US20210159483A1 - Positive active material for rechargeable lithium ion battery, preparing method of the same, and rechargeable lithium ion battery comprising the same - Google Patents

Positive active material for rechargeable lithium ion battery, preparing method of the same, and rechargeable lithium ion battery comprising the same Download PDF

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US20210159483A1
US20210159483A1 US17/102,751 US202017102751A US2021159483A1 US 20210159483 A1 US20210159483 A1 US 20210159483A1 US 202017102751 A US202017102751 A US 202017102751A US 2021159483 A1 US2021159483 A1 US 2021159483A1
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active material
positive electrode
electrode active
lithium
lithium ion
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Sun Tai KIM
Hye Won Park
Eun Hui PARK
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Posco Future M Co Ltd
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Posco Chemical Co Ltd
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/06—Sulfates; Sulfites
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C01B17/24—Preparation by reduction
    • C—CHEMISTRY; METALLURGY
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    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
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    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
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    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
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    • 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
    • C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
    • H—ELECTRICITY
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    • 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
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    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • H—ELECTRICITY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
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    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
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    • 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
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    • 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
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H—ELECTRICITY
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • H—ELECTRICITY
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    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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

  • aspects of embodiments of the present disclosure relate to a positive electrode active material for rechargeable lithium ion batteries, a method for preparing the positive electrode active material, and a rechargeable lithium ion battery including the positive electrode active material, and more particularly, to a positive electrode active material for rechargeable lithium ion batteries capable of reducing residual lithium impurities while forming a lithium-sulfur (Li-S) compound coating layer on a surface of the positive electrode active material through a washing process using a compound containing sulfur, thereby reducing initial resistance and leakage current generation to improve battery performance, a method for preparing the positive electrode active material, and a rechargeable lithium ion battery including the positive electrode active material.
  • Li-S lithium-sulfur
  • a rechargeable lithium ion battery (e.g., lithium secondary battery) which stores electricity using the principle of oxidation and reduction reactions of lithium has high voltage and energy density. Due to its high energy density, it has been used as a power source for small-sized electronic devices such as mobile phones, notebook computers, and digital cameras because it is advantageous in miniaturization and weight reduction compared to other rechargeable batteries (lead storage batteries, nickel cadmium, nickel hydrogen, etc.).
  • Conventional positive electrode active materials for rechargeable lithium ion batteries were prepared by mixing lithium hydroxide or lithium carbonate in a precursor, followed by heat treatment, and after this heat treatment, residual lithium hydroxide and lithium carbonate that had not participated in the reaction for preparing the positive electrode active material remained.
  • the residual lithium hydroxide increases a pH of the slurry to cause solidification phenomenon of the slurry, thereby making it difficult to prepare an electrode plate, and the residual lithium carbonate increases swelling phenomenon of the batteries, leading to cycle performance degradation and gas generation as well causing the battery to swell.
  • the lithium impurity of LiOH that remains on a surface may react with CO 2 in the atmosphere to additionally form Li 2 CO 3 , which not only increases initial irreversible capacity and interferes with movement of lithium ions on the surface, but also reacts with an electrolyte during electrochemical reaction to cause decomposition reaction in which CO 2 gas is generated, thus disadvantageously causing swelling phenomenon of the battery and high-temperature stability degradation.
  • Li in the active material may experience desorption in the process of removing residual lithium impurities, which may shorten battery life in the long-term perspective, or an active material surface may be oxidized after washing to form a NiO phase, which may reduce capacity or increase resistance, for example. Accordingly, there is a need for researches on a washing additive capable of removing the residual Li impurities to a desired level, while minimizing problems such as a decrease in the capacity of the active material due to washing.
  • Embodiments of the present disclosure are directed to a positive electrode (e.g., cathode) active material prepared by using a compound containing sulfur added in a washing (e.g., water-washing) process for removing residual lithium impurities (Li 2 CO 3 and LiOH) that are present on a surface of the active material to form a Li—S coating layer on the surface of the positive electrode active material (e.g., high-nickel positive electrode active material) containing 80 mol % or more of Ni, thereby minimizing problems such as decreased capacity of the active material due to washing and effectively removing residual lithium impurities, while improving resistance and leakage current as well, and to a method of preparing the positive electrode active material.
