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WO2015019483A1 - Matériau actif d'électrode positive pour batteries secondaires à électrolyte non aqueux, électrode positive pour batteries secondaires à électrolyte non aqueux l'utilisant, et batterie secondaire à électrolyte non aqueux - Google Patents

Matériau actif d'électrode positive pour batteries secondaires à électrolyte non aqueux, électrode positive pour batteries secondaires à électrolyte non aqueux l'utilisant, et batterie secondaire à électrolyte non aqueux Download PDF

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Publication number
WO2015019483A1
WO2015019483A1 PCT/JP2013/071590 JP2013071590W WO2015019483A1 WO 2015019483 A1 WO2015019483 A1 WO 2015019483A1 JP 2013071590 W JP2013071590 W JP 2013071590W WO 2015019483 A1 WO2015019483 A1 WO 2015019483A1
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WO
WIPO (PCT)
Prior art keywords
positive electrode
active material
electrode active
secondary battery
nonaqueous secondary
Prior art date
Application number
PCT/JP2013/071590
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English (en)
Japanese (ja)
Inventor
心 ▲高▼橋
崇 中林
達哉 遠山
小西　宏明
孝亮 馮
章 軍司
翔 古月
Original Assignee
株式会社日立製作所
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Publication date
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Priority to PCT/JP2013/071590 priority Critical patent/WO2015019483A1/fr
Publication of WO2015019483A1 publication Critical patent/WO2015019483A1/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
    • H01M4/50—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/12—Complex oxides containing manganese and at least one other metal element
    • C01G45/1221—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof
    • C01G45/125—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof of the type (MnO3)n-, e.g. CaMnO3
    • C01G45/1257—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof of the type (MnO3)n-, e.g. CaMnO3 containing lithium, e.g. Li2MnO3 or Li2(MxMn1-x)O3
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Complex oxides containing nickel and at least one other metal element
    • C01G53/42—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
    • C01G53/44—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • 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
    • 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 a positive electrode active material for a non-aqueous secondary battery, a positive electrode for a non-aqueous secondary battery using the same, a non-aqueous secondary battery, and a manufacturing method thereof.
  • Lithium ion secondary batteries have a higher energy density than nickel metal hydride batteries and the like, and are used, for example, as power sources for portable electronic devices.
  • application to medium and large-sized applications such as hybrid vehicles, electric vehicles, stationary uninterruptible power supplies, and power leveling has been promoted.
  • an electric vehicle there is a demand for a longer travel distance, and a further increase in energy density is required.
  • the improvement of the coulomb efficiency and the initial charge / discharge efficiency are required.
  • a layered oxide positive electrode active material of LiCoO 2 , LiCo 1/3 Ni 1/3 Mn 1/3 O 2 is used as the positive electrode active material.
  • the discharge capacity is 150 to 180 Ah / kg, and further higher capacity is required.
  • Patent Document 1 the composition ratio of Li, Co, Ni, and Mn is Li 1+ (1/3) x Co 1-xy Ni (1/2) y Mn (2/3) x + (1/2 )
  • An active material for a lithium secondary battery containing a solid solution of a lithium transition metal composite oxide satisfying y has been proposed.
  • Patent Document 2 discloses I (635) and I (605), which are represented by the chemical formula Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 and have respective intensities of 635 cm ⁇ 1 and 605 cm ⁇ 1 in Raman spectroscopic measurement. ), The discharge capacity and the charge / discharge efficiency are improved when 0.6 ⁇ I (635) / I (605) ⁇ 1.5.
  • the present invention has been made in view of the above points, and the object thereof is a positive electrode active material for a non-aqueous secondary battery having a larger discharge capacity and a high Coulomb efficiency or initial charge / discharge efficiency, and It is to obtain a non-aqueous secondary battery.
  • a positive electrode active material for a non-aqueous secondary battery having a large discharge capacity and high coulomb efficiency is provided.
  • the positive electrode active material for a non-aqueous secondary battery of the present invention that achieves high energy density can be expressed as a solid solution of Li 2 MnO 3 , LiNiO 2 , and LiMnO 2 . Note that a simple mixture of Li 2 MnO 3 powder, LiNiO 2 powder, and LiMnO 2 powder is clearly distinguished from a solid solution.
  • composition formula xLi 2 MnO 3 — (1-x) LiNiaMnbMcO 2
  • M is Co, Ta, Zr, Cr, Ni, Fe, V, Al, Mg, Ti, W, etc.
  • X in the composition formula represents the ratio of Li 2 MnO 3 in xLi 2 MnO 3 — (1-x) LiNiaMnbMcO 2 .
  • a in the composition formula indicates the content ratio (atomic weight ratio) of Ni in the positive electrode active material.
  • a is 0.5 or less, the content ratio of Ni mainly contributing to the charge / discharge reaction is decreased, and the capacity is decreased.
  • b represents the content ratio (atomic weight ratio) of Mn in the positive electrode active material.
  • the composition ratio of Li, Mn, Ni, and O may be in the above range.
  • the composition ratio of M is preferably 5 mol% or less in the proportion of the entire transition metal.
  • the above composition contains Li, Ni, and Mn as main components and contains almost no Co. Since Co is expensive, the positive electrode active material in the present embodiment has an advantage of low cost in addition to high energy density. Moreover, decomposition of the electrolytic solution and suppression of gas generation are possible, and cycle characteristics are improved.
