WO2021039063A1 - 二次電池 - Google Patents

二次電池 Download PDF

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Publication number
WO2021039063A1
WO2021039063A1 PCT/JP2020/024532 JP2020024532W WO2021039063A1 WO 2021039063 A1 WO2021039063 A1 WO 2021039063A1 JP 2020024532 W JP2020024532 W JP 2020024532W WO 2021039063 A1 WO2021039063 A1 WO 2021039063A1
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Prior art keywords
positive electrode
additional layer
transition metal
secondary battery
layer
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PCT/JP2020/024532
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English (en)
French (fr)
Japanese (ja)
Inventor
聡 澁谷
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Panasonic Intellectual Property Management Co Ltd
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Panasonic Intellectual Property Management Co Ltd
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Priority to JP2021542042A priority Critical patent/JP7496521B2/ja
Priority to CN202080059460.5A priority patent/CN114270573B/zh
Priority to US17/637,537 priority patent/US12341180B2/en
Priority to EP20857188.5A priority patent/EP4024502A4/en
Publication of WO2021039063A1 publication Critical patent/WO2021039063A1/ja
Anticipated expiration legal-status Critical
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/664—Ceramic materials
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/665—Composites
    • H01M4/667—Composites in the form of layers, e.g. coatings
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 secondary battery technology.
  • a non-aqueous electrolyte secondary battery having a positive electrode, a negative electrode, and an electrolyte and charging / discharging by moving lithium ions between the positive electrode and the negative electrode is widely used.
  • Patent Document 1 includes, as a positive electrode for a non-aqueous electrolyte secondary battery, a positive electrode current collector, a protective layer formed on the positive electrode current collector, and a lithium-containing transition metal oxide on the protective layer.
  • the protective layer contains an inorganic compound having a thickness of 1 ⁇ m to 5 ⁇ m and having a lower oxidizing power than the lithium-containing transition metal oxide, and a conductive material, comprising a positive electrode mixture layer formed in the above.
  • a positive electrode for an electrolyte secondary battery is disclosed.
  • Patent Document 2 describes a secondary battery including a positive electrode and a negative electrode, wherein the positive electrode includes a positive electrode current collector and a positive electrode mixture layer held by the positive electrode current collector, and the positive electrode mixture is provided.
  • the layer has a first positive electrode mixture layer formed on the positive electrode current collector and a second positive electrode mixture layer covering the first positive electrode mixture layer, and the first positive electrode mixture layer is a layer.
  • the secondary battery discloses that the second positive electrode mixture layer contains a first positive electrode active material capable of releasing oxygen when overcharged, and the second positive electrode mixture layer contains a second positive electrode active material having higher moisture resistance than the first positive electrode active material. Has been done.
  • a secondary battery when an internal short circuit occurs due to the piercing of a foreign substance (for example, a metal object such as a nail), the battery may generate heat and become hot.
  • a foreign substance for example, a metal object such as a nail
  • an object of the present disclosure is to provide a secondary battery capable of suppressing an increase in battery temperature when an internal short circuit occurs due to the piercing of a foreign substance.
  • the secondary battery includes a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, and the positive electrode includes a positive electrode current collector and a positive electrode.
  • a transition metal oxide containing the content of the inert material of the additional layer is 60 mass% or more, basis weight of the additional layer is a 3.8 g / m 2 or more 50 g / m 2 or less ..
  • the secondary battery includes a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, and the positive electrode includes a positive electrode current collector and a positive electrode.
  • a transition metal oxide containing the content of the inert material of the additional layer is 60 mass% or more, basis weight of the additional layer is a 3.8 g / m 2 or more 50 g / m 2 or less .
  • Li-containing transition metal oxides having a crystal structure belonging to any of the space groups Fm3m, C2 / M, Immm, and P3m1 It is difficult for Li-containing transition metal oxides having a crystal structure belonging to any of the space groups Fm3m, C2 / M, Immm, and P3m1 to reversibly occlude and release chemical species that serve as charge carriers such as lithium ions.
  • the material the so-called electrochemically inert material.
  • inert materials include 60 wt% or more, an additional layer having 3.8 g / m 2 or more 50 g / m 2 or less of basis weight in the positive electrode, piercing of foreign matter (for example, a metal material such as a nail)
  • foreign matter for example, a metal material such as a nail
  • the additional layer becomes a resistance component, and the amount of current flowing between the positive electrode and the negative electrode through the foreign matter is suppressed.
  • the rise in battery temperature when an internal short circuit occurs due to the piercing of a foreign substance is suppressed.
  • the secondary battery is a power storage device that can be repeatedly charged and discharged, for example, a non-aqueous electrolyte secondary battery, an aqueous secondary battery, and the like, specifically, a lithium ion secondary battery and an alkaline secondary battery.
