WO2012127920A1 - Matériau actif d'électrode de batterie secondaire, procédé de production associé, et batterie secondaire pourvue dudit matériau actif d'électrode - Google Patents

Matériau actif d'électrode de batterie secondaire, procédé de production associé, et batterie secondaire pourvue dudit matériau actif d'électrode Download PDF

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Publication number
WO2012127920A1
WO2012127920A1 PCT/JP2012/052917 JP2012052917W WO2012127920A1 WO 2012127920 A1 WO2012127920 A1 WO 2012127920A1 JP 2012052917 W JP2012052917 W JP 2012052917W WO 2012127920 A1 WO2012127920 A1 WO 2012127920A1
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Prior art keywords
active material
secondary battery
electrode active
lithium
spinel structure
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PCT/JP2012/052917
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English (en)
Japanese (ja)
Inventor
徹 川合
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株式会社 村田製作所
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Publication of WO2012127920A1 publication Critical patent/WO2012127920A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
    • 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
    • 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 generally relates to an electrode active material for a secondary battery, a method for manufacturing the same, and a secondary battery, and more specifically, for a secondary battery mainly composed of a lithium nickel manganese composite oxide having a spinel structure.
  • the present invention relates to an electrode active material, a manufacturing method thereof, and a secondary battery including an electrode including the electrode active material.
  • a secondary battery having a high energy density a secondary battery that is charged and discharged by moving lithium ions between a positive electrode and a negative electrode is used.
  • a lithium transition metal composite oxide such as lithium cobaltate (LiCoO 2 ) is generally used as a positive electrode active material.
  • a lithium transition metal composite oxide such as lithium cobaltate (LiCoO 2 )
  • LiCoO 2 lithium cobaltate
  • a lithium manganese oxide material having a spinel structure has attracted attention as a positive electrode material.
  • lithium nickel manganese composite oxide has characteristics such as high operating voltage and high energy density.
  • Patent Document 1 JP 2002-158008 A (hereinafter referred to as Patent Document 1), JP 2009-505929 A (hereinafter referred to as Patent Document 2), etc., a positive electrode material that has been actively studied in recent years. is there.
  • the inventor has found that the amount of the impurities generated in the synthesis of the lithium nickel manganese composite oxide adversely affects the charge / discharge capacity and charge / discharge rate characteristics of the secondary battery.
  • the object of the present invention is to limit the amount of impurities in the electrode active material mainly composed of lithium nickel manganese composite oxide having a spinel structure, thereby providing a large discharge capacity and good high rate charging characteristics. It is to provide a secondary battery electrode active material, a manufacturing method thereof, and a secondary battery including the same.
  • An electrode active material for a secondary battery according to the present invention is an electrode active material for a secondary battery mainly composed of a lithium nickel manganese composite oxide having a spinel structure, and the lithium nickel manganese composite having a spinel structure
  • the ratio of the main peak intensity of the (200) plane of the impurity having a rock salt type structure to the main peak intensity of the (111) plane by X-ray diffraction of the oxide is 2.0% or less and has a spinel type structure.
  • the half width of the diffraction line on the (111) plane of the lithium nickel manganese composite oxide is 0.120 ° or less.
  • the secondary battery of the present invention includes an electrode containing the above-described secondary battery electrode active material.
  • the method for producing an electrode active material for a secondary battery according to the present invention includes a mixing step of mixing a starting raw material including a lithium-containing raw material, a nickel-containing raw material, and a manganese-containing raw material, and a mixture obtained in the mixing step as a first A first firing step for firing at a temperature; and a second firing step for firing the fired product obtained in the first firing step at a second temperature lower than the first temperature.
  • the discharge capacity is large and good high rate charging characteristics are achieved.
  • a secondary battery electrode active material can be obtained.
  • the lithium nickel manganese composite oxide having the type structure and the impurities include, for example, Ni 6 MnO 8 having a rock salt type structure, Li x Ni 1-x O (0 ⁇ x ⁇ 1), and the like.
  • the ratio of the main peak intensity of the (200) plane of the impurity having the rock salt structure to the main peak intensity of the (111) plane by X-ray diffraction of the lithium nickel manganese composite oxide having a spinel structure is 2.0% or less. is there.
