 1.5 V.
  • non-aqueous secondary battery active material and the non-aqueous secondary battery of the present invention have been described above, but the present invention is not limited to the above-described embodiments. In the range which does not deviate from the summary of the present invention, it can carry out with various forms which gave change, improvement, etc. which a person skilled in the art can make.
  • the present invention will be specifically described by way of examples of the non-aqueous secondary battery active material and the non-aqueous secondary battery of the present invention.
  • LiF powder Soekawa Chemical Co., Ltd., average particle size: 3 ⁇ m
  • commercially available Fe powder average particle size: 3 ⁇ m
  • the mixing was performed at a milling speed of 600 rpm and a milling time of 24 hours.
  • the X-ray diffraction analysis (CuK ⁇ ) of the obtained mixed powder (active material # 01) was performed. The results are shown in FIG. In addition, in FIG.
  • the X-ray-diffraction pattern of the mixed powder (active material # 00) of the same mixture ratio obtained by hand stirring for several minutes is collectively shown. Since the diffraction peak of the active material # 01 is broader than that of the active material # 00, it was found that the particles become finer by milling. In addition, in each of # 01 and # 00, respective diffraction peaks of LiF and Fe were obtained, and in # 01, it was found that LiF was not reacted with Fe by milling.
  • Electrode for lithium ion secondary battery An electrode was produced using active material # 01. Mix active material # 01 and acetylene black (AB) as conductive aid, and further mix polytetrafluoroethylene (PTFE) as a binder for binding active material and conductive aid, and use appropriate amount of solvent (Ethanol) was added and sufficiently kneaded to prepare a paste-like electrode mixture.
  • the compounding ratio of the active material # 01, AB and PTFE was 1: 1.66: 1.33 by mass ratio.
  • this electrode mixture was applied to both sides of a current collector (aluminium mesh, thickness: 20 ⁇ m), dried, and pressure-bonded to obtain a sheet-like electrode.
  • a lithium ion secondary battery was manufactured using the electrode manufactured according to the above procedure as a positive electrode.
  • the negative electrode to be opposed to the positive electrode was metal lithium (500 ⁇ m in thickness).
  • the positive electrode was cut into a diameter of 13 mm, and the negative electrode was cut into a diameter of 15 mm, and a separator (glass filter made by Hoechst Celanese, celgard 2400) was sandwiched between the two to make an electrode battery.
  • the electrode battery was housed in a battery case (CR2032 coin cell manufactured by Takasen Co., Ltd.).
  • the battery case, ethylene carbonate and diethyl carbonate 1 LiPF 6 in a solvent mixture was poured a non-aqueous electrolyte at a concentration of 1M in 1 (volume ratio). The battery case was sealed to obtain a lithium ion secondary battery # 11.
  • the lithium ion secondary battery # 11 was found to exhibit reversible charge / discharge characteristics at a high capacity (the capacity at the fifth cycle is 225 mAh / g). That is, an active material composed of a mixture of LiF, which is an alkali metal salt, and Fe, which is a transition metal, exhibits reversible charge and discharge characteristics, and a non-aqueous secondary battery using the active material has high capacity. all right. Since the capacity of a general lithium ion secondary battery commercially available is about 150 mAh / g, the # 11 lithium ion secondary battery has a capacity about 1.5 times higher than usual. Moreover, according to the discharge curve of FIG. 3, the slope of the graph largely changed at the voltage bordering around 2.0 V. This suggests that LiFeF 3 began to be decomposed into LiF and Fe at around 2.0 V.

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PCT/JP2010/000049 2009-01-23 2010-01-06 非水系二次電池用活物質および非水系二次電池 Ceased WO2010084701A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US13/145,056 US20110285353A1 (en) 2009-01-23 2010-01-06 Active material for non-aqueous-system secondary battery and non-aqueous-system secondary battery
KR1020117015249A KR101354085B1 (ko) 2009-01-23 2010-01-06 비수계 이차 전지용 활물질, 비수계 이차 전지 및 그의 충방전 방법
EP10733309A EP2383821A4 (en) 2009-01-23 2010-01-06 ACTIVE MATERIAL FOR WATER-FREE SECONDARY BATTERY AND WATER-FREE SECONDARY BATTERY
CN201080003846.0A CN102272989A (zh) 2009-01-23 2010-01-06 非水系二次电池用活性物质及非水系二次电池

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JP2009012860A JP5013217B2 (ja) 2009-01-23 2009-01-23 非水系二次電池用活物質および非水系二次電池

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JP5461463B2 (ja) * 2011-03-15 2014-04-02 三菱重工業株式会社 電極活物質およびこれを備えた二次電池用正極並びに二次電池
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