  • a non-aqueous electrolyte secondary battery for example, a non-aqueous electrolyte secondary battery, an aqueous secondary battery, and the like, specifically, a lithium ion secondary battery and an alkaline secondary battery.
  • the following batteries and the like can be mentioned.
  • a lithium ion secondary battery will be described as an example.
  • FIG. 1 is a cross-sectional view of a lithium ion secondary battery which is an example of the embodiment.
  • a winding type electrode body 14 in which a positive electrode 11 and a negative electrode 12 are wound via a separator 13, an electrolyte, and above and below the electrode body 14, respectively, are arranged.
  • the insulating plates 18 and 19 and a battery case 15 for accommodating the above members are provided.
  • the battery case 15 is composed of a bottomed cylindrical case body 16 and a sealing body 17 that closes an opening of the case body 16.
  • the winding type electrode body 14 instead of the winding type electrode body 14, other forms of electrode bodies such as a laminated type electrode body in which positive electrodes and negative electrodes are alternately laminated via a separator may be applied.
  • the battery case 15 include a metal case such as a cylinder, a square, a coin, and a button, and a resin case (laminated battery) formed by laminating a resin sheet.
  • the case body 16 is, for example, a bottomed cylindrical metal container.
  • a gasket 28 is provided between the case body 16 and the sealing body 17 to ensure the airtightness inside the battery.
  • the case body 16 has, for example, an overhanging portion 22 that supports the sealing body 17 with a part of the side surface overhanging inward.
  • the overhanging portion 22 is preferably formed in an annular shape along the circumferential direction of the case main body 16, and the sealing body 17 is supported on the upper surface thereof.
  • the sealing body 17 has a structure in which a filter 23, a lower valve body 24, an insulating member 25, an upper valve body 26, and a cap 27 are laminated in this order from the electrode body 14 side.
  • Each member constituting the sealing body 17 has, for example, a disk shape or a ring shape, and each member except the insulating member 25 is electrically connected to each other.
  • the lower valve body 24 and the upper valve body 26 are connected to each other at their central portions, and an insulating member 25 is interposed between the peripheral portions thereof.
  • the lower valve body 24 When the internal pressure of the lithium ion secondary battery 10 rises due to heat generated by an internal short circuit or the like, for example, the lower valve body 24 is deformed and broken so as to push the upper valve body 26 toward the cap 27 side, and the lower valve body 24 and the upper valve body are broken. The current path between 26 is cut off. When the internal pressure further rises, the upper valve body 26 breaks and gas is discharged from the opening of the cap 27.
  • the positive electrode lead 20 attached to the positive electrode 11 extends to the sealing body 17 side through the through hole of the insulating plate 18, and the negative electrode lead 21 attached to the negative electrode 12 is the insulating plate. It extends to the bottom side of the case body 16 through the outside of 19.
  • the positive electrode lead 20 is connected to the lower surface of the filter 23, which is the bottom plate of the sealing body 17, by welding or the like, and the cap 27, which is the top plate of the sealing body 17 electrically connected to the filter 23, serves as the positive electrode terminal.
  • the negative electrode lead 21 is connected to the inner surface of the bottom of the case body 16 by welding or the like, and the case body 16 serves as a negative electrode terminal.
  • the positive electrode 11, the negative electrode 12, the non-aqueous electrolyte, and the separator 13 will be described in detail below.
  • FIG. 2 is a cross-sectional view showing an example of a positive electrode used in the secondary battery of the present embodiment.
  • the positive electrode 11 shown in FIG. 2 includes a positive electrode current collector 30, a positive electrode mixture layer 32 arranged on the positive electrode current collector 30, and an additional layer 34 arranged on the positive electrode mixture layer 32.
  • a separator (not shown) is arranged on the additional layer 34. That is, in the positive electrode 11 shown in FIG. 2, the additional layer 34 is located between the positive electrode mixture layer 32 and the separator.
  • the position of the additional layer 34 is not particularly limited. For example, as shown in FIG. 3, the additional layer 34 is arranged on the positive electrode current collector 30, and the positive electrode mixture layer 32 is arranged on the additional layer 34. You may.
  • the additional layer 34 may be located between the positive electrode current collector 30 and the positive electrode mixture layer 32. Further, for example, as shown in FIG. 4, the additional layer 34 is located between the positive electrode mixture layer 32 arranged on the positive electrode current collector 30 side and the positive electrode mixture layer 32 arranged on the separator side. May be good.
  • the additional layer 34 and the positive electrode mixture layer 32 may be provided only on one surface of the positive electrode current collector 30, or may be provided on both sides of the positive electrode current collector 30.