  • the half width of the diffraction line at the (111) plane of the lithium nickel manganese composite oxide having a spinel structure is 0.120 ° or less.
  • the discharge capacity of the secondary battery can be increased by limiting the amount of impurities not involved in the charge / discharge reaction to a small amount as represented by the ratio of the main peak intensity.
  • the half-value width of the diffraction line on the (111) plane to the above value or less and enhancing the crystallinity of the lithium nickel manganese composite oxide having a spinel structure, the insertion / extraction reaction of lithium ions Since it is performed smoothly, the high rate charging characteristics of the secondary battery can be improved. Therefore, according to the present invention, by reducing the amount of impurities having a rock salt type structure and increasing the crystallinity of the lithium nickel manganese composite oxide having a spinel type structure, the discharge capacity is large and a good high rate is obtained. An electrode active material for a secondary battery exhibiting charging characteristics can be obtained.
  • One embodiment of the secondary battery of the present invention includes a positive electrode containing the above electrode active material.
  • One embodiment of the manufacturing method of the electrode active material of the present invention as a lithium-nickel-manganese composite oxide having a spinel structure represented by the general formula Li [Ni x Mn 2-x ] O 4 (0 ⁇ x ⁇ 0. 6)
  • the method for producing an electrode active material of the present invention includes at least a mixing step of mixing a lithium-containing raw material, a nickel-containing raw material, and a manganese-containing raw material to obtain a mixture, and a firing step of firing the above mixture.
  • the firing step preferably includes first and second firing steps. In the first firing step, the mixture is fired at a first temperature, and in the second firing step, the fired product obtained in the first firing step is fired at a second temperature lower than the first temperature. Is preferred.
  • the first temperature is preferably in the range of 800 ° C to 1050 ° C.
  • the second temperature is preferably in the range of 500 ° C to 750 ° C.
  • examples of the lithium-containing raw material include lithium oxides, carbonates, inorganic acid salts, organic acid salts, and chlorides. Specifically, it is preferable to use at least one selected from lithium carbonate and lithium hydroxide as the lithium-containing raw material.
  • nickel-containing raw material examples include nickel metal, nickel oxide, carbonate, inorganic acid salt, organic acid salt, and chloride. Specifically, it is preferable to use at least one selected from metallic nickel, nickel oxide and nickel hydroxide as the nickel-containing raw material.
  • manganese-containing raw material examples include manganese oxides, carbonates, inorganic acid salts, organic acid salts, and chlorides. Specifically, it is preferable to use at least one selected from manganese dioxide, trimanganese tetraoxide, and manganese carbonate as the manganese-containing raw material.
  • the nickel-containing raw material and the manganese-containing raw material may be a composite compound of nickel and manganese, and examples of the composite compound of nickel and manganese include a composite oxide of nickel and manganese and a composite hydroxide of nickel and manganese. Specifically, it is preferable to use nickel manganese composite oxide or nickel manganese composite hydroxide having a molar ratio of Ni and Mn of 1: 1 to 1: 3.
  • the mixing method and mixing conditions in the mixing step and the baking method and baking conditions in the baking step can be arbitrarily set in consideration of required characteristics, productivity, and the like of the nonaqueous electrolyte secondary battery.
  • a lithium-containing raw material, a nickel-containing raw material, and a manganese-containing raw material are mixed and dispersed in a solvent such as water, whereby the obtained slurry is spray-dried and then fired. preferable.
  • a positive electrode is formed.
  • a positive electrode active material is mixed with a conductive agent and a binder, an organic solvent or water is added to form a positive electrode active material slurry, and this positive electrode active material slurry is applied onto the electrode current collector by an arbitrary coating method.
  • the positive electrode is formed by drying.
  • a negative electrode is formed.
  • a negative electrode active material is mixed with a conductive agent and a binder, an organic solvent or water is added to form a negative electrode active material slurry, and this negative electrode active material slurry is applied onto the electrode current collector by an arbitrary coating method.
  • the negative electrode is formed by drying.
  • the negative electrode active material is not particularly limited, but a carbon material such as spherical graphite or a lithium titanium composite oxide such as spinel type lithium titanate (Li 4 Ti 5 O 12 ) is used. Can do. Even when a lithium-titanium composite oxide having a high reference potential is used as the negative electrode active material, the effects of the present invention described above can be obtained.