  • the intensities of the peak of 430 cm ⁇ 1 attributed to Li 2 MnO 3 and the peak of 600 cm ⁇ 1 attributed to layered LiMO 2 in Raman spectroscopy are I (430) and I ( 600) (I (430) / I (600)) is less than 0.3.
  • I (430) / I (600) is a value that changes by controlling the surface state of the positive electrode active material, and the Coulomb efficiency is improved by setting the above range.
  • Examples of the surface treatment method include sodium sulfate treatment, ammonium sulfate treatment, aluminum nitrate treatment, boric acid treatment, ammonium vanadate treatment, ammonium fluoride treatment, and mixed treatment thereof.
  • I (660) and I (600) which are intensities of 660 cm ⁇ 1 and 600 cm ⁇ 1 in Raman spectroscopic measurement
  • I (660) / I (600) is smaller than 0.35. preferable.
  • I (660) / I (600) also changes depending on the surface state of the positive electrode active material, and the cycle characteristics are improved within the above range.
  • the above configuration having these characteristics is preferable because it can provide a positive electrode active material for a non-aqueous secondary battery that has high energy density, high coulomb efficiency, high cycle characteristics, and low cost.
  • the method for producing the positive electrode active material according to the present invention is not particularly limited, and various methods such as a coprecipitation method and a solid phase method can be employed.
  • a dry ball mill for pulverization and mixing of raw materials, for example, a dry ball mill, a dry bead mill, a dry planetary ball mill, a dry attritor, a dry jet mill, a wet ball mill, a wet bead mill, a wet planetary ball mill, a wet attritor, and a wet jet mill are used. be able to.
  • Examples of the compound containing Li include lithium acetate, lithium nitrate, lithium carbonate, and lithium hydroxide.
  • Examples of the Ni-containing compound include nickel acetate, nickel nitrate, nickel carbonate, nickel sulfate, and nickel hydroxide.
  • Examples of the compound containing Mn include manganese acetate, manganese nitrate, manganese carbonate, manganese sulfate, manganese oxide, and the like.
  • the composition of the positive electrode active material can be determined by elemental analysis such as inductively coupled plasma (ICP).
  • the method for controlling the surface state of the positive electrode active material is as follows. A predetermined amount of the starting nitrate, acetate, sulfate, and ammonium salt is dissolved in water or an organic solvent. This solution was mixed with the positive electrode active material, and the solvent was evaporated. The solvent is preferably evaporated by heating and stirring or spray drying. Finally, the obtained powder is heat-treated at 200 ° C. or higher and 600 ° C. or lower, preferably 300 ° C. or higher and 500 ° C. or lower. The heating time is 1 hour or more and 20 hours or less, preferably 3 hours or more and 8 hours or less.
  • the compound dissolved in water or an organic solvent may be an inorganic compound or a compound containing a metal element selected from the group of Na, Li, B, Al, Si, P, and V.
  • a positive electrode for a non-aqueous secondary battery according to the present invention includes the above positive electrode active material.
  • energy density can be improved, coulombic efficiency can be improved, cycle characteristics can be improved, and cost can be reduced.
  • a nonaqueous secondary battery according to the present invention includes the positive electrode described above. By using it for the positive electrode, a non-aqueous secondary battery with low resistance (high output) can be obtained.
  • the non-aqueous secondary battery according to the present invention can be preferably used for, for example, an electric vehicle.
  • the non-aqueous secondary battery includes a positive electrode including a positive electrode active material, a negative electrode including a negative electrode active material, a separator, an electrolytic solution, an electrolyte, and the like.
  • the negative electrode active material is not particularly limited as long as it is a material that can occlude and release lithium ions.
  • a material generally used in non-aqueous secondary batteries can be used as the negative electrode active material.
  • graphite, silica, lithium alloy, silicon alloy, tin alloy, aluminum alloy and the like can be exemplified.
  • separator those generally used in non-aqueous secondary batteries can be used.
  • examples thereof include polyolefin microporous films and nonwoven fabrics such as polypropylene, polyethylene, and a copolymer of propylene and ethylene.
  • electrolytic solution and the electrolyte those generally used in non-aqueous secondary batteries can be used.
  • diethyl carbonate, dimethyl carbonate, ethylene carbonate, propylene carbonate, vinylene carbonate, methyl acetate, ethyl methyl carbonate, methyl propyl carbonate, dimethoxyethane and the like can be exemplified as the electrolytic solution.
  • the lithium ion secondary battery 1 includes an electrode group having a positive electrode 2 with a positive electrode active material applied to both sides of a current collector, a negative electrode 3 with a negative electrode active material applied to both sides of the current collector, and a separator 4.
  • the positive electrode 2 and the negative electrode 3 are wound through a separator 4 to form a wound electrode group. This wound body is inserted into the battery can 5.
  • the negative electrode 3 is electrically connected to the battery can 5 via the negative electrode lead piece 7.
  • a sealing lid 8 is attached to the battery can 5 via a packing 9.
  • the positive electrode 2 is electrically connected to the sealing lid 8 through the positive electrode lead piece 6.