  • the positive electrode current collector 30 a metal foil such as aluminum that is stable in the potential range of the positive electrode, a film in which the metal is arranged on the surface layer, or the like can be used.
  • the thickness of the positive electrode current collector 30 is preferably in the range of, for example, 1 ⁇ m or more and 20 ⁇ m or less.
  • the positive electrode mixture layer 32 preferably contains a positive electrode active material, and further contains a binder, a conductive material, and the like.
  • the thickness of the positive electrode mixture layer 32 is preferably in the range of, for example, 20 ⁇ m or more and 100 ⁇ m or less.
  • the positive electrode active material is a material capable of reversibly occluding and releasing chemical species that serve as charge carriers such as lithium ions.
  • the crystal structure belonging to the space group R-3m (the crystal structure of the space group R-3m is a layered structure).
  • Such as a lithium transition metal oxide Such as a lithium transition metal oxide.
  • the metal elements constituting the lithium-containing transition metal oxide used as the positive electrode active material are, for example, cobalt (Co), nickel (Ni), manganese (Mn), magnesium (Mg), aluminum (Al), and calcium (Ca).
  • the crystal structure of the positive electrode active material is specified by the peak seen in the diffraction pattern obtained when X-ray diffraction (XRD) measurement is performed.
  • the X-ray diffraction pattern is obtained by a powder X-ray diffraction method under the following conditions using a powder X-ray diffractometer (manufactured by Rigaku Co., Ltd., trade name "RINT-TTR", radiation source Cu-K ⁇ ).
  • the conductive material contained in the positive electrode mixture layer 32 include carbon powders such as carbon black, acetylene black, ketjen black, and graphite. These may be used alone or in combination of two or more. May be used.
  • binder contained in the positive electrode mixture layer 32 examples include fluororesins such as polytetrafluoroethylene (PTFE) and polyvinylidene fluoride (PVdF), PAN, polyimide resins, acrylic resins, and polyolefin resins. Can be used. These may be used alone or in combination of two or more.
  • fluororesins such as polytetrafluoroethylene (PTFE) and polyvinylidene fluoride (PVdF), PAN, polyimide resins, acrylic resins, and polyolefin resins.
  • the additional layer 34 preferably contains an inert material, and further contains a conductive material, a binder, and the like.
  • the thickness of the additional layer 34 is preferably in the range of 1 ⁇ m or more and 5 ⁇ m or less, for example.
  • the conductive material the same conductive material as that used for the positive electrode mixture layer 32 can be used.
  • the binder the same binder as that used for the positive electrode mixture layer 32 can be used.
  • the inert material is a Li-containing transition metal oxide having a crystal structure belonging to any of the space groups Fm3m, C2 / M, Immm, and P3m1.
  • the Li-containing transition metal oxide is a material in which it is difficult to reversibly occlude and release chemical species that serve as charge carriers such as lithium ions, and is preferably 2.5V to 4.2V (vs. Li /). It is a material that cannot occlude and release lithium ions reversibly in the potential range of Li +).
  • the crystal structure of the Inactive Material is identified by the peaks found in the diffraction pattern obtained when X-ray diffraction (XRD) measurements are taken. The conditions for XRD measurement are as described above.
  • the inert material is a Li-containing transition metal having a crystal structure belonging to the space group Fm3m and containing Fe or Mn as a main component as a transition metal in that the additional layer 34 can sufficiently function as a resistance component at the time of internal short circuit.
  • the oxide and the transition metal may contain at least one of Li-containing transition metal oxides having Cu or Ni as a main component and having a crystal structure belonging to any of the space groups C2 / M, Immm, and P3m1. preferable.
  • the main component of the transition metal means the transition metal contained most in the Li-containing transition metal oxide.
  • the inert material is represented by Li x F y M 1-y O 2 (0.5 ⁇ x ⁇ 1.5, 0.5 ⁇ y ⁇ 1, M is a transition metal other than Fe), and is a space group.
  • Li-containing transition metal oxide belonging to Fm3m represented by Li x Mn y M 1-y O 2 (0.5 ⁇ x ⁇ 1.5, 0.5 ⁇ y ⁇ 1, M is a transition metal other than Mn)
  • Li-containing transition metal oxide belonging to the space group Fm3m Li x Cu y M 1-y O 2 (0.5 ⁇ x ⁇ 1.5, 0.5 ⁇ y ⁇ 1, M is a transition metal other than Cu) in expressed, space group C2 / M, Immm, Li-containing transition metal oxide having a crystal structure belonging to any one of P3m1, and Li x Ni y M 1-y O 2 (0.5 ⁇ x ⁇ 1.5 , 0.5 ⁇ y ⁇ 1, M is a transition metal other than Ni), and at least one of the
  • the content of the inert material in the additional layer 34 may be 60% by mass or more, but more preferably 90% by mass or more. If the content of the inert material in the additional layer 34 is less than 50% by mass, the additional layer 34 does not function sufficiently as a resistance component when an internal short circuit occurs due to the piercing of a foreign substance, resulting in an internal short circuit. The rise in battery temperature when it occurs cannot be sufficiently suppressed.
