WO2019132080A1 - Matériau actif de cathode pour batterie secondaire au lithium, et batterie secondaire au lithium le comprenant - Google Patents

Matériau actif de cathode pour batterie secondaire au lithium, et batterie secondaire au lithium le comprenant Download PDF

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Publication number
WO2019132080A1
WO2019132080A1 PCT/KR2017/015757 KR2017015757W WO2019132080A1 WO 2019132080 A1 WO2019132080 A1 WO 2019132080A1 KR 2017015757 W KR2017015757 W KR 2017015757W WO 2019132080 A1 WO2019132080 A1 WO 2019132080A1
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Prior art keywords
secondary battery
lithium secondary
active material
cathode active
formula
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PCT/KR2017/015757
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English (en)
Korean (ko)
Inventor
손정수
권수연
최수안
전상훈
안지선
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주식회사 엘 앤 에프
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Priority to PCT/KR2017/015757 priority Critical patent/WO2019132080A1/fr
Publication of WO2019132080A1 publication Critical patent/WO2019132080A1/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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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 cathode active material for a lithium secondary battery and a lithium secondary battery comprising the same.
  • LiCoO 2 and LiMn 2 O 4 And so on LiCoO 2 and LiMn 2 O 4 And so on.
  • LiCoO 2 has a limitation in realizing a high capacity battery
  • LiMn 2 O 4 has a low energy density, and has a short life characteristic due to a problem of Mn ion elution.
  • the nickel-based cathode active material can realize a high capacity characteristic, but has poor thermal stability and low life characteristics at high temperature.
  • the present embodiments provide a cathode active material for a lithium secondary battery having excellent lifetime characteristics and thermal stability while securing a high capacity characteristic of the lithium secondary battery and a lithium ion battery including the same.
  • the cathode active material for a secondary battery may include a compound represented by the following general formula (1).
  • M3 is at least one element selected from the group consisting of alkaline earth metal, alkali metal, Group 3 to Group 12 metal elements and Group 13 to Group 15 elements
  • M1 is Ni x Co y Mn z
  • M2 is Ti a Zr b Mg c M3 d
  • Q comprises at least one of P and S, wherein -0.1? K? 0.1, 0.0007??? 0.05, 0??? 0.1, 0.800? X? 0.880, 0.01? Y? 0.15, 0.01? Z ? 0.199, 1.6? (A + b) / c? 10, 0? D? 0.01.
  • the lithium secondary battery according to one embodiment may include a cathode, a cathode, and an electrolyte including a cathode active material for a lithium secondary battery according to one embodiment.
  • the positive electrode active material for a secondary battery according to an embodiment of the present invention can be used in a lithium secondary battery by combining appropriate doping elements under specific conditions so that the capacity of the battery can be increased while maintaining excellent thermal stability, The lithium secondary battery having excellent lifetime characteristics can be realized.
  • the cathode active material for a lithium secondary battery may include a compound represented by the following general formula (1).
  • M3 is at least one element selected from the group consisting of alkaline earth metal, alkali metal, Group 3 to Group 12 metal elements and Group 13 to Group 15 elements
  • M1 is Ni x Co y Mn z
  • M2 is Ti a Zr b Mg c M3 d
  • Q comprises at least one of P and S, wherein -0.1? K? 0.1, 0.0007??? 0.05, 0??? 0.1, 0.800? X? 0.880, 0.01? Y? 0.15, 0.01? Z ? 0.199, 1.6? (A + b) / c? 10, 0? D? 0.01.
  • k may be -0.1 or more and 0.1 or less. Accordingly, the molar ratio of Li can be 0.9 or more and 1.1 or less. When the molar ratio of Li is less than 0.9, Ni is liable to be incorporated into the Li phase and the occupancy rate of the metal sites of the lithium site becomes large, and it is difficult to obtain a Li-Ni composite oxide capable of realizing a high capacity battery. When the molar ratio of Li is larger than 1.1, the incorporation of Li into the metal site increases, so that Ni separated from the metal site is mixed into the Li phase and the metal occupation ratio of the lithium site becomes large. Therefore, k is preferably in the above range, more specifically, 0? K? 0.05.
