WO2017094163A1 - Matériau actif d'électrode positive pour une batterie à électrolyte non aqueux, électrode positive pour une batterie à électrolyte non aqueux, batterie à électrolyte non aqueux et bloc de batteries - Google Patents

Matériau actif d'électrode positive pour une batterie à électrolyte non aqueux, électrode positive pour une batterie à électrolyte non aqueux, batterie à électrolyte non aqueux et bloc de batteries Download PDF

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WO2017094163A1
WO2017094163A1 PCT/JP2015/083995 JP2015083995W WO2017094163A1 WO 2017094163 A1 WO2017094163 A1 WO 2017094163A1 JP 2015083995 W JP2015083995 W JP 2015083995W WO 2017094163 A1 WO2017094163 A1 WO 2017094163A1
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active material
positive electrode
nonaqueous electrolyte
electrolyte battery
electrode active
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PCT/JP2015/083995
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English (en)
Japanese (ja)
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泰伸 山下
圭吾 保科
康宏 原田
義之 五十崎
高見　則雄
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株式会社東芝
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Priority to JP2017553569A priority Critical patent/JP6523483B2/ja
Priority to PCT/JP2015/083995 priority patent/WO2017094163A1/fr
Publication of WO2017094163A1 publication Critical patent/WO2017094163A1/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
    • 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
    • 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

  • Embodiments of the present invention relate to a positive electrode active material for a nonaqueous electrolyte battery, a positive electrode for a nonaqueous electrolyte battery, a nonaqueous electrolyte battery, and a battery pack.
  • phosphates such as lithium iron manganese phosphate have been studied.
  • a positive electrode for a non-aqueous electrolyte battery for example, a positive electrode containing lithium iron manganese phosphate / carbon nanocomposite powder and an inorganic binder is known.
  • Lithium iron manganese phosphate has been regarded as a problem of side reaction at a high potential because of its low reaction activity and high reaction potential.
  • lithium iron manganese phosphate and the non-aqueous electrolyte react with charge / discharge, and the reaction product film is formed of iron phosphate. May form on the surface of manganese lithium.
  • the coating formed on the surface of lithium iron manganese phosphate increases the electrical resistance between lithium iron manganese phosphate and the non-aqueous electrolyte, lowers the discharge capacity at a high discharge rate, and shortens the cycle life. May be a factor.
  • the non-aqueous electrolyte battery using lithium iron manganese phosphate as the positive electrode active material tends to have a low discharge capacity at a high discharge rate and a short cycle life.
  • the problem to be solved by the present invention is that, while using phosphate as a positive electrode active material, a decrease in discharge capacity at a high discharge rate hardly occurs, and a positive electrode active material for a non-aqueous electrolyte battery having a long cycle life, It is to provide a positive electrode for a water electrolyte battery, a nonaqueous electrolyte battery, and a battery pack.
  • the positive electrode active material for a nonaqueous electrolyte battery has active material particles and a coating on the surface of the active material particles.
  • the active material particles are LiMn 1-xy Fe x A y PO 4 (A represents at least one element selected from the group consisting of Mg, Ca, Al, Ti, Zn and Zr, and x and y are 0 ⁇ x ⁇ 0.3 and 0 ⁇ y ⁇ 0.1).
  • the coating includes an oxide containing boron and lithium and a carbonaceous material.
  • the partial expanded sectional view of FIG. The schematic sectional drawing which shows an example of the nonaqueous electrolyte battery which concerns on 3rd Embodiment.
  • the expanded sectional view of the A section of FIG. The partial notch perspective view which shows an example of the other nonaqueous electrolyte battery which concerns on 3rd Embodiment.
  • the expanded sectional view of the B section of FIG. The schematic exploded perspective view which shows the battery pack which concerns on 4th Embodiment.
  • the block diagram which shows the electric circuit of the battery pack of FIG.
  • a positive electrode active material for a non-aqueous electrolyte battery having active material particles and a coating containing an oxide and carbonaceous material containing boron and lithium on the surface of the active material particles is provided.
  • an oxide containing boron and lithium may be referred to as a boron-lithium containing oxide.
  • FIG. 1 shows a schematic cross-sectional view for explaining the positive electrode active material for a non-aqueous electrolyte battery of this embodiment
  • FIG. 2 shows a partially enlarged cross-sectional view of FIG. 1 and 2
  • a positive electrode active material 10 for a nonaqueous electrolyte battery has active material particles 11 and a film 12 formed on the surface thereof.
  • Active material particles 11 may include a phosphate salt represented by LiMn 1-x-y Fe x A y PO 4.
  • A represents at least one element selected from the group consisting of Mg, Ca, Al, Ti, Zn and Zr, and x and y are 0 ⁇ x ⁇ 0.3, 0 ⁇ y ⁇ 0.1.
  • the active material particles 11 preferably have an olivine structure.
  • the average particle diameter of the primary particles of the active material particles 11 is preferably in the range of 0.01 ⁇ m to 1 ⁇ m, and more preferably in the range of 0.01 ⁇ m to 0.5 ⁇ m.