  • the upper limit of the content of the inert material in the additional layer 34 is not particularly limited.
  • the additional layer 34 may contain a positive electrode active material. The content of the positive electrode active material in the additional layer 34 is not particularly limited as long as it does not impair the effect of the present disclosure of suppressing an increase in battery temperature when an internal short circuit occurs, but for example.
  • the positive electrode mixture layer 32 may contain an inert material.
  • the content of the inert material in the positive electrode mixture layer 32 is preferably such that the decrease in battery capacity is not caused, for example, preferably 2% by mass or less, and preferably 1% by mass or less. More preferred.
  • Basis weight of the additional layer 34 is sufficient if 3.8 g / m 2 or more 50 g / m 2 or less, it is preferred preferably at 7 g / m 2 or more and 20 g / m 2 or less. If the basis weight of the additional layer 34 is less than 3.8 g / m 2 , when an internal short circuit occurs due to the piercing of a foreign substance, the additional layer 34 does not function sufficiently as a resistance component and an internal short circuit occurs. The rise in battery temperature cannot be sufficiently suppressed. Further, when the basis weight of the additional layer 34 is more than 50 g / m 2 , the electric resistance of the positive electrode 11 increases and the battery capacity in the normal state decreases.
  • the additional layer 34 is located between the positive electrode mixture layer 32 and the separator among the positions shown in FIGS. 2 to 4 (FIG. 2). According to the position of the additional layer 34 shown in FIG. 2, the current collection between the positive electrode current collector 30 and the positive electrode mixture layer 32 is not hindered by the additional layer 34, so that the decrease in battery capacity is suppressed.
  • the porosity of the additional layer 34 is preferably 25% or more and 55% or less, and 30% or more and 50% or less. Is more preferable. If the porosity of the additional layer 34 is less than 25%, it becomes difficult for the electrolyte to penetrate into the positive electrode mixture layer 32, and the battery capacity may decrease. Further, when the porosity of the additional layer 34 exceeds 55%, it may not be possible to suppress an increase in the battery temperature when an internal short circuit occurs, as compared with the case where the porosity of the additional layer 34 is 55% or less.
  • the additional layer 34 is located between the positive electrode current collector 30 and the positive electrode mixture layer 32 (FIG.
  • the porosity is preferably, for example, 70% or more and 87% or less in terms of reducing the battery capacity, suppressing an increase in the battery temperature when an internal short circuit occurs, and the like.
  • the porosity of the additional layer 34 is calculated by the following formula.
  • Porosity (%) of additional layer 34 100- [[W ⁇ (d ⁇ ⁇ )] ⁇ 100]
  • W Metsuke amount of additional layer (g / cm 2 )
  • d Thickness of additional layer (cm)
  • ⁇ Average density of additional layer (g / cm 3 )
  • the particle shape of the inert material include a spherical shape, a polyhedral shape, a needle shape, a necking shape, and the like, but when the additional layer 34 is located between the positive electrode mixture layer 32 and the separator, the inert material
  • the particle shape of the above is preferably polyhedral, needle-shaped, or necked, in that the electrolyte easily penetrates into the positive electrode mixture layer 32 and the battery capacity is improved.
  • the particle size of the inert material is, for example, preferably 5 ⁇ m or less, more preferably 1.5 ⁇ m or less, from the viewpoint of being able to more effectively suppress an increase in battery temperature when an internal short circuit occurs. ..
  • the particle size means a 50% particle size (D50) in which the integrated% with respect to the particle size is 50% in the particle size distribution measured by the laser diffraction / scattering method.
  • the additional layer 34 containing the inert material releases Li ions at the time of initial charging to form the additional layer 34 using the precursor serving as the inert material, and fills the secondary battery including the additional layer 34. It is obtained by changing the precursor into an inert material by discharging.
  • the precursor that becomes an inert material by charging include Li 5 FeO 4 , Li 6 MnO 4 , Li 2 CuO 2 , Li 2 NiO 2 , Li 2 Cu 0.6 Ni 0.4 O 2 .
  • the negative electrode 12 includes a negative electrode current collector such as a metal foil and a negative electrode mixture layer formed on the negative electrode current collector.
  • a negative electrode current collector such as a metal foil and a negative electrode mixture layer formed on the negative electrode current collector.