  • a washing e.g., water-washing
  • Embodiments of the present disclosure are also directed to a rechargeable lithium ion battery including the positive electrode active material according to an embodiment of the present disclosure.
  • a positive electrode active material for rechargeable lithium ion batteries includes: a lithium metal oxide active material; and a coating layer on a surface of the active material, wherein the coating layer includes a sulfur compound.
  • the lithium metal oxide active material as a core may be represented by the following Chemical Formula 1:
  • the above range is only an example of the present application, and the present disclosure is not limited thereto).
  • the positive electrode active material may include a core and a coating layer, where the core is a lithium metal oxide, the coating layer includes sulfur, and a sulfur compound in the coating layer includes a lithium sulfur oxide and/or a sulfur compound.
  • the positive electrode active material may include a coating layer including a lithium sulfur oxide and a sulfur compound.
  • the lithium sulfur compound in the positive electrode active material, may be Li 2 S, Li 2 SO 4 , and Li 2 SnO x (where n is 1 ⁇ n ⁇ 8).
  • contents thereof may vary depending on type and amount of the sulfur compound to be treated, but specifically, the Li 2 SO 4 compound may be included in an amount ranging from 70 percent by weight (wt %) to 99 wt %, the Li 2 S compound may be included in an amount ranging from 5 wt % to 10 wt %, and the remaining sulfur compounds Li 2 S, Li 2 S 4 , Li 2 S 6 , Li 2 S 8 and Li 2 SO n (where n is 1 ⁇ n ⁇ 8 except Li 2 SO 4 ) may be included in an amount ranging from 0 wt % to 5 wt %. No specific change in battery characteristics according to the change in weight ratio of the sulfur compounds has been reported.
  • an added amount of the sulfur compound is specifically in a range from 0.5 wt % to 5.0 wt %.
  • the amount of sulfur compound is less than 0.5 wt %, residual Li reduction effects and coating effects are insufficient, and when the amount of sulfur compound is more than 5.0 wt %, a sulfur level increases higher than a certain value (more than 1000 ppm), such that a side reaction with an electrolyte solution may be caused and battery life performance may be degraded. Accordingly, it is advantageous to proceed with the coating with the addition amount within the above range.
  • a specific reaction formula for reducing residual lithium impurities of the sulfur compound is as follows.
  • Sulfur compound of M z S x O y (x ranges from 1 to 8, y ranges from 1 to 8, M is Na or K, z ranges from 0 to 3) may react with the residual lithium impurities (Li 2 CO 3 and LiOH) through a substitution reaction and form a Li—S compound coating layer on a surface of the active material in the process of washing (e.g., water washing), thereby favorably reducing resistance and reducing leakage current generation.
  • the positive electrode active material may have a reduced initial resistance of the battery as compared to an active material without a coating layer that includes a lithium sulfur oxide and a sulfur compound.
  • a positive active material for rechargeable lithium ion batteries by adding a compound including sulfur in the process of washing, residual lithium impurities (Li 2 CO 3 and LiOH) present on a surface of a lithium metal oxide are effectively removed while a Li—S compound coating layer is formed on the surface of the lithium metal oxide.
  • the residual lithium (LiOH+Li 2 CO 3 ) of the lithium metal oxide before wet treatment may be 6,000 ppm or more. It is not that there is no effect of reducing residual lithium impurities or no effect of forming a coating layer even if the residual lithium is less than 6,000 ppm, but if the residual lithium is less than 6,000 ppm, the effect of removing residual lithium by washing may be excessive, resulting in desorption of lithium in the active material, and thus the active material performance in terms of capacity or cycles may be degraded. Accordingly, in order to achieve effective washing effects without degrading cell performance, it is preferable that the residual lithium (LiOH+Li 2 CO 3 ) of the active material is 6,000 ppm or more.
  • the positive electrode active material includes round-shaped secondary particles in which primary particles have a diameter ranging from 0.1 to 2 ⁇ m.