  • the primary particles may be aggregated to form secondary particles of 10 ⁇ m or less.
  • the coating film 12 includes a boron-lithium-containing oxide 13 and a carbonaceous material 14 as shown in FIG.
  • the thickness of the film 12 is preferably in the range of 1 nm to 50 nm, more preferably in the range of 5 nm to 20 nm.
  • the boron-lithium-containing oxide 13 preferably has a function of conducting lithium ions.
  • the boron-lithium-containing oxide 13 is preferably a composite of lithium oxide and boron oxide represented by zLi 2 O—wB 2 O 3 .
  • z and w are preferably in a molar ratio of 0.5: 1 to 5: 1, and more preferably in a range of 0.5: 1 to 2: 1.
  • a composite in which the molar ratio of z and w is in the above range has a high density, and the effect of suppressing side reactions with the nonaqueous electrolyte is improved.
  • the content of the boron-lithium-containing oxide 13 is preferably in the range of 0.5 mass% or more and 5.0 mass% or less with respect to the active material particles 11 as the boron content, and 0.5 mass% or more and 3. More preferably, it is in the range of 0% by mass or less.
  • the amount of boron can be measured by quantifying a solution obtained by dissolving the active material particles 11 with acid and then diluting with pure water by ICP (Inductively Coupled Plasma) analysis.
  • the carbonaceous material 14 has electrical conductivity.
  • the carbonaceous material 14 is preferably attached to the surface of the active material particles 11 in a fibrous form.
  • the fibrous carbonaceous material is preferably spread three-dimensionally along the surface of the active material particles 11. That is, the carbonaceous material 14 is preferably in a porous shape having pores.
  • the coating 12 is preferably in a form in which the pores of the porous carbonaceous material 14 are filled with the boron-lithium-containing oxide 13.
  • the content of the carbonaceous material 14 is preferably in the range of 0.5 mass% or more and 5.0 mass% or less with respect to the active material particles 11.
  • the amount of carbon contained in the coating 12 is determined by quantitative analysis of the elemental composition on the active material surface by SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-ray-Spectroscopy) Combined with the quantitative analysis of film thickness and composition by XPS (X-ray Photoelectron Spectroscopy: X-ray photoelectron spectroscopy) in the depth direction, the thickness of the coating 12 and the amount of carbon and boron contained in the coating 12 can be determined. It can be calculated by calculating and making it correspond to the amount of boron obtained by ICP analysis.
  • the positive electrode active material for a non-aqueous electrolyte battery of the present embodiment has a maximum peak on the (311) plane at the interface portion of the active material particles in an X-ray diffraction pattern measured by an X-ray diffraction method using Cu—K ⁇ rays. It is preferable that the diffraction angle 2 ⁇ is shifted to a high angle in the range of 0.01 ° or more and 0.15 ° or less than the diffraction angle 2 ⁇ of the maximum peak of the (311) plane in the bulk portion of the active material particles.
  • the X-ray diffraction pattern of the interface portion of the active material particles can be measured by an in-plane X-ray diffraction method.
  • the in-plane X-ray diffraction method is a method for evaluating a lattice plane perpendicular to a sample surface by fixing the incident angle of X-rays near the total reflection critical angle.
  • the incident depth of X-rays on a sample is usually several tens of nm.
  • the X-ray diffraction pattern of the bulk portion of the active material particles can be measured by an out-of-plane X-ray diffraction method.
  • the out-of-plane X-ray diffraction method is a method for evaluating a lattice plane parallel to a sample surface by changing the incident angle of X-rays.
  • the X-ray incident depth on the sample is usually several tens of ⁇ m.
  • pre-processing is performed as follows. First, the nonaqueous electrolyte battery is charged to a state close to a state in which lithium ions are completely detached from the positive electrode active material crystals. Next, the nonaqueous electrolyte battery is disassembled in a glove box filled with argon, and the electrode is taken out. The extracted electrode is washed with an appropriate solvent and dried under reduced pressure. As the solvent, for example, ethyl methyl carbonate can be used. After washing and drying, make sure that there are no white precipitates such as lithium salts on the surface.
  • the solvent for example, ethyl methyl carbonate can be used. After washing and drying, make sure that there are no white precipitates such as lithium salts on the surface.
  • the diffraction angle 2 ⁇ of the maximum peak of the (311) plane at the interface part of the active material particles is shifted to a high angle, suggesting that a part of the interface of the active material particles is substituted with boron. It is thought that there is.
  • the reason for this is that when the X-ray diffraction pattern of the interface part and the bulk part is measured for the active material particles before and after the formation of the film containing the boron-lithium-containing oxide, the diffraction angle 2 ⁇ of the (311) plane of the bulk part Is the same as before and after the formation of the film, but the diffraction angle 2 ⁇ of the (311) plane at the interface portion is shifted to a high angle after the film is formed.
  • the coating becomes difficult to peel off from the active material particle. It can be stably protected over a long period of time.
  • the positive electrode active material for a non-aqueous electrolyte battery is produced, for example, by preparing active material particles coated with a porous carbonaceous material, and then filling the carbonaceous material of the active material particles with a boron-lithium-containing oxide. can do.