  • a metal foil that is stable in the potential range of the negative electrode such as copper, a film in which the metal is arranged on the surface layer, or the like can be used.
  • the negative electrode mixture layer includes, for example, a negative electrode active material, a binder, and the like.
  • the negative electrode active material contained in the negative electrode mixture layer is not particularly limited as long as it is a material capable of occluding and releasing lithium ions, and for example, a carbon material and an alloy can be formed with lithium.
  • the carbon material natural graphite, non-graphitizable carbon, graphites such as artificial graphite, cokes and the like can be used, and examples of the alloy compound include those containing at least one kind of metal capable of forming an alloy with lithium. Be done.
  • the element that can be alloyed with lithium is preferably silicon or tin, and silicon oxide or tin oxide in which these are bonded to oxygen can also be used. Further, a mixture of the above carbon material and a compound of silicon or tin can be used. In addition to the above, those having a charge / discharge potential for metallic lithium such as lithium titanate higher than those of carbon materials can also be used.
  • a fluororesin, a PAN, a polyimide resin, an acrylic resin, a polyolefin resin, or the like can be used as in the case of the positive electrode.
  • SBR styrene-butadiene rubber
  • CMC styrene-butadiene rubber
  • PAA polyacrylic acid
  • PAA-Na, PAA-K, etc., or a partially neutralized salt Polyvinyl alcohol (PVA) or the like may be used.
  • the electrolyte includes, for example, a non-aqueous solvent and an electrolyte salt dissolved in the non-aqueous solvent.
  • the electrolyte is not limited to the liquid electrolyte, and may be a solid electrolyte using a gel polymer or the like.
  • the non-aqueous solvent for example, esters, ethers, nitriles such as acetonitrile, amides such as dimethylformamide, and a mixed solvent of two or more of these can be used.
  • the non-aqueous solvent may contain a halogen substituent in which at least a part of hydrogen in these solvents is substituted with a halogen atom such as fluorine.
  • esters examples include cyclic carbonates such as ethylene carbonate (EC), propylene carbonate (PC) and butylene carbonate, dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC) and methylpropyl carbonate.
  • cyclic carbonates such as ethylene carbonate (EC), propylene carbonate (PC) and butylene carbonate, dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC) and methylpropyl carbonate.
  • Ethylpropyl carbonate chain carbonate such as methylisopropylcarbonate, cyclic carboxylic acid ester such as ⁇ -butyrolactone (GBL), ⁇ -valerolactone (GVL), methyl acetate, ethyl acetate, propyl acetate, methyl propionate (MP) ), Chain carboxylic acid esters such as ethyl propionate and ⁇ -butyrolactone.
  • GBL ⁇ -butyrolactone
  • VL ⁇ -valerolactone
  • MP methyl propionate
  • Chain carboxylic acid esters such as ethyl propionate and ⁇ -butyrolactone.
  • ethers examples include 1,3-dioxolane, 4-methyl-1,3-dioxolane, tetrahydrofuran, 2-methyltetrahexyl, propylene oxide, 1,2-butylene oxide, 1,3-dioxane, 1,4.
  • -Cyclic ethers such as dioxane, 1,3,5-trioxane, furan, 2-methylfuran, 1,8-cineole, crown ether, 1,2-dimethoxyethane, diethyl ether, dipropyl ether, diisopropyl ether, dibutyl ether , Dihexyl ether, ethyl vinyl ether, butyl vinyl ether, methyl phenyl ether, ethyl phenyl ether, butyl phenyl ether, pentyl phenyl ether, methoxy toluene, benzyl ethyl ether, diphenyl ether, dibenzyl ether, o-dimethoxybenzene, 1,2-diethoxy Chain ethers such as ethane, 1,2-dibutoxyethane, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol dibutyl
  • a fluorinated cyclic carbonate such as fluoroethylene carbonate (FEC), a fluorinated chain carbonate, a fluorinated chain carboxylic acid ester such as methyl fluoropropionate (FMP), or the like. ..
  • the electrolyte salt is preferably a lithium salt.
  • the lithium salt LiBF 4, LiClO 4, LiPF 6, LiAsF 6, LiSbF 6, LiAlCl 4, LiSCN, LiCF 3 SO 3, LiCF 3 CO 2, Li (P (C 2 O 4) F 4), LiPF 6-x (C n F 2n + 1 ) x (1 ⁇ x ⁇ 6, n is 1 or 2), LiB 10 Cl 10 , LiCl, LiBr, LiI, lithium chloroborane, lithium lower aliphatic carboxylate, Li 2 B Borates such as 4 O 7 , Li (B (C 2 O 4 ) F 2 ), LiN (SO 2 CF 3 ) 2 , LiN (C 1 F 2l + 1 SO 2 ) (C m F 2m + 1 SO 2 ) ⁇ l , M is an integer of 0 or more ⁇ and other imide salts.