  • M1 may be a nickel-based lithium metal oxide having a layered structure, that is, Ni x Co y Mn z .
  • the nickel-based lithium metal oxide of this embodiment has a high molar ratio of nickel. That is, in M1 of Formula 1, the molar ratio x of nickel may be in the range of 0.800? X? 0.880, more specifically, 0.820? X? 0.860. When the molar ratio of nickel satisfies the above range, a high capacity lithium secondary battery can be realized.
  • the nickel-based lithium metal oxide includes Co and Mn, and y and z, which are contents of Co and Mn, may be in the range of 0.01? Y? 0.15 and 0.01? Z? 0.199, respectively. More specifically, y and z may be in the range of 0.05? Y? 0.15 and 0.03? Z? 0.1, respectively.
  • the structural stability of the cathode active material capable of realizing a high capacity can be improved.
  • M2 may include at least three kinds of dopants, and may further include M3 as needed. That is, M2 can be expressed as Ti a Zr b Mg c M d .
  • the total molar ratio alpha of M2, that is, a + b + c + d, may be in the range of 0.0007??? 0.05, more specifically 0.005?? 0.03 or 0.008?? 0.04.
  • a, b and c which represent the molar ratios of the respective doping elements in M2, may be 1.6? (A + b) / c? 10, more specifically 1.9? (A + b) / c? 8 or 2.6 ? (A + b) / c? 5.
  • the molar ratio of M3, which is an additional doping element may be in the range of 0? D? 0.01, more specifically, 0? D? 0.009 as necessary.
  • the structural stability and surface stabilization of the cathode active material can be improved.
  • Ti may be included in a ratio of 0.0005? A? 0.02, or 0.001? A? 0.01.
  • Ti may be included in the above ratio, it is possible to control the phase transition of the nickel-based lithium metal oxide to the irreversible region when the lithium is desorbed and inserted in the charge-discharge process.
  • the structural stability of the cathode active material can be improved by controlling the expansion of the c-axis in the nickel metal-oxide having a layered crystal structure.
  • Zr may be contained in a ratio of 0.0001? B? 0.01, or 0.0005? B? 0.005.
  • Zr is partially substituted with the transition metal located on the surface of the nickel-based lithium metal oxide particle, and an oxide containing Zr is formed on the surface of the nickel-based lithium metal oxide particle, So that stabilization of the surface can be improved.
  • Mg may be contained in a ratio in the range of 0.0001? C? 0.01, or 0.001? C? 0.005.
  • Mg is contained in the above ratio, cation mixing between lithium and nickel in the lithium layer of the nickel-based lithium metal oxide having the layered crystal structure can be suppressed. Accordingly, by improving the structural stability of the cathode active material, a lithium secondary battery having improved capacity and life characteristics at the same time can be realized.
  • M3 is a dopant other than M1 and M2 described above and may include at least one of an alkaline earth metal, an alkali metal, a Group 3 to Group 12 metal element, and a Group 13 to Group 15 element.
  • M3 may be Al, B, P, S, Mo, V, W, Ca, Na, Zn, Cr, Fe, Cu, Ru, Sr, Be, Si, Ge, Ba, , Ta, Ga, Os, As, and Sb.
  • the C may include at least one of Al and B.
  • M3 may include both Al and B.
  • the molar ratio of Al may be in a range of 0.001? Al? 0.01, more specifically 0.002? Al? 0.01.
  • the molar ratio of B may be in the range of 0.0001? B? 0.001, more specifically, 0.0005? B? 0.001.
  • B is confirmed to be related to the densification of the positive electrode active material particles.
  • B is contained in the above-mentioned ratio, the inter-primary-particle bonding of the above-mentioned nickel-based lithium oxide is made robust, And the ion conductivity can be improved.