  • the following method can be used as a method for producing active material particles coated with a porous carbonaceous material.
  • active material particles are generated by a hydrothermal method in the presence of an organic compound to obtain active material particles whose surfaces are coated with the organic compound.
  • the active material particles are heat-treated to thermally decompose the organic compound to obtain a carbonaceous material.
  • a water-soluble polymer such as sodium carboxymethyl cellulose can be used.
  • the active material particles coated with the porous carbonaceous material are obtained, for example, by mixing active material particles produced by a solid phase method and an organic compound to obtain active material particles having an organic compound attached to the surface, Alternatively, the active material particles can be heat treated to thermally decompose the organic compound to obtain a carbonaceous material.
  • a solid phase method or a liquid phase method can be used.
  • the following method can be used. First, a dispersion is prepared in which active material particles coated with a carbonaceous material are dispersed in a solvent in which a lithium compound and a boron compound are dissolved. Next, this dispersion is heated at 80 ° C. with stirring, and the boron compound and lithium compound are allowed to enter the pores of the carbonaceous material while evaporating the solvent to obtain a precursor powder.
  • the obtained precursor powder is fired to react the boron compound and the lithium compound that have entered the pores of the carbonaceous material, thereby generating a boron-lithium-containing oxide.
  • the temperature of the baking treatment is usually 450 ° C. or higher and 600 ° C. or lower.
  • the heat treatment time is usually 3 hours or longer and 10 hours or shorter.
  • the solvent used in the liquid phase method examples include alcohols such as methanol and ethanol, organic solvents such as NMP, or water.
  • organic solvents such as NMP, or water.
  • the lithium compound it is desirable to use lithium hydroxide or lithium nitrate.
  • the boron compound it is desirable to use boric acid or boron oxide (B 2 O 3 ). It is also desirable to use lithium borate as the compound containing lithium and boron.
  • the positive electrode active material for a non-aqueous electrolyte battery of the present embodiment described above a film containing an oxide containing boron and lithium (boron-lithium containing oxide) and a carbonaceous material is formed on the surface of the active material particles. Therefore, the side reaction between the active material particles and the non-aqueous electrolyte hardly occurs. For this reason, the nonaqueous electrolyte battery using the positive electrode active material for a nonaqueous electrolyte battery according to the present embodiment has a high discharge rate due to the coating of the reaction product of the nonaqueous electrolyte being formed on the surface of the active material particles. The discharge capacity is less likely to decrease, and the cycle life is prolonged.
  • a positive electrode for a non-aqueous electrolyte battery having a current collector and a positive electrode active material layer formed on the current collector is provided.
  • the positive electrode active material the positive electrode active material for a nonaqueous electrolyte battery according to the first embodiment described above is used.
  • the positive electrode active material layer is formed on one side or both sides of the current collector.
  • the current collector is preferably an aluminum foil or an aluminum alloy foil containing one or more elements selected from Mg, Ti, Zn, Mn, Fe, Cu and Si. Further, considering the expansion and contraction of the active material accompanying charging / discharging, an electrolytic foil whose surface is roughened is more desirable.
  • the mixing ratio of the positive electrode active material, the conductive agent and the binder contained in the positive electrode active material layer is 80% by mass to 95% by mass of the positive electrode active material, 3% by mass to 18% by mass of the conductive agent, and the binder. Is preferably 2% by mass or more and 17% by mass or less.
  • the amount of the conductive agent 3% by mass or more the effect of ensuring the conductivity of the electrode can be exhibited.
  • the amount of the conductive agent 18% by mass or less the decomposition of the nonaqueous electrolyte on the surface of the conductive agent under high temperature storage can be reduced.
  • Sufficient electrode strength can be obtained by setting the binder to an amount of 2% by mass or more. By setting the binder to an amount of 17% by mass or less, the internal resistance in the positive electrode active material layer can be reduced.
  • Examples of the conductive agent include carbonaceous materials such as acetylene black, carbon black, graphite, carbon nanofiber, and carbon nanotube. These carbonaceous materials may be used alone or a plurality of carbonaceous materials may be used.
  • the binder binds the positive electrode active material, the conductive agent and the current collector.
  • the binder include polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVdF), and fluorine rubber, acrylic resin, cellulose such as carboxymethyl cellulose, and the like.
  • a positive electrode active material, a conductive agent, and a binder are suspended in a solvent to prepare a slurry. This slurry is applied to one or both sides of the current collector and dried to form a positive electrode active material layer. Then press.
  • the positive electrode active material, the conductive agent, and the binder can be formed in a pellet shape and used as the positive electrode active material layer.
  • the positive electrode active material for nonaqueous electrolyte battery of the first embodiment described above is used as the positive electrode active material
  • the positive electrode active material for nonaqueous electrolyte battery of the present embodiment is used.
  • a non-aqueous electrolyte battery having a positive electrode is less likely to have a reduced discharge capacity at a high discharge rate and has a long cycle life.
  • a nonaqueous electrolyte battery including a positive electrode, a negative electrode, and a nonaqueous electrolyte is provided.