  • lithium salt these may be used alone or in combination of a plurality of types.
  • LiPF 6 is preferably used from the viewpoint of ionic conductivity, electrochemical stability, and the like.
  • concentration of the lithium salt is preferably 0.8 to 1.8 mol per 1 L of the non-aqueous solvent.
  • a porous sheet having ion permeability and insulating property is used as the separator 13.
  • the porous sheet include a microporous thin film, a woven fabric, and a non-woven fabric.
  • an olefin resin such as polyethylene or polypropylene, cellulose or the like is suitable.
  • the separator 13 may be a laminate having a cellulose fiber layer and a thermoplastic resin fiber layer such as an olefin resin, or a separator 13 coated with an aramid resin or the like may be used.
  • Example 1 [Preparation of positive electrode active material] 98 parts by mass of positive electrode active material (composition: LiNi 0.88 Co 0.09 Al 0.03 O 2 ), 1 part by mass of acetylene black as a conductive material, and 1 part by mass of polyvinylidene fluoride as a binder. The mixture was mixed to prepare a slurry for a positive electrode mixture layer. Further, as a precursor, Li 5 FeO 4 (average particle size: 1 ⁇ m) was mixed at a ratio of 99 parts by mass, acetylene black at 0.5 parts by mass, and polyvinylidene fluoride at a ratio of 0.5 parts by mass to prepare a slurry for an additional layer. Prepared.
  • the slurry for the positive electrode mixture layer is applied to an aluminum foil having a thickness of 15 ⁇ m, the slurry for the additional layer is applied and dried on the coating film, and the obtained coating film is rolled to obtain positive electrodes on both sides of the aluminum foil.
  • a positive electrode was prepared in which a mixed material layer was formed and an additional layer was formed on the positive electrode mixed material layer.
  • the basis weight of the positive electrode mixture layer per one side was set to 270 g / m 2
  • the basis weight of the additional layer was set to 10 g / m 2 .
  • a negative electrode mixture slurry was prepared by mixing 98 parts by mass of the negative electrode active material (graphite), 1 part by mass of SBR, and 1 part by mass of CMC, and further adding an appropriate amount of water. Next, the negative electrode mixture slurry was applied to a copper foil having a thickness of 15 ⁇ m, and the coating film was dried. Then, the coating film was rolled to produce a negative electrode having negative electrode mixture layers formed on both sides of the negative electrode current collector.
  • Lithium hexafluorophosphate LiPF 6
  • LiPF 6 Lithium hexafluorophosphate
  • EC ethylene carbonate
  • MEC methyl ethyl carbonate
  • the positive electrode and the negative electrode were laminated so as to face each other via a separator, and wound around the positive electrode to prepare an electrode body.
  • the additional layer of the positive electrode is located between the positive electrode mixture layer and the separator (that is, the position of the additional layer is on the separator side).
  • the electrode body and the electrolytic solution were housed in a bottomed cylindrical battery case body, the electrolytic solution was injected, and then the opening of the battery case body was sealed with a gasket and a sealing body to prepare a test cell. ..
  • the test cell was charged at a constant current of 0.2 C in an environment of 25 ° C. until the battery voltage became 4.2 V, and then charged at a constant voltage until the current value became 0.02 C. Next, the battery was discharged at a constant current of 0.05 C until the battery voltage reached 2.5 V.
  • the test cell after charging and discharging was disassembled in a dry room, and a sample of an additional layer was collected. Powder X-ray diffraction measurement was performed on the collected sample under the above-mentioned conditions to obtain an X-ray diffraction pattern. As a result, a diffraction peak showing a crystal structure belonging to the space group Fm3m was confirmed. Further, as a result of composition analysis of this sample by ICP, the composition was LiFeO 2. That is, by charging and discharging the test cell, an additional layer containing LiFeO 2 having a crystal structure belonging to the space group Fm3m was formed. Further, since the Li 5 FeO 4 component was not confirmed in the sample collected from the additional layer, it is presumed that almost all of the Li 5 FeO 4 in the additional layer was converted to the above Li FeO 2 by the above charging and discharging. To.
  • Example 2 In the preparation of the slurry for the additional layer of the positive electrode, the test was carried out in the same manner as in Example 1 except that Li 6 MnO 4 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m). A cell was prepared.
  • Example 2 The test cell of Example 2 was charged and discharged in the same manner as in Example 1, and the additional layer was analyzed. As a result, an additional layer containing LiMnO 2 having a crystal structure belonging to the space group Fm3m could be formed. Further, it is presumed that almost all Li 6 MnO 4 in the additional layer was converted to the above Li MnO 2 by charging / discharging.