  • the binder is not particularly limited, and various polymer compounds such as polyethylene, polyvinylidene fluoride, polyhexafluoropropylene, polytetrafluoroethylene, polyethylene oxide, and carboxymethylcellulose can be used.
  • the organic solvent is not particularly limited, and examples thereof include basic solvents such as dimethyl sulfoxide, dimethylformamide, N-methylpyrrolidone, propylene carbonate, diethyl carbonate, dimethyl carbonate, and ⁇ -butyrolactone, acetonitrile, tetrahydrofuran, Nonaqueous solvents such as nitrobenzene and acetone, and protic solvents such as methanol and ethanol can be used.
  • the kind of organic solvent, the compounding ratio of the organic compound and the organic solvent, the kind of additive and the amount of the additive, and the like can be arbitrarily set in consideration of the required characteristics and productivity of the secondary battery.
  • the positive electrode 14 obtained above is immersed in an electrolyte, and after impregnating the positive electrode 14 with the electrolyte, on the positive current collector at the bottom center of the case 11 that also serves as the positive electrode terminal.
  • the positive electrode 14 is placed. Thereafter, the separator 16 impregnated with the electrolyte is laminated on the positive electrode 14, the negative electrode 15 and the current collector plate 17 are sequentially laminated, and the electrolyte is injected into the internal space.
  • a metal spring member 18 is placed on the current collector plate 17, and a gasket 13 is arranged on the periphery, and a sealing plate 12 that also serves as a negative electrode terminal is fixed to the case 11 with a caulking machine or the like to seal the exterior.
  • a sealing plate 12 that also serves as a negative electrode terminal is fixed to the case 11 with a caulking machine or the like to seal the exterior.
  • the electrolyte is interposed between the positive electrode 14 and the negative electrode 15 which is a counter electrode, and transports charge carriers between the two electrodes.
  • an electrolyte one having an ionic conductivity of 10 ⁇ 5 to 10 ⁇ 1 S / cm at room temperature can be used.
  • an electrolytic solution in which an electrolyte salt is dissolved in an organic solvent can be used.
  • the electrolyte salt include LiPF 6 , LiClO 4 , LiBF 4 , LiCF 3 SO 3 , Li (CF 3 SO 2 ) 2 N, Li (C 2 F 5 SO 2 ) 2 N, Li (CF 3 SO 2 ) 3 C, Li (C 2 F 5 SO 2 ) 3 C, or the like can be used.
  • organic solvent ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, ⁇ -butyrolactone, tetrahydrofuran, dioxolane, sulfolane, dimethylformamide, dimethylacetamide, N-methyl-2-pyrrolidone, etc. are used. be able to.
  • a solid electrolyte for electrolyte.
  • the polymer compound used in the solid electrolyte include polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-ethylene copolymer, vinylidene fluoride-monofluoroethylene copolymer, and fluoride.
  • Vinylidene fluoride polymers such as vinylidene-trifluoroethylene copolymer, vinylidene fluoride-tetrafluoroethylene copolymer, vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene terpolymer, and acrylonitrile-methyl methacrylate copolymer Polymer, acrylonitrile-methyl acrylate copolymer, acrylonitrile-ethyl methacrylate copolymer, acrylonitrile-ethyl acrylate copolymer, acrylonitrile-methacrylic acid copolymer, acrylonitrile-a Examples include acrylonitrile polymers such as ryllic acid copolymers and acrylonitrile-vinyl acetate copolymers, as well as polyethylene oxide, ethylene oxide-propylene oxide copolymers, and polymers of these acrylates and methacrylates.
  • electrolyte solution contains electrolyte solution and made it gelatinous as electrolyte.
  • electrolyte salt may be used as an electrolyte as it is.
  • an electrolyte Li 2 S-P 2 S 5 based, Li 2 S-B 2 S 3 type, Li 2 and S-SiS 2 system sulfide glass represented, such as an oxide having a NASICON-type structure
  • An inorganic solid electrolyte may be used as an oxide having a NASICON-type structure.
  • the coin-type secondary battery has been described, but it is needless to say that the battery shape is not particularly limited, and can be applied to a cylindrical type, a square type, a sheet type, and the like. Also, the exterior method is not particularly limited, and a metal case, mold resin, aluminum laminate film, or the like may be used.