  • the positive electrode for a nonaqueous electrolyte battery according to the second embodiment described above is used as the positive electrode.
  • FIG. 3 is a schematic cross-sectional view of a nonaqueous electrolyte battery
  • FIG. 4 is an enlarged cross-sectional view of part A of FIG.
  • Each figure is a schematic diagram for promoting explanation and understanding of the invention, and its shape, dimensions, ratio, etc. are different from the actual apparatus, but these are considered in consideration of the following explanation and known techniques. The design can be changed as appropriate.
  • the flat wound electrode group 21 is housed in a bag-like exterior member 22 made of a laminate film in which an aluminum foil is interposed between two resin layers.
  • the flat wound electrode group 21 is formed by winding a laminate in which the negative electrode 23, the separator 24, the positive electrode 25, and the separator 24 are laminated in this order from the outside in a spiral shape and press-molding.
  • the outermost negative electrode 23 has a negative electrode layer 23b formed on one surface on the inner surface side of the negative electrode current collector 23a.
  • negative electrode layers 23b are formed on both surfaces of the negative electrode current collector 23a.
  • the active material in the negative electrode layer 23b includes a titanium oxide compound having a TiO 2 (B) structure.
  • positive electrode layers 25b are formed on both surfaces of the positive electrode current collector 25a.
  • the negative electrode terminal 26 is connected to the negative electrode current collector 23 a of the outermost negative electrode 23, and the positive electrode terminal 27 is connected to the positive electrode current collector 25 a of the inner positive electrode 25. .
  • the negative terminal 26 and the positive terminal 27 are extended from the opening of the bag-shaped exterior member 22 to the outside.
  • the liquid non-aqueous electrolyte is injected from the opening of the bag-shaped exterior member 22.
  • the positive electrode for a nonaqueous electrolyte battery of the second embodiment described above is used as the positive electrode.
  • the negative electrode, nonaqueous electrolyte, separator, exterior member, positive electrode terminal, and negative electrode terminal used in the nonaqueous electrolyte battery of this embodiment will be described in detail.
  • the negative electrode includes a negative electrode current collector and a negative electrode active material layer.
  • the negative electrode active material layer includes a negative electrode active material, a conductive agent, and a binder.
  • the negative electrode active material layer is formed on one side or both sides of the negative electrode current collector.
  • the negative electrode active material includes a titanium composite oxide. Titanium composite oxides such as spinel lithium titanate, monoclinic ⁇ -type titanium composite oxide, anatase type titanium composite oxide, ramsdelide type lithium titanate, TiNb 2 O 7 , Ti 2 Nb 2 O 9, etc. And titanium-containing oxides.
  • the lithium titanate for example, it has a crystal structure of monoclinic type, represented by the general formula Li x Ti 1-y M1 y Nb 2-z M2 z O 7 ⁇ ⁇ , M1 is Zr, Si And at least one selected from the group consisting of Sn, Fe, Co, Mn and Ni, and M2 is a compound which is at least one selected from the group consisting of V, Nb, Ta, Mo, W and Bi.
  • the blending ratio of the negative electrode active material, the conductive agent and the binder is such that the negative electrode active material is 70% by mass to 96% by mass, the conductive agent is 2% by mass to 28% by mass, and the binder is 2% by mass to 28% by mass. % Or less is preferable. If the conductive agent is less than 2% by mass, the current collection performance of the negative electrode active material layer may be reduced, and the large current characteristics of the nonaqueous electrolyte battery may be reduced. On the other hand, if the binder is less than 2% by mass, the binding property between the negative electrode active material layer and the negative electrode current collector is lowered, and the cycle characteristics may be lowered. On the other hand, from the viewpoint of increasing the capacity, the conductive agent and the binder are each preferably 28% by mass or less.
  • the negative electrode current collector is made of an aluminum foil that is electrochemically stable in a potential range nobler than 1.0 V or an aluminum alloy foil containing elements such as Mg, Ti, Zn, Mn, Fe, Cu, and Si. Preferably it is formed.
  • the negative electrode can be produced, for example, by the following method. First, a negative electrode active material, a conductive agent, and a binder are suspended in a solvent to prepare a slurry. This slurry is applied to one or both sides of the negative electrode current collector and dried to form a negative electrode active material layer. Then press. Alternatively, the negative electrode active material, the conductive agent, and the binder can be formed in a pellet shape and used as the negative electrode active material layer.
  • Nonaqueous electrolyte As the non-aqueous electrolyte, a liquid non-aqueous electrolyte or a gel non-aqueous electrolyte can be used.
  • the liquid non-aqueous electrolyte is prepared by dissolving the electrolyte in an organic solvent.
  • the concentration of the electrolyte is preferably in the range of 0.5 to 2.5 mol / l.
  • the gel-like nonaqueous electrolyte is prepared by combining a liquid electrolyte and a polymer material.