  • the compound represented by Formula 1 may have I (003/104) of 1.8 or more, more specifically 1.8 or more and 2 or less, as measured by X-ray diffraction analysis using a CuK? Ray.
  • the positive electrode active material has a layered crystal structure containing no lithium excess phase
  • substitution of lithium contained in the transition metal that is, cation mixing, between the transition metal contained in the transition metal layer and the lithium layer occurs, .
  • the peak intensity ratio I (003/104) of the XRD measurement results can be used, and generally, the larger the I (003/104), the less the cationic mixing is.
  • the diffraction peak of the (003) plane is inherent to the layered crystal structure, and the diffraction peak of the (104) plane is measured not only in the layered crystal structure but also in the cubic crystal structure. Therefore, the larger the I (003/104), the closer to the single phase of the layered crystal structure. That is, the crystallinity of the nickel-based lithium metal oxide is improved.
  • the I (003/104) range of the compound represented by Formula 1 is as described above. I (003/104) satisfies the above range, the lithium secondary battery using the cathode active material of this embodiment has an excellent initial capacity and can improve lifetime characteristics at room temperature and high temperature environment.
  • the cathode active material for a lithium secondary battery according to one embodiment described above can be usefully used for the anode of a lithium secondary battery. That is, the lithium secondary battery according to an embodiment of the present invention includes a cathode and an anode including the above-described cathode active material and an electrolyte.
  • the lithium secondary battery according to an embodiment of the present invention may include an electrode assembly including a cathode, a cathode, and a separator disposed between the anode and the cathode.
  • the negative electrode may be prepared by preparing a composition for forming a negative electrode active material layer by mixing a negative electrode active material, a binder and a conductive material, and then applying the composition to an anode current collector such as copper.
  • the negative electrode active material a material capable of intercalating / deintercalating lithium is used.
  • the negative active material include lithium metal, lithium alloy, coke, artificial graphite, natural graphite, Lt; / RTI >
  • binder examples include polyvinyl alcohol, carboxymethylcellulose / styrene-butadiene rubber, hydroxypropylene cellulose, diacetylene cellulose, polyvinyl chloride, polyvinylpyrrolidone, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene Polypropylene and the like can be used, but the present invention is not limited thereto.
  • the binder may be mixed in an amount of 1 to 30% by weight based on the total amount of the composition for forming the negative electrode active material layer.
  • the conductive material is not particularly limited as long as it has electrical conductivity without causing chemical changes in the battery, and specifically includes graphite such as natural graphite and artificial graphite; Carbon black such as acetylene black, ketjen black, channel black, furnace black, lamp black, and summer black; Conductive fibers such as carbon fiber and metal fiber; Metal powders such as carbon fluoride, aluminum, and nickel powder; Conductive whiskey such as zinc oxide and potassium titanate; Conductive metal oxides such as titanium oxide; Conductive materials such as polyphenylene derivatives and the like can be used.
  • the conductive material may be mixed in an amount of 0.1 to 30% by weight based on the total amount of the composition for forming the anode active material layer.
  • the anode includes the cathode active material for a lithium secondary battery according to an embodiment. That is, the cathode active material, the binder and optionally the conductive material may be mixed to prepare a composition for forming a cathode active material layer, and then the composition may be applied to a cathode current collector such as aluminum. Further, the conductive material, binder and solvent are used in the same manner as in the case of the above-mentioned anode.
  • a non-aqueous electrolyte or a known solid electrolyte may be used, and a lithium salt dissolved therein may be used.
  • the lithium salt may be, for example, LiPF 6 , LiBF 4 , LiSbF 6 , LiAsF 6 , LiClO 4 , LiCF 3 SO 3 , Li (CF 3 SO 2 ) 2 N, LiC 4 F 9 SO 3 , LiSbF 6 , LiAlO 4 , LiAlCl 4 , LiCl, and LiI may be used.