  • the wound body is insulated by the insulating plate 10.
  • the electrode group may not be the wound body shown in FIG. 1, but may be a laminated body in which the positive electrode 2 and the negative electrode 3 are laminated via the separator 4.
  • Lithium carbonate, manganese carbonate, and nickel carbonate were added to a zirconia pot, acetone was further added, and the mixture was pulverized and mixed without dissolution using a planetary ball mill apparatus.
  • the obtained slurry was dried to obtain a raw material powder.
  • This raw material powder was calcined in the atmosphere at 500 ° C. for 12 hours to obtain a lithium transition metal oxide.
  • the obtained lithium transition metal oxide was added to a zirconia pot, further added with acetone, and pulverized and mixed without dissolution using a planetary ball mill apparatus.
  • the obtained slurry was dried and then fired in the atmosphere at 1000 ° C. for 12 hours to produce the target positive electrode active material.
  • the composition of the positive electrode active material was 0.5Li 2 MnO 3 -0.5LiNi 0.625 Mn 0.375 O 2 .
  • Examples 1 to 4 Four types of samples prepared by adding 5, 7.5, 10, and 15% by mass of sodium sulfate to the above positive electrode active material 0.5Li 2 MnO 3 -0.5LiNi 0.625 Mn 0.375 O 2 and mixing them at 300 ° C. After calcination for a period of time, it was washed with water to produce four active materials of Examples 1 to 4.
  • Comparative Example 1 The positive electrode active material 0.5Li 2 MnO 3 -0.5LiNi 0.625 Mn 0.375 O 2 was used as the active material of Comparative Example 1 without performing ammonium sulfate treatment.
  • positive electrodes were prepared using the five types of positive electrode active materials prepared as described above, and five types of prototype batteries were manufactured.
  • the positive electrode active material, the conductive additive, and the binder were weighed so as to have a weight ratio of 85: 10: 5 and mixed uniformly to prepare a positive electrode slurry.
  • the positive electrode slurry was applied on an aluminum current collector foil having a thickness of 15 ⁇ m, dried at 120 ° C., and compression-molded so as to have an electrode density of 2.0 g / cm 3 with a press to obtain an electrode plate. Thereafter, the electrode plate was punched into a disk shape having a diameter of 15 mm to produce a positive electrode.
  • the negative electrode was produced using metallic lithium.
  • a solution obtained by dissolving LiPF 6 at a concentration of 1.0 mol / L in a mixed solvent of ethylene carbonate and dimethyl carbonate having a volume ratio of 1: 2 was used.
  • Table 1 summarizes the Raman spectroscopic measurement results (I 430 / I 600 , I 660 / I 600 ), 1 st discharge capacity, Coulomb efficiency (%), and capacity retention rate at the 60th cycle for five positive electrode active materials.
  • Li 2 MnO 3 has a high resistance, and it is easy to release oxygen from the surface during the first charge, and the irreversible capacity It is considered that the 1 st discharge capacity and Coulomb efficiency have been improved by removing Li 2 MnO 3 from the surface, that is, by lowering I (430) / I (600) because it is a substance that tends to increase. .
  • the capacity maintenance rate can be increased by setting I (660) / I (600) ⁇ 0.35.
  • I (660) is because the peak attributable to the Li 4 Mn 5 O 12, it is considered that the cycle characteristic is deteriorated by that there is a certain level of Li 4 Mn 5 O 12 on the surface.
  • I (600) is a layered structure and I (660) is a peak due to the spinel structure, and it is presumed that there is no direct correlation between the composition and the value of I (660) / I (600). Even when the composition range is changed, it is considered that there is a certain effect within the above numerical range.
  • M is Co, Ta, Zr, Cr, Ni, Fe, V, Al, Mg, Ti, W, etc.
  • the irreversible capacity was reduced by reducing the ratio of Li 2 MnO 3 in the surface layer portion, and the effects of improving the initial discharge capacity and Coulomb efficiency were obtained.
  • M is Co, Ta, Zr, Cr, Ni, Fe, V, Al, Mg, Ti, W, etc.
  • the positive electrode active material of the present invention can be used as a positive electrode by being slurried with various binders and conductive materials that are disclosed, and using this positive electrode, a negative electrode such as graphite or Si, and a non-aqueous electrolyte.
  • a lithium ion battery capable of increasing energy density and improving cycle characteristics can be provided.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'objectif de la présente invention est de pourvoir à un matériau actif d'électrode positive qui possède une haute capacité de décharge et un haut rendement coulombien. Un matériau actif d'électrode positive pour batteries secondaires à électrolyte non aqueux est décrit, qui est composé d'un oxyde composite de lithium qui est représenté par la formule de composition xLi2MnO3-(1-x)LiNiaMnbMcO2 (dans laquelle M représente au moins un élément choisi parmi Co, Ta, Zr, Cr, Ni, Fe, V, Al, Mg, Ti et W, et x, a, b et c représentent respectivement des nombres qui satisfont les relations suivantes: 0,2 < x < 0,8; 0,5 < a < 1; 0 < b < 0,5; 0 ≤ c < 0,05; et a + b + c =1). De plus, le rapport de l'intensité I(430), qui est l'intensité du matériau actif d'électrode positive à 430cm-1 déterminée par spectroscopie Raman, sur l'intensité I(600), qui est l'intensité du matériau actif d'électrode positive à 600cm-1 déterminée par spectroscopie Raman, satisfait I(430)/I(600) < 0,3.
PCT/JP2013/071590 2013-08-09 2013-08-09 Matériau actif d'électrode positive pour batteries secondaires à électrolyte non aqueux, électrode positive pour batteries secondaires à électrolyte non aqueux l'utilisant, et batterie secondaire à électrolyte non aqueux WO2015019483A1 (fr)