  • electrolyte examples include lithium perchlorate (LiClO 4 ), lithium hexafluorophosphate (LiPF 6 ), lithium tetrafluoroborate (LiBF 4 ), lithium hexafluoroarsenide (LiAsF 6 ), trifluorometa Lithium salts such as lithium sulfonate (LiCF 3 SO 3 ) and bistrifluoromethylsulfonylimitolithium [LiN (CF 3 SO 2 ) 2 ] are included. These electrolytes can be used alone or in combination of two or more.
  • the electrolyte preferably contains LiPF 6.
  • organic solvents examples include propylene carbonate (PC), ethylene carbonate (EC), cyclic carbonates such as vinylene carbonate; diethyl carbonate (DEC), dimethyl carbonate (DMC), chain like methyl ethyl carbonate (MEC) Carbonates; cyclic ethers such as tetrahydrofuran (THF), 2-methyltetrahydrofuran (2MeTHF), dioxolane (DOX); chain ethers such as dimethoxyethane (DME) and dietoethane (DEE); ⁇ -butyrolactone (GBL), ⁇ - Methyl ⁇ -butyrolactone (MBL) acetonitrile (AN) and sulfolane (SL) are included. These organic solvents can be used alone or in combination of two or more.
  • PC propylene carbonate
  • EC ethylene carbonate
  • DEC diethyl carbonate
  • DMC dimethyl carbonate
  • MEC chain like methyl eth
  • Examples of more preferable organic solvents include two or more selected from the group consisting of propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl carbonate (DMC), and methyl ethyl carbonate (MEC). And a mixed solvent containing ⁇ -butyrolactone (GBL). By using such a mixed solvent, a nonaqueous electrolyte battery having excellent low temperature characteristics can be obtained.
  • PC propylene carbonate
  • EC ethylene carbonate
  • DEC diethyl carbonate
  • DMC dimethyl carbonate
  • MEC methyl ethyl carbonate
  • GBL ⁇ -butyrolactone
  • polymer material examples include polyvinylidene fluoride (PVdF), polyacrylonitrile (PAN), and polyethylene oxide (PEO).
  • PVdF polyvinylidene fluoride
  • PAN polyacrylonitrile
  • PEO polyethylene oxide
  • a porous film formed from a material such as polyethylene, polypropylene, cellulose, and polyvinylidene fluoride (PVdF), a synthetic resin nonwoven fabric, and the like can be used.
  • PVdF polyvinylidene fluoride
  • a porous film made of polyethylene or polypropylene is preferable from the viewpoint of improving safety because it can be melted at a constant temperature to interrupt the current.
  • a laminated film bag-like container or a metal container is used as the exterior member.
  • the shape include a flat type, a square type, a cylindrical type, a coin type, a button type, a sheet type, and a laminated type.
  • a large battery mounted on a two-wheel to four-wheel automobile or the like may be used.
  • the laminate film a multilayer film in which a metal layer is interposed between resin films is used.
  • the metal layer is preferably an aluminum foil or an aluminum alloy foil for weight reduction.
  • a polymer material such as polypropylene (PP), polyethylene (PE), nylon, and polyethylene terephthalate (PET) can be used.
  • the laminate film can be formed into the shape of an exterior member by sealing by heat sealing.
  • the laminate film preferably has a thickness of 0.2 mm or less.
  • the metal container can be formed from aluminum or an aluminum alloy.
  • the aluminum alloy preferably contains elements such as magnesium, zinc and silicon.
  • the content of transition metals such as iron, copper, nickel and chromium is preferably 100 ppm or less. Thereby, it becomes possible to dramatically improve long-term reliability and heat dissipation in a high temperature environment.
  • the metal container preferably has a thickness of 0.5 mm or less, and more preferably has a thickness of 0.2 mm or less.
  • the positive electrode terminal is formed of a material having electrical stability and conductivity in a range where the potential with respect to the lithium ion metal is 3.0 V or more and 4.5 V or less.
  • Examples of the material of the positive electrode terminal include aluminum or an aluminum alloy containing one or more elements selected from Mg, Ti, Zn, Mn, Fe, Cu, and Si.
  • the positive electrode terminal is preferably formed of the same material as the positive electrode current collector in order to reduce contact resistance with the positive electrode current collector.
  • the negative electrode terminal is formed of a material having electrical stability and conductivity in a range where the potential with respect to the lithium ion metal is 1.0 V or more and 3.0 V or less.
  • the material of the negative electrode terminal include aluminum or an aluminum alloy containing one or more elements selected from Mg, Ti, Zn, Mn, Fe, Cu, and Si.
  • the negative electrode terminal is preferably formed from the same material as the negative electrode current collector in order to reduce the contact resistance with the negative electrode current collector.
  • the nonaqueous electrolyte battery according to the present embodiment is not limited to the structure shown in FIGS. 3 and 4 described above, and may be, for example, the battery shown in FIGS. 5 and 6.
  • FIG. 5 is a partially cutaway perspective view schematically showing another nonaqueous electrolyte battery according to the present embodiment
  • FIG. 6 is an enlarged cross-sectional view of a portion B in FIG.
  • the nonaqueous electrolyte battery 30 shown in FIG. 5 and FIG. 6 is configured with a laminated electrode group 31 housed in an exterior material 32. As shown in FIG. 6, the stacked electrode group 31 has a structure in which positive electrodes 33 and negative electrodes 34 are alternately stacked with separators 35 interposed therebetween.