  • Examples of the solvent of the non-aqueous electrolyte include cyclic carbonates such as ethylene carbonate, propylene carbonate, butylene carbonate, and vinylene carbonate; Chain carbonates such as dimethyl carbonate, methyl ethyl carbonate and diethyl carbonate; Esters such as methyl acetate, ethyl acetate, propyl acetate, methyl propionate, ethyl propionate and?
  • a gelated polymer electrolyte in which an electrolyte solution is impregnated with a polymer electrolyte such as polyethylene oxide or polyacrylonitrile, or an inorganic solid electrolyte such as LiI or Li 3 N can be used.
  • a polymer electrolyte such as polyethylene oxide or polyacrylonitrile
  • an inorganic solid electrolyte such as LiI or Li 3 N
  • the separator may be an olefin-based polymer such as polypropylene, which is chemically resistant and hydrophobic; A sheet or a nonwoven fabric made of glass fiber, polyethylene or the like can be used.
  • a solid electrolyte such as a polymer is used as the electrolytic solution, the solid electrolytic solution may also serve as a separation membrane.
  • the 1Mn 0 .06 (OH) 2 the lithium source material LiOH, Ti raw material is TiO 2, Zr source material is ZrO 2, and Mg raw material of Mg (OH) 2, were mixed in a dry process.
  • the material thus obtained was pulverized and classified to prepare a cathode active material of Example 1 having an average particle diameter of 10 mu m.
  • the slurry was uniformly applied to an aluminum (Al) current collector, and then NMP was evaporated through hot air drying.
  • the slurry was compressed by a roll press and then vacuum dried in a vacuum oven at 100 ° C to 200 ° C for 12 hours to prepare a positive electrode.
  • Lithium metal Li-metal
  • LiPF 6 LiPF 6
  • EC ethylene carbonate: DMC: Dimethyl Carbonate
  • a CR2032 half-cell was fabricated according to a conventional manufacturing method.
  • Example 1 0.82812 0.09859 0.05915 0.00877 0.00153 0.00384 - - 2.682 1.8358
  • Example 2 0.82855 0.09864 0.05918 0.00877 0.00102 0.00384 - - 2.549 1.8229
  • Example 3 0.82893 0.09868 0.05921 0.00877 0.00153 0.00288 - - 3.576 1.8168
  • Example 4 0.82304 0.09798 0.05879 0.00877 0.00153 0.00384 0.00519 0.00086 2.682 1.8621
  • Example 5 0.83055 0.09888 0.05933 0.00586 0.00154 0.00384 - - 1.922 1.8168
  • Example 6 0.82376 0.09807 0.05884 0.00877 0.00153 0.00384 0.00519 - 2.682 1.8638
  • Example 7 0.82740 0.09850 0.05910 0.00877 0.00153 0.00
  • the lithium secondary batteries produced according to Examples 1 to 5 and Comparative Examples 1 to 3 were evaluated for forming efficiency.
  • the lithium secondary batteries produced according to Examples 1 to 5 and Comparative Examples 1 to 3 were repeatedly charged and discharged at a high temperature (45 ° C) of 3.0 V to 4.3 V and a charging of 1.0 C and a discharge of 1.0 C 30 th / 1 th capacity retention rate (30th cycle capacity with respect to the first cycle capacity) was calculated and shown in Table 2 below.
  • the measurement range was 30 ⁇ ⁇ to 400 ⁇ ⁇ .
  • Example 1 213.95 94.69 90.31 223.5
  • Example 2 213.07 92.01 87.75 -
  • Example 3 212.59 93.86 89.53 -
  • Example 4 213.95 93.69 91.31 226.82
  • Example 5 215.43 92.64 89.93 -
  • Example 6 214.12 93.72 90.28 225.17
  • Example 7 213.23 92.15 90.15 224.37 Comparative Example 1 216.33 91.30 87.57 - Comparative Example 2 207.24 91.11 87.5 - Comparative Example 3 211.62 91.47 82.93 -
  • cathode active materials prepared according to Examples 1, 4, and 6 to 7 are also excellent in thermal stability.