  • Example 3 The test was carried out in the same manner as in Example 1 except that Li 2 CuO 2 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m) in the preparation of the slurry for the additional layer of the positive electrode. A cell was prepared.
  • Example 3 The test cell of Example 3 was charged and discharged in the same manner as in Example 1, and the additional layer was analyzed. As a result, an additional layer containing LiCuO 2 having a crystal structure belonging to the space group C2 / m could be formed. Further, the charge and discharge, Li 2 CuO 2 additional layer is presumed to have been converted almost all the LiCuO 2.
  • Example 4 In the preparation of the slurry for the additional layer of the positive electrode, the test was carried out in the same manner as in Example 1 except that Li 2 NiO 2 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m). A cell was prepared.
  • Example 4 The test cell of Example 4 was charged and discharged in the same manner as in Example 1, and the additional layer was analyzed. As a result, an additional layer containing LiNiO 2 having a crystal structure belonging to the space group P3m1 could be formed. Further, the charge and discharge, Li 2 NiO 2 additional layer is presumed to have been converted almost all of the above LiNiO 2.
  • Example 5 In the preparation of the positive electrode, a test cell was prepared and charged / discharged in the same manner as in Example 1 except that the basis weight of the additional layer was set to 3.8 g / m 2.
  • Example 6 In the preparation of the positive electrode, a test cell was prepared and charged / discharged in the same manner as in Example 1 except that the basis weight of the additional layer was set to 50 g / m 2.
  • Example 7 In the preparation of the slurry for the additional layer of the positive electrode, the test was carried out in the same manner as in Example 1 except that Li 2 NiO 2 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m). A cell was prepared.
  • Example 7 The test cell of Example 7 was charged and discharged in the same manner as in Example 1 except that the battery voltage to be charged was changed to 4.1 V, and the additional layer was analyzed. As a result, an additional layer containing Li 1.4 NiO 2 having a crystal structure belonging to two kinds of space groups Immm and P3m1 could be formed. Further, it is presumed that almost all Li 2 NiO 2 in the additional layer was converted to the above Li 1.4 NiO 2 by charging and discharging.
  • Example 8 In the preparation of the slurry for the additional layer of the positive electrode, it was carried out except that Li 2 Cu 0.6 Ni 0.4 O 2 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m). A test cell was prepared in the same manner as in Example 1.
  • Example 8 The test cell of Example 8 was charged and discharged in the same manner as in Example 1, and the additional layer was analyzed. As a result, an additional layer containing LiCu 0.6 Ni 0.4 O 2 having a crystal structure belonging to the space group C2 / m could be formed. Further, the charge and discharge, Li 2 Cu 0.6 Ni 0.4 O 2 additional layer is presumed to have been converted almost all of the above LiCu 0.6 Ni 0.4 O 2.
  • Example 9 In the preparation of the positive electrode, a test cell was prepared in the same manner as in Example 1 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film. The additional layer of the positive electrode is located between the aluminum foil and the positive electrode mixture layer (that is, the position of the additional layer is on the positive electrode current collector side). The test cell of Example 9 was charged and discharged in the same manner as in Example 1.
  • Example 10 In the production of the positive electrode, a test cell was produced in the same manner as in Example 2 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film. The additional layer of the positive electrode is located between the aluminum foil and the positive electrode mixture layer (that is, the position of the additional layer is on the positive electrode current collector side). The test cell of Example 10 was charged and discharged in the same manner as in Example 2.
  • Example 11 In the preparation of the positive electrode, a test cell was prepared in the same manner as in Example 3 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film. The test cell of Example 11 was charged and discharged in the same manner as in Example 3.
  • Example 12 In the preparation of the positive electrode, a test cell was prepared in the same manner as in Example 4 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film. The test cell of Example 12 was charged and discharged in the same manner as in Example 4.
  • Example 13 In the preparation of the positive electrode, a test cell was prepared in the same manner as in Example 5 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film. The test cell of Example 13 was charged and discharged in the same manner as in Example 5.
  • Example 14 In the preparation of the positive electrode, a test cell was prepared in the same manner as in Example 6 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film. The test cell of Example 14 was charged and discharged in the same manner as in Example 6.
  • Example 15 In the preparation of the positive electrode, Li 5 FeO 4 (average particle diameter: 1 [mu] m) instead of Li 5 FeO 4 (average particle size: 0.3 [mu] m) for the use of, applying the slurry for additional layer to the aluminum foil, the coating A test cell was prepared in the same manner as in Example 1 except that the slurry for the positive electrode mixture layer was applied on the film. The test cell of Example 15 was charged and discharged in the same manner as in Example 1.