  • the positive electrode active material includes secondary particles formed by agglomeration of the aforementioned primary particles, and the secondary particles have a diameter ranging from 1 to 20 ⁇ m or less.
  • a method of preparing a positive electrode active material for rechargeable lithium ion batteries includes firing a precursor material and a lithium material to obtain a lithium metal oxide; dissolving a sulfur material in water to prepare a washing solution; immersing the lithium metal oxide positive electrode active material in the washing solution to wash the lithium metal oxide; and secondary heat-treating the washed lithium metal oxide positive electrode active material.
  • the method of preparing the positive electrode active material for rechargeable lithium ion batteries by dissolving of the sulfur material in water to prepare the washing solution and by immersing of the lithium metal oxide in the washing solution to wash the lithium metal oxide, residual lithium impurities may be removed while a sulfur compound coating layer may be uniformly formed on a surface.
  • the secondary heat-treating may be performed at a temperature ranging from 130° C. to less than 550° C.
  • a crystalline state may be maintained in a state that moisture of the sulfur compound is removed.
  • a structure of the sulfur compound is deformed, such that a density of the structure is lowered and a conductivity is lowered, thereby reducing the coating effect.
  • a stable temperature range for the heat treatment of the positive electrode material using the sulfur compound may be greater than 130° C. and less than 550° C.
  • FIG. 1 illustrates capacity data of washed coin cells prepared according to an embodiment using a sulfur compound and according to a comparative example, respectively.
  • FIG. 2 illustrates resistance data of washed coin cells prepared according to an embodiment using a sulfur compound and according to a comparative example, respectively.
  • FIG. 3 illustrates overcharge leakage current measurement data of washed coin cells prepared according to an embodiment using a sulfur compound and according to a comparative example, respectively.
  • FIG. 4 illustrates life characteristics and resistance increase rate data of washed coin cells prepared according to an embodiment using a sulfur compound and according to a comparative example, respectively.
  • a positive electrode (e.g., cathode) active material was prepared through the following method. After mixing a dried metal oxide precursor with LiOH, the mixture was filled in a saggar and then fired in an oxygen (O 2 ) atmosphere at a firing temperature ranging from 700 to 900° C. in a firing furnace to prepare an active material.
  • O 2 oxygen
  • a sulfur compound was added to the fired product to perform wet washing treatment so as to remove residual lithium impurities, and thus a final positive electrode active material in which the residual lithium impurities were controlled and a coating layer including Li 2 S and Li 2 SO 4 as main compounds was formed was obtained.
  • LiOH(wt %) [(2 ⁇ Q1 ⁇ Q2) ⁇ 0.1 ⁇ 23.94 ⁇ 1000/((5 ⁇ 50)/100)]
  • Li 2 CO 3 (wt %) [(Q2 ⁇ Q1) ⁇ 0.1 ⁇ 73.89 ⁇ 1000/((5 ⁇ 50)/100)]
  • a coin cell was prepared using the positive electrode plate, a lithium (Li) metal foil as a negative electrode plate, a polypropylene as a separator, and a general electrolyte (LiPF 6 salt in ethyl carbonate/ethyl-methyl carbonate/dimethyl carbonate (EC/EMC/DMC)).
  • FIG. 1 illustrates capacity results of a washed coin cell prepared using a sulfur compound and a conventional washed coin cell.
  • FIG. 2 illustrates initial resistance results at 0.2 C of a washed coin cell prepared using a sulfur compound and a conventional washed coin cell.
  • the 0.2 C initial resistance result was improved from an average of 18.5 ⁇ to 17.5 ⁇ .
  • FIG. 3 illustrates 4.7 V overcharge-120 hr-leakage current evaluation results of a washed coin cell prepared using a sulfur compound and a conventional washed coin cell.
  • FIG. 4 illustrates measurement results of 30 cyc high-temperature life characteristics and resistance increase rate of a washed coin cell prepared using a sulfur compound and a conventional washed coin cell.
  • the surface of the positive electrode active material is coated with a sulfur compound while residual lithium impurities are reduced in the process of washing, thereby improving problems such as initial resistance and leakage current during an overcharge test.

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