  • the electrode active material of the present invention is used for the positive electrode, but it can also be applied to the negative electrode.
  • Example shown below is an example and this invention is not limited to the following Example.
  • Example 1 A lithium nickel manganese composite oxide having a spinel structure was synthesized by the following method.
  • the obtained dry powder was put into a container containing alumina as a main component and fired at a temperature of 900 ° C. (first firing temperature) in an air atmosphere for 10 hours (first firing step).
  • the obtained fired product was cooled to room temperature and then pulverized in a mortar.
  • the obtained fired powder was put in a container containing alumina as a main component and fired for 20 hours at a temperature of 700 ° C. (second firing temperature) in an air atmosphere (second firing step).
  • an electrode active material composed mainly of a lithium nickel manganese composite oxide having a spinel structure was synthesized.
  • a coin-type nonaqueous electrolyte secondary battery 1 includes a case 11 that also serves as a positive electrode terminal, a sealing plate 12 that also serves as a negative electrode terminal, and a gasket 13 that insulates the case 11 and the sealing plate 12.
  • the electrode active material prepared above, acetylene black, and polyvinylidene fluoride were mixed at a mass ratio of 88: 6: 6 to prepare a positive electrode mixture.
  • This positive electrode mixture was dispersed in a solvent (N-methyl-2-pyrrolidone) to prepare a positive electrode slurry.
  • the positive electrode slurry was applied on the surface of an aluminum foil having a thickness of 20 ⁇ m at a coating amount of 7 mg / cm 2 and dried at a temperature of 140 ° C., and then pressed at a pressure of 1 ton / cm 2 to obtain a positive electrode sheet.
  • the positive electrode 14 was produced by punching this positive electrode sheet into a disk having a diameter of 12 mm.
  • the negative electrode 15 As the negative electrode 15 as a counter electrode, a disk made of a metal lithium foil having a diameter of 15.5 mm was used. A current collector plate 17 was bonded to the negative electrode 15. As the separator 16, a disk-like polyethylene porous film having a diameter of 16 mm was used.
  • the electrolytic solution an organic electrolytic solution in which 1 mol of lithium hexafluorophosphate (LiPF 6 ) was dissolved per liter of the solvent in a solvent in which ethylene carbonate and diethyl carbonate were mixed at a volume ratio of 3: 7 was used. In this way, a coin-type non-aqueous electrolyte secondary battery 1 having a diameter of 20 mm and a thickness of 3.2 mm was produced.
  • the charge / discharge characteristics were evaluated using the coin-type nonaqueous electrolyte secondary battery 1 produced as described above. In a constant temperature bath at 25 ° C., the battery was charged and discharged for 3 cycles at a current value of 0.18 mA / cm 2 and a voltage range of 3.0 to 5.0 V. The discharge capacity at the third cycle was measured and determined as “discharge capacity (0.18 mA / cm 2 ) [mAh / g]”.
  • Examples 2 to 3, Comparative Examples 1 to 3 An electrode active material was synthesized in the same manner as in Example 1 except that the molar ratio of Li in the starting material was changed as shown in Table 1, and powder X-ray diffraction measurement was performed. Using the obtained electrode active material as a positive electrode active material, a coin-type non-aqueous electrolyte secondary battery 1 was produced in the same manner as in Example 1. Using the produced coin-type non-aqueous electrolyte secondary battery 1, the charge / discharge characteristics of the battery were evaluated in the same manner as in Example 1.
  • Examples 4 to 6, Comparative Examples 4 to 6 An electrode active material was synthesized in the same manner as in Example 1 except that the molar ratio of Ni and Mn in the starting material was changed as shown in Table 1, and powder X-ray diffraction measurement was performed. Using the obtained electrode active material as a positive electrode active material, a coin-type non-aqueous electrolyte secondary battery 1 was produced in the same manner as in Example 1. Using the produced coin-type non-aqueous electrolyte secondary battery 1, the charge / discharge characteristics of the battery were evaluated in the same manner as in Example 1.