  • the positive electrode layer 33b contains a positive electrode active material.
  • each negative electrode current collector 34a and a negative electrode layer 34b contains a negative electrode active material.
  • One side of the negative electrode current collector 34 a of each negative electrode 34 protrudes from the negative electrode 34.
  • the protruding negative electrode current collector 34 a is electrically connected to the strip-shaped negative electrode terminal 36.
  • the tip of the strip-shaped negative electrode terminal 36 is drawn out from the exterior member 32 to the outside.
  • the positive electrode current collector 33 a of the positive electrode 33 protrudes from the positive electrode 33 on the side opposite to the protruding side of the negative electrode current collector 34 a.
  • a positive electrode current collector 33 a protruding from the positive electrode 33 is electrically connected to a belt-like positive electrode terminal 37.
  • the front end of the strip-like positive electrode terminal 37 is located on the side opposite to the negative electrode terminal 36 and is drawn out from the side of the exterior member 32 to the outside.
  • the materials, blending ratios, dimensions, and the like of the members constituting the nonaqueous electrolyte battery 30 shown in FIGS. 5 and 6 are the same as those of the components of the nonaqueous electrolyte battery 20 described in FIGS. 3 and 4. .
  • the discharge capacity is hardly reduced at a high discharge rate, and the cycle life is increased. Becomes longer.
  • a battery pack provided with a nonaqueous electrolyte battery is provided.
  • the nonaqueous electrolyte battery of the third embodiment described above is used as the nonaqueous electrolyte battery.
  • the battery pack of this embodiment will be described with reference to the drawings.
  • the battery pack has one or a plurality of nonaqueous electrolyte batteries (unit cells).
  • each unit cell is electrically connected in series or in parallel.
  • FIG. 7 and 8 show an example of a battery pack including a plurality of nonaqueous electrolyte batteries.
  • FIG. 7 is an exploded perspective view of the battery pack.
  • FIG. 7 is a block diagram showing an electric circuit of the battery pack of FIG. In the non-aqueous electrolyte secondary battery pack 40 shown in FIG. 7, the non-aqueous electrolyte battery 20 shown in FIG.
  • the plurality of single cells 41 are stacked such that the negative electrode terminal 26 and the positive electrode terminal 27 extending to the outside are aligned in the same direction, and are fastened with an adhesive tape 42 to constitute an assembled battery 43. These unit cells 41 are electrically connected to each other in series as shown in FIGS.
  • the printed wiring board 44 is disposed to face the side surface of the unit cell 41 from which the negative electrode terminal 26 and the positive electrode terminal 27 extend. As shown in FIG. 7, a thermistor 45 (see FIG. 8), a protection circuit 46, and a terminal 47 for energizing external devices are mounted on the printed wiring board 44. An insulating plate (not shown) is attached to the surface of the printed wiring board 44 facing the assembled battery 43 in order to avoid unnecessary connection with the wiring of the assembled battery 43.
  • the positive electrode side lead 48 is connected to the positive electrode terminal 27 located in the lowermost layer of the assembled battery 43, and the tip thereof is inserted into the positive electrode side connector 49 of the printed wiring board 44 and electrically connected thereto.
  • the negative electrode side lead 50 is connected to the negative electrode terminal 26 located in the uppermost layer of the assembled battery 43, and the tip thereof is inserted into the negative electrode side connector 51 of the printed wiring board 44 and electrically connected thereto.
  • the positive connector 49 and the negative connector 51 are connected to the protection circuit 46 through wirings 52 and 53 (see FIG. 8) formed on the printed wiring board 44.
  • the thermistor 45 is used to detect the temperature of the unit cell 41 and is not shown in FIG. 7, but is provided in the vicinity of the unit cell 41 and its detection signal is transmitted to the protection circuit 46. .
  • the protection circuit 46 can cut off the plus side wiring 54a and the minus side wiring 54b between the protection circuit 46 and the terminal 47 for energization to an external device under a predetermined condition.
  • the predetermined condition is, for example, when the temperature detected by the thermistor 45 is equal to or higher than a predetermined temperature.
  • the predetermined condition is when an overcharge, overdischarge, overcurrent, or the like of the unit cell 41 is detected. Such detection of overcharge or the like is performed for each single battery 41 or the entire single battery 41.
  • a battery voltage may be detected and a positive electrode potential or a negative electrode potential may be detected.
  • a lithium electrode used as a reference electrode is inserted into each unit cell 41.
  • the voltage detection wiring 55 is connected to each of the single cells 41, and the detection signal is transmitted to the protection circuit 46 through the wiring 55.
  • protective sheets 56 made of rubber or resin are disposed on the three side surfaces of the assembled battery 43 excluding the side surfaces from which the positive electrode terminal 27 and the negative electrode terminal 26 protrude.