  • a cathode active material doped to contain Ti, Zr and Mg at a specific molar ratio is employed as in the present embodiment, a high capacity characteristic can be secured, and at the same time, lithium having excellent lifetime characteristics and thermal stability at room temperature and high temperature A secondary battery can be realized.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

La présente invention concerne un matériau actif de cathode pour une batterie secondaire au lithium, son procédé de préparation et une batterie secondaire au lithium le comprenant. Un matériau actif de cathode pour une batterie secondaire au lithium, selon un mode de réalisation, peut comprendre un composé représenté par la formule chimique suivante 1. [Formule chimique 1] Li1+k[M11-α M2α]O2-βQβ. Dans la formule chimique 1, M1 est NixCoyMnz, M2 est TiaZrbMgcM3d, M3 comprend au moins l'un parmi un métal alcalino-terreux, un métal alcalin, un élément métallique des groupes 3 à 12, et un élément des groupes 13 à 15, et Q comprend au moins l'un de P et S, où -0,1 ≤ k ≤ 0,1, 0,0007≤ α ≤ 0,05, 0 ≤ β ≤ 0,1, 0,800 ≤ x ≤ 0,880, 0,01 ≤ y ≤ 0,15, 0,01 ≤ z ≤ 0,199, 1,6 ≤ (a+b)/c ≤ 10, et 0 ≤ d ≤ 0,01.
PCT/KR2017/015757 2017-12-29 2017-12-29 Matériau actif de cathode pour batterie secondaire au lithium, et batterie secondaire au lithium le comprenant WO2019132080A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101601917B1 (ko) * 2014-02-11 2016-03-09 울산과학기술원 리튬 이차전지용 양극 활물질, 이들의 제조방법, 및 이를 포함하는 리튬 이차전지
KR20170045833A (ko) * 2015-10-20 2017-04-28 주식회사 엘지화학 다층 구조의 금속 산화물들을 포함하는 양극 활물질 제조용 전구체 및 이를 사용하여 제조된 리튬 이차전지용 양극 활물질
KR101746187B1 (ko) * 2014-10-15 2017-06-12 주식회사 포스코 리튬 이차 전지용 양극 활물질, 및 이를 포함하는 리튬 이차 전지
KR20170119691A (ko) * 2015-03-31 2017-10-27 난통 리샤인 뉴 머티리얼 컴퍼니 리미티드 고용량 니켈-코발트계 리튬이온 양극재 및 그 제조 방법
KR20170133188A (ko) * 2016-05-25 2017-12-05 주식회사 엘 앤 에프 양극 활물질, 이의 제조방법 및 이를 포함하는 리튬 이차 전지

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101601917B1 (ko) * 2014-02-11 2016-03-09 울산과학기술원 리튬 이차전지용 양극 활물질, 이들의 제조방법, 및 이를 포함하는 리튬 이차전지
KR101746187B1 (ko) * 2014-10-15 2017-06-12 주식회사 포스코 리튬 이차 전지용 양극 활물질, 및 이를 포함하는 리튬 이차 전지
KR20170119691A (ko) * 2015-03-31 2017-10-27 난통 리샤인 뉴 머티리얼 컴퍼니 리미티드 고용량 니켈-코발트계 리튬이온 양극재 및 그 제조 방법
KR20170045833A (ko) * 2015-10-20 2017-04-28 주식회사 엘지화학 다층 구조의 금속 산화물들을 포함하는 양극 활물질 제조용 전구체 및 이를 사용하여 제조된 리튬 이차전지용 양극 활물질
KR20170133188A (ko) * 2016-05-25 2017-12-05 주식회사 엘 앤 에프 양극 활물질, 이의 제조방법 및 이를 포함하는 리튬 이차 전지

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