  • Example 16 In the preparation of the positive electrode, Li 5 FeO 4 (average particle diameter: 1 [mu] m) instead of Li 5 FeO 4 (average particle size: 1.5 [mu] m) for the use of, applying the slurry for additional layer to the aluminum foil, the coating A test cell was prepared in the same manner as in Example 1 except that the slurry for the positive electrode mixture layer was applied on the film. The test cell of Example 16 was charged and discharged in the same manner as in Example 1.
  • Example 1 The test was carried out in the same manner as in Example 1 except that Al 2 O 3 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m) in the preparation of the slurry for the additional layer of the positive electrode. A cell was prepared and charged / discharged.
  • Al 2 O 3 average particle size: 1 ⁇ m
  • Li 5 FeO 4 average particle size: 1 ⁇ m
  • Example 2 A test cell was prepared in the same manner as in Example 1 except that Al 2 O 3 (average particle size: 1 ⁇ m) was used instead of Li 5 FeO 4 (average particle size: 1 ⁇ m) in the preparation of the positive electrode. .. A test cell was prepared and charged / discharged in the same manner as in Example 1 except that the slurry for the additional layer was applied to the aluminum foil and the slurry for the positive electrode mixture layer was applied on the coating film.
  • Example 9 except that the basis weight of the additional layer was set to 2 g / m 2 in the production of the positive electrode, the slurry for the additional layer was applied to the aluminum foil, and the slurry for the positive electrode mixture layer was applied on the coating film.
  • a test cell was prepared in the same manner as in the above.
  • the test cell of Comparative Example 3 was charged and discharged in the same manner as in Example 1.
  • ⁇ Comparative example 4> In the preparation of the positive electrode, a test cell was prepared and charged / discharged in the same manner as in Example 1 except that the basis weight of the additional layer was set to 2 g / m 2.
  • Space group Fm3m, C2 / M, Immm, Li -containing transition metal oxide having a crystal structure belonging to any one of P3m1 include (inert materials), basis weight 3.8 g / m 2 or more 50 g / m 2 or less
  • Examples 1 to 16 using a positive electrode containing a certain additional layer include a positive electrode that does not contain the above-mentioned inert material or contains the above-mentioned inert material, but contains an additional layer having a grain size of less than 3.8 g / m 2.
  • the maximum temperature reached by the battery during the nail piercing test could be kept low. That is, it can be said that in Examples 1 to 16, the increase in battery temperature when an internal short circuit occurs due to the piercing of a foreign substance can be suppressed.
  • Example 17 Li 5 FeO 4 (average particle size: 1 ⁇ m) is 94 parts by mass, positive electrode active material (composition: LiNi 0.88 Co 0.09 Al 0.03 O 2 ) is 5 parts by mass, and acetylene black is 0.5 parts by mass.
  • Polyfluoride vinylidene was mixed at a ratio of 0.5 parts by mass to prepare a slurry for an additional layer, the slurry for an additional layer was applied to an aluminum foil, and the slurry for a positive electrode mixture layer was applied on the coating film. Except for this, a test cell was prepared in the same manner as in Example 9. The test cell of Example 17 was charged and discharged in the same manner as in Example 1.
  • Example 18 Li 5 FeO 4 (average particle size: 1 ⁇ m) is 60 parts by mass, positive electrode active material (composition: LiNi 0.88 Co 0.09 Al 0.03 O 2 ) is 29 parts by mass, and acetylene black is 0.5 parts by mass.
  • Polyfluoride vinylidene was mixed at a ratio of 0.5 parts by mass to prepare a slurry for an additional layer, the slurry for an additional layer was applied to an aluminum foil, and the slurry for a positive electrode mixture layer was applied on the coating film. Except for this, a test cell was prepared in the same manner as in Example 9. The test cell of Example 18 was charged and discharged in the same manner as in Example 1.
  • Example 17 to 18 and Comparative Example 5 The test cells after charging and discharging of Examples 17 to 18 and Comparative Example 5 were disassembled in a dry room, and a sample of an additional layer was collected. No Li 5 FeO 4 component was confirmed in the sample collected from the additional layer, and almost all of them were Li FeO 2 components. That is, the content of LiFeO 2 in the additional layer is 94% by mass in Example 17, 60% by mass in Example 18, and 40% by mass in Comparative Example 5.
  • Example 17 was at 500 ° C.
  • Example 18 was at 500 ° C.
  • Comparative Example 5 was at 630 ° C. From these results, it is necessary to increase the content of the inert material in the additional layer to 60% by mass or more in order to suppress the increase in battery temperature when an internal short circuit occurs due to the piercing of a foreign substance.

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