  • Examples 7 to 8, Comparative Examples 7 to 10 An electrode active material was synthesized in the same manner as in Example 1 except that the first baking temperature was changed as shown in Table 1, and powder X-ray diffraction measurement was performed. Using the obtained electrode active material as a positive electrode active material, a coin-type non-aqueous electrolyte secondary battery 1 was produced in the same manner as in Example 1. Using the produced coin-type non-aqueous electrolyte secondary battery 1, the charge / discharge characteristics of the battery were evaluated in the same manner as in Example 1.
  • the discharge capacity is large and good high rate charging characteristics are achieved.
  • a secondary battery electrode active material can be obtained.

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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)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

La présente invention concerne un matériau actif d'électrode de batterie secondaire qui possède une forte capacité de décharge et des caractéristiques de taux de charge élevé en limitant la quantité d'impuretés dans le matériau actif d'électrode, qui comporte, en tant que composant primaire, un oxyde complexe de lithium-nickel-manganèse à structure spinelle. La présente invention concerne également un procédé de production du matériau actif et une batterie secondaire pourvue du matériau actif. Le matériau actif d'électrode de batterie secondaire comporte, en tant que composant primaire, un oxyde complexe de lithium-nickel-manganèse à structure spinelle. Le rapport de la résistance maximum principale dans le plan (200) d'impuretés possédant une structure halite par rapport à la résistance maximum principale dans le plan (111) résultant d'une diffraction de rayons X de l'oxyde complexe de lithium-nickel-manganèse à structure spinelle n'est pas supérieur à 2,0 %, et la demi-largeur de bande de la ligne de diffraction dans le plan (111) de l'oxyde complexe de lithium-nickel-manganèse à structure spinelle n'est pas supérieure à 0,120°.
PCT/JP2012/052917 2011-03-18 2012-02-09 Matériau actif d'électrode de batterie secondaire, procédé de production associé, et batterie secondaire pourvue dudit matériau actif d'électrode WO2012127920A1 (fr)

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JP2011060238 2011-03-18
JP2011-060238 2011-03-18

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015174225A1 (fr) * 2014-05-12 2015-11-19 旭化成株式会社 Oxyde complexe de lithium-manganèse-nickel et son procédé de fabrication, substance active pour batterie rechargeable à électrolyte non aqueux le contenant, électrode positive, et batterie rechargeable à électrolyte non aqueux

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08298115A (ja) * 1995-04-26 1996-11-12 Japan Storage Battery Co Ltd リチウム電池用正極活物質およびその製造法
JPH11343120A (ja) * 1998-05-29 1999-12-14 Toda Kogyo Corp スピネル酸化物粒子粉末の製造方法
JP2002158007A (ja) * 2000-11-16 2002-05-31 Tanaka Chemical Corp リチウムマンガンニッケル複合酸化物およびその製造方法
JP2002316823A (ja) * 2001-02-16 2002-10-31 Tosoh Corp リチウムマンガン複合酸化物とその製造方法並びにその用途
JP2004303710A (ja) * 2003-04-01 2004-10-28 Sumitomo Metal Mining Co Ltd 非水系電解質二次電池用正極活物質およびその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08298115A (ja) * 1995-04-26 1996-11-12 Japan Storage Battery Co Ltd リチウム電池用正極活物質およびその製造法
JPH11343120A (ja) * 1998-05-29 1999-12-14 Toda Kogyo Corp スピネル酸化物粒子粉末の製造方法
JP2002158007A (ja) * 2000-11-16 2002-05-31 Tanaka Chemical Corp リチウムマンガンニッケル複合酸化物およびその製造方法
JP2002316823A (ja) * 2001-02-16 2002-10-31 Tosoh Corp リチウムマンガン複合酸化物とその製造方法並びにその用途
JP2004303710A (ja) * 2003-04-01 2004-10-28 Sumitomo Metal Mining Co Ltd 非水系電解質二次電池用正極活物質およびその製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015174225A1 (fr) * 2014-05-12 2015-11-19 旭化成株式会社 Oxyde complexe de lithium-manganèse-nickel et son procédé de fabrication, substance active pour batterie rechargeable à électrolyte non aqueux le contenant, électrode positive, et batterie rechargeable à électrolyte non aqueux
JPWO2015174225A1 (ja) * 2014-05-12 2017-04-20 旭化成株式会社 リチウムマンガンニッケル複合酸化物及びその製造方法、並びにそれを含む非水電解質二次電池用である活物質、正極及び非水電解質二次電池

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