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PCT/JP2013/071590 WO2015019483A1 (fr) 2013-08-09 2013-08-09 Matériau actif d'électrode positive pour batteries secondaires à électrolyte non aqueux, électrode positive pour batteries secondaires à électrolyte non aqueux l'utilisant, et batterie secondaire à électrolyte non aqueux

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10290861B2 (en) 2015-12-18 2019-05-14 Samsung Electronics Co., Ltd. Composite positive active material, method of preparing the same, positive electrode including the composite positive active material, and lithium battery including the positive electrode

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Publication number Priority date Publication date Assignee Title
JP2009158415A (ja) * 2007-12-27 2009-07-16 Mitsui Mining & Smelting Co Ltd 非水電解液二次電池用正極活物質及びそれを有する非水電解液二次電池
JP2011029000A (ja) * 2009-07-24 2011-02-10 Nissan Motor Co Ltd リチウムイオン電池用正極材料の製造方法
WO2012111614A1 (fr) * 2011-02-18 2012-08-23 三井金属鉱業株式会社 Matériau d'électrode positive à solution solide de type lithium-manganèse

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JP2009158415A (ja) * 2007-12-27 2009-07-16 Mitsui Mining & Smelting Co Ltd 非水電解液二次電池用正極活物質及びそれを有する非水電解液二次電池
JP2011029000A (ja) * 2009-07-24 2011-02-10 Nissan Motor Co Ltd リチウムイオン電池用正極材料の製造方法
WO2012111614A1 (fr) * 2011-02-18 2012-08-23 三井金属鉱業株式会社 Matériau d'électrode positive à solution solide de type lithium-manganèse

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DENIS Y. W. YU ET AL.: "Surface Modification of Li-Excess Mn-based Cathode Materials", JOURNAL OF THE ELECTROCHEMICAL SOCIETY, vol. 157, no. 11, 7 September 2010 (2010-09-07), pages A1177 - A1182 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10290861B2 (en) 2015-12-18 2019-05-14 Samsung Electronics Co., Ltd. Composite positive active material, method of preparing the same, positive electrode including the composite positive active material, and lithium battery including the positive electrode

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