  • the assembled battery 43 is stored in the storage container 57 together with each protective sheet 56 and the printed wiring board 44. That is, the protective sheet 56 is disposed on each of the inner side surface in the long side direction and the inner side surface in the short side direction of the storage container 57, and the printed wiring board 44 is disposed on the inner side surface opposite to the protective sheet 56 in the short side direction. Be placed.
  • the assembled battery 43 is located in a space surrounded by the protective sheet 56 and the printed wiring board 44.
  • the lid 58 is attached to the upper surface of the storage container 57.
  • a heat shrink tape may be used instead of the adhesive tape.
  • protective sheets are arranged on both side surfaces of the assembled battery, the heat shrinkable tape is circulated, and then the heat shrinkable tape is heat shrunk to bind the assembled battery.
  • the configuration in which the unit cells 41 are connected in series is shown.
  • the unit cells 41 may be connected in parallel or in parallel with the series connection. It is good also as a structure which combined the connection.
  • the assembled battery packs can be further connected in series and in parallel.
  • the aspect of a battery pack is changed suitably according to a use.
  • a use of the battery pack according to the present embodiment one that is required to exhibit excellent cycle characteristics when a large current is taken out is preferable.
  • Specific examples include a power source for a digital camera, a two-wheel or four-wheel hybrid electric vehicle, a two-wheel or four-wheel electric vehicle, an in-vehicle device such as an assist bicycle.
  • the battery pack according to the present embodiment is suitably used for in-vehicle use.
  • the nonaqueous electrolyte battery according to the third embodiment is provided as a nonaqueous electrolyte battery, the discharge capacity is hardly reduced at a high discharge rate, and the cycle life is long. become longer.
  • the solution in which the starting material was dissolved was put in a pressure vessel and sealed, and hydrothermally treated at 200 ° C. for 3 hours with stirring. After the hydrothermal treatment, the product was recovered by a centrifugal separator. The recovered product was dried by lyophilization. The dried product was pulverized in ethanol with a planetary ball mill apparatus, and then heat-treated at 700 ° C. for 1 hour in an argon atmosphere to obtain active material particles.
  • the obtained active material particles had a composition of LiMn 0.85 Fe 0.10 Mg 0.05 PO 4 and the surface was coated with a porous carbonaceous material having pores. Moreover, content of the carbonaceous material with respect to active material particle was 2.0 mass%.
  • N-methyl is adjusted so that the positive electrode active material prepared as described above is 90% by mass, 5% by mass of acetylene black as a conductive agent, and 5% by mass of polyvinylidene fluoride (PVdF) as a binder.
  • a slurry was prepared by adding to and mixing with pyrrolidone (NMP). The prepared slurry is applied to a current collector made of an aluminum foil having a thickness of 15 ⁇ m, dried, and pressed to have a current collector and a positive electrode active material layer having an electrode density of 1.8 g / cm 3. A positive electrode was produced.
  • An X-ray diffraction pattern (X-ray source: Cu—K ⁇ ray) of the produced positive electrode was measured using an in-plane method and an out-of-plane method.
  • the incident angle was fixed at 0.8 °
  • the step width was 0.02 °
  • the measurement time for each step was 0.4 seconds.
  • the step width was 0.02 ° and the measurement time for each step was 0.4 seconds.
  • the peak angle (2 ⁇ ) of the (311) plane of the positive electrode active material particles was measured. Then, a value obtained by subtracting the peak angle obtained by the out-of-plane method from the peak angle obtained by the in-plane method was calculated as a shift amount of the peak angle of the (311) plane in the interface portion of the positive electrode active material particles. The result is shown in the column of “(311) plane shift amount” in Table 1.
  • a tripolar cell was produced using the produced positive electrode.
  • the working electrode used was a positive electrode punched into a 2 cm square and pressed on a titanium plate.
  • As the reference electrode and the counter electrode a nickel mesh bonded with lithium metal was used.
  • Example 2 In the filling of the boron-lithium-containing oxide into the porous carbonaceous material of Example 1, the mass ratio of the amount of boron in the methanol solution to the amount of active material particles is 1.0%.
  • a positive electrode active material was produced in the same manner as in Example 1 except that the mixture was mixed in an amount ratio of 100. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 3 In the filling of the boron-lithium-containing oxide into the porous carbonaceous material in Example 1 (2), the methanol solution and the active material particles are mixed, and the mass ratio of the amount of boron and the amount of active material particles in the methanol solution is 2.5. : A positive electrode active material was produced in the same manner as in Example 1 except that the mixture was mixed in an amount ratio of 100. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 4 In the filling of the boron-lithium-containing oxide into the porous carbonaceous material of Example 1, the mass ratio of the amount of boron in the methanol solution to the amount of active material particles is 5.0%. : A positive electrode active material was produced in the same manner as in Example 1 except that the mixture was mixed in an amount ratio of 100. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 5 Example 3 (2) Example 3 except that the porous carbonaceous material was filled with the boron-lithium-containing oxide except that the molar ratio of lithium hydroxide to boric acid in the methanol solution was 3: 1.
  • a positive electrode active material was produced in the same manner. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • CMC carboxymethyl cellulose
  • a positive electrode active material was produced in the same manner as in Example 1 except for the above.
  • a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured.
  • a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 7 In the production of active material particles coated with porous carbonaceous material in Example 1 (1), 30% titanium sulfate aqueous solution was used instead of magnesium sulfate heptahydrate, lithium sulfate, manganese sulfate pentahydrate Product, iron sulfate heptahydrate, 30% aqueous titanium sulfate solution, diammonium hydrogen phosphate, sodium carboxymethyl cellulose (CMC) at a molar ratio of Li, Mn, Fe, Ti, PO 4 , CMC at 3: 0.
  • CMC carboxymethyl cellulose
  • a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • the composition of the particles is LiMn 0.84 Fe 0.10 Zn 0.06 PO 4 , the carbonaceous material content is 1.0% by mass relative to the active material particles), and (2) boron-lithium content in the porous carbonaceous material For oxide filling Te, the content of boron,
  • a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 1 A positive electrode active material was produced in the same manner as in Example 1 except that (2) the porous carbonaceous material was not filled with the boron-lithium-containing oxide. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 6 a positive electrode active material was produced in the same manner as in Example 6 except that (2) the porous carbonaceous material was not filled with the boron-lithium-containing oxide. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 7 a positive electrode active material was prepared in the same manner as in Example 7 except that (2) the porous carbonaceous material was not filled with the boron-lithium-containing oxide. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 8 a positive electrode active material was produced in the same manner as in Example 8, except that (2) the porous carbonaceous material was not filled with the boron-lithium-containing oxide. Using the obtained positive electrode active material, a positive electrode was produced in the same manner as in Example 1, and the shift amount of the peak angle of the (311) plane at the interface portion of the positive electrode active material particles was measured. Further, using the obtained positive electrode, a tripolar cell was produced in the same manner as in Example 1, and a discharge rate characteristic test and a cycle characteristic test were performed. The results are shown in Table 1.
  • Example 9 A laminate type cell was produced using the positive electrode produced in Example 1 and containing the positive electrode active material having a film containing a boron-lithium-containing oxide and a carbonaceous material formed on the surface.
  • the negative electrode was produced as follows. First, 90% by mass of spinel-type titanium oxide powder, 5% by mass of acetylene black, and 5% by mass of polyvinylidene fluoride (PVdF) were added to N-methylpyrrolidone (NMP) and mixed to prepare a slurry. This slurry was applied to both surfaces of a current collector made of an aluminum foil having a thickness of 15 ⁇ m, dried, and pressed to prepare a negative electrode having an electrode density of 2.0 g / cm 3 .
  • PVdF polyvinylidene fluoride
  • a positive electrode, a separator made of a polyethylene porous film having a thickness of 25 ⁇ m, a negative electrode and a separator were laminated in this order, and then wound in a spiral shape. This was heated and pressed at 90 ° C. to produce a flat electrode group having a width of 30 mm and a thickness of 3.0 mm.
  • the obtained electrode group was housed in a pack made of a laminate film and vacuum dried at 80 ° C. for 24 hours.
  • the laminate film is formed by forming a polypropylene layer on both sides of an aluminum foil having a thickness of 40 ⁇ m, and the overall thickness is 0.1 mm.
  • a liquid non-aqueous electrolyte was poured into a laminate film pack containing the electrode group. Thereafter, the pack was completely sealed by heat sealing to produce a nonaqueous electrolyte battery having the structure shown in FIG. 3 described above, a width of 35 mm, a thickness of 3.2 mm, and a height of 65 mm.
  • the obtained nonaqueous electrolyte battery is less likely to have a reduced discharge capacity at a high discharge rate and has a long cycle life.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

La présente invention porte, selon un mode de réalisation, sur un matériau actif d'électrode positive pour une batterie à électrolyte non aqueux, ledit matériau actif comprenant : des particules de matériau actif ; et des revêtements formés sur la surface des particules de matériau actif. Les particules de matériau actif comprennent un phosphate représenté par LiMn1-x-yFexAyPO4 (A représente au moins un élément métallique choisi dans le groupe constitué par le magnésium (Mg), le calcium (Ca), l'aluminium (Al), le titane (Ti), le zinc (Zn) et le zirconium (Zr), et x et y satisfont à 0 < x ≤ 0,3 et 0 ≤ y ≤ 0,1). Les revêtements comprennent un oxyde contenant du bore et du lithium, et un matériau carboné.
PCT/JP2015/083995 2015-12-03 2015-12-03 Matériau actif d'électrode positive pour une batterie à électrolyte non aqueux, électrode positive pour une batterie à électrolyte non aqueux, batterie à électrolyte non aqueux et bloc de batteries WO2017094163A1 (fr)

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PCT/JP2015/083995 WO2017094163A1 (fr) 2015-12-03 2015-12-03 Matériau actif d'électrode positive pour une batterie à électrolyte non aqueux, électrode positive pour une batterie à électrolyte non aqueux, batterie à électrolyte non aqueux et bloc de batteries

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JP2020145108A (ja) * 2019-03-07 2020-09-10 住友大阪セメント株式会社 電極材料、該電極材料の製造方法、電極、及びリチウムイオン電池
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