WO2018024661A1 - Procédé de fabrication d'un matériau de cathode à faible surface bet et à masse volumique tassée élevée et matériau de cathode spécial - Google Patents

Procédé de fabrication d'un matériau de cathode à faible surface bet et à masse volumique tassée élevée et matériau de cathode spécial Download PDF

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Publication number
WO2018024661A1
WO2018024661A1 PCT/EP2017/069291 EP2017069291W WO2018024661A1 WO 2018024661 A1 WO2018024661 A1 WO 2018024661A1 EP 2017069291 W EP2017069291 W EP 2017069291W WO 2018024661 A1 WO2018024661 A1 WO 2018024661A1
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Prior art keywords
mixed oxide
general formula
surface area
bet surface
cathode material
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Ceased
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PCT/EP2017/069291
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German (de)
English (en)
Inventor
Stipan Katusic
Peter Kress
Armin Wiegand
Harald Alff
Tobias RENGER
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Evonik Operations GmbH
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Evonik Degussa GmbH
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Publication of WO2018024661A1 publication Critical patent/WO2018024661A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Complex oxides containing nickel and at least one other metal element
    • C01G53/42—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
    • C01G53/44—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • 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
    • C01P2006/11—Powder tap density
    • 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
    • C01P2006/12—Surface area
    • 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
    • C01P2006/12—Surface area
    • C01P2006/13—Surface area thermal stability thereof at high temperatures
    • 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
    • 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
    • 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 invention relates to a method for producing a cathode material with a low BET surface area and high tamped density, as well as a special cathode material itself.
  • One way to improve the discharge rates and cycle stability of cathode materials is to incorporate certain doping elements into the grid of the cathode material. These are those doping elements which have a similar ion radius as lithium. Although the ionic radius of sodium is greater than that of lithium, positive effects on discharge rate and cycle stability were found.
  • the preparation comprises the steps of (1) preparing a metal salt solution, (2) dissolving a dispersing agent and a sodium salt, (3) precipitating the sodium-doped precursor and (4) treating the
  • Precursor at 400-800 ° C over a period of 1-12 hours to form an oxide precursor and (5) mixing the oxide precursor with lithium salts, milling the mixture in a ball mill and (6) final treatment at 700-1000 ° C a period of 1 -40 hours.
  • a particularly preferred doping component is Al.
  • a disadvantage of this method is that the tamped density of the resulting cathode materials is often too low.
  • a cathode material based on lithium mixed oxides should have a high tamped density in order to keep the volume of the battery small with a given energy capacity.
  • US2005 / 106463 discloses an electrode material for a lithium secondary battery containing lithium / transition metal mixed oxides and boron.
  • the electrode material has a specific surface area of 0.1 to 8 m 2 / g and a tamped density of 1.6 g to 3.0 g / cm 3 .
  • the electrode material is prepared by mixing a mixture of a lithium, nickel, manganese and cobalt compound and boric acid in the desired stoichiometric ratio with each other, from which produces a dispersion in water, the dispersion milled until a particle diameter of 30 ⁇ is reached. This is followed by spray drying.
  • the material thus obtained is thermally treated at elevated temperature.
  • the tamped density varies with the type of thermal treatment.
  • the method mentioned in US2005 / 106463 comprises many steps.
  • Tamping density which can not be changed later or only by loss of energy capacity.
  • the object of the present invention was therefore to provide a process which leads to high tamped densities of the powder and which has good electrochemical data.
  • the invention relates to a process for preparing a powdery mixed oxide A of the general formula Lii + x (NiaCobMnc) BdNa e 02
  • Mixed oxide is the intimate mixing of all mixed oxide components to understand. It is therefore largely a mixture at the atomic level, not a physical mixture of oxides.
  • the mixed oxide particles are usually present in the form of aggregated primary particles.
  • the process is particularly suitable for the preparation of mixed oxides A, in which at least one of the conditions d + e> 0.05 and d ⁇ e is met.
  • Atomizing gas is preferably 0.01 to 0.5 kg / Nm 3 .
  • a further preferred embodiment provides that within the reaction space, the flame and the aerosol are partially spatially separated from each other.
  • the spatial separation can be done for example by a bell that surrounds the introduced into the reaction space aerosol. Only at a later time are the products resulting from the ignition of the flame essentially water, and the particles formed from the aerosol, the reaction product, brought together. The particles thus obtained have favorable sintering properties in the subsequent thermal treatment.
  • the solution used should have the highest possible concentration. An optimum should be aimed at between the production quantity and the material properties of the powder. For the process according to the invention, these requirements are best satisfied in a range from 5 to 20% by weight, based on the sum of Li, Ni, Mn, and Co.
  • the concentration of the solution in the atomizing gas is preferably 0.1 to 1 kg / Nm 3 and more preferably 0.3 to 0.7 kg / Nm 3 .
  • hydrogen methane, ethane, propane, butane and mixtures thereof can be used. Preference is given to using hydrogen.
  • the oxygen-containing gas is usually air.
  • the amount of oxygen is to be selected in the inventive method so that it is sufficient at least for complete conversion of the fuel gas and all metal compounds. It is usually beneficial one Use excess oxygen. This excess is conveniently expressed as the ratio of oxygen present / combustion of the fuel gas necessary oxygen and referred to as lambda. Lambda is preferably 1, 1 to 6.0, particularly preferably 2.0 to 4.0.
  • the metal compounds and the boric acid are present in a solution.
  • the solution can be heated.
  • all soluble metal compounds which are oxidizable can be used. These may be inorganic metal compounds, such as nitrates, chlorides, bromides, or organic metal compounds, such as alkoxides or carboxylates, inorganic and / or organic metal compounds.
  • the alkoxides used may preferably be ethylates, n-propylates, isopropylates, n-butylates and / or tert-butylates.
  • the carboxylates which can be used are the compounds based on acetic acid, propionic acid, butanoic acid, hexanoic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, octanoic acid, 2-ethylhexanoic acid, valeric acid, capric acid and / or lauric acid.
  • at least one metal nitrate is used.
  • the solvent may preferably be selected from the group consisting of water, Cs-C2o alkanes, Ci-Ci5-alkanecarboxylic acids and / or Ci-Cis alkanols. Particular preference may be given to using water or a mixture of water and an organic solvent.
  • organic solvents or as a component of mixtures of organic solvents, alcohols such as methanol, ethanol, n-propanol, isopropanol, n-butanol or tert-butanol, diols such as ethanediol, pentanediol, 2-methyl-2, 4-pentanediol, Ci-Ci2-carboxylic acids such as acetic acid, propionic acid, butanoic acid, hexanoic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, octanoic acid, 2-ethylhexanoic acid, valeric acid, capric acid, lauric acid.
  • benzene, toluene, naphtha and / or gasoline can be used.
  • an aqueous solvent is used.
  • Another object of the invention is a process for preparing a powdery mixed oxide B of the general formula A of the general formula Lii + x (NiaCobMnc) BdNa e 02 with 0 ⁇ x ⁇ 0.5; 0 ⁇ a ⁇ 1; 0 ⁇ b ⁇ 1; 0 ⁇ c ⁇ 1; 0.001 ⁇ d ⁇ 0, 1, 0.001 ⁇ e ⁇ 0.2;
  • a BET surface area of 0.1 to 5 m 2 / g, preferably 0.3 to 2 m 2 / g, and a tamped density of 1000 to 2500 g / l, preferably 1 100 to 2000 g / l,
  • the preparation of the mixed oxide B comprises the process steps for the preparation of the mixed oxide A.
  • c) brings the aerosol in a reaction chamber with a flame to react, wherein the flame is obtained from a mixture of a fuel gas and air and in which the total amount of oxygen at least for the complete conversion of the fuel gas and the
  • the solid at 700 to 1 100 ° C, preferably 800 to 1000 ° C, over a period of 2 to 36 hours, preferably 1 to 10 hours, thermally treated.
  • Mixed oxide B has a higher crystallinity than mixed oxide A.
  • Another object of the invention is a special powdery mixed oxide B of the general formula Lii + x (Ni a CobMnc) BdNa e 02 with 0 ⁇ x ⁇ 0.5; 0 ⁇ a ⁇ 1; 0 ⁇ b ⁇ 1; 0 ⁇ c ⁇ 1; 0.001 ⁇ d ⁇ 0, 1; 0.001 ⁇ e ⁇ 0.2, which has a BET surface area of 0, 1 to 5 m 2 / g and a tamped density of 1000 to 2500 g / l and in which the XPS-ESCA in a near-surface layer with a depth of 5 nm certain sodium concentration of the mixed oxide particles is highest and decreases inwards.
  • the higher level of sodium on the surface can be beneficial in the use of the mixed oxide in lithium-ion batteries.
  • Substrate subtraction calculated taking into account the relative sensitivity factors of the respective specified electron levels. The information is given in area percent. The accuracy is relative to +/- 5% relative.
  • Another object of the invention is the use of special, powdery mixed oxide as a cathode material in lithium-ion batteries.
  • an aerosol is generated by means of a nozzle, which is atomized into a reaction space.
  • a blast gas flame burns out of hydrogen and air, in which the aerosol is brought to the reaction.
  • the solid is separated on a filter of gaseous substances.
  • the solid is heated to a temperature of 800 to 960 ° C over 3 to 10 hours in a rotary kiln over a period of 4 to 6 hours.
  • Table 1 lists all relevant parameters for the preparation of the cathode material.
  • Table 2 shows BET surface areas and tamped densities of the mixed oxides produced.
  • Flammenspraypyrolyse similar to Example 1 and Comparative Examples 2 and 3 according to the invention. Sodium as the only doping element (Example 3) does not give sufficiently high
  • Table 3 shows the determined by XPS-ESCA sodium concentration of a mixed oxide powder according to the invention and a comparative example.
  • the mixed oxide powder according to the invention has the highest sodium concentration at the surface.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un oxyde mixte pulvérulent A de formule générale Li1 +x(NiaCobMnc)BdNaeO2 avec 0 < x ≤ 0,5; 0 < a ≤ 1; 0 ≤ b ≤ 1; 0 < c ≤ 1; 0,001 ≤ d ≤ 0,1, 0,001 < e ≤ 0,2; d + e ≥ 0,0 et d < e, ayant une surface BET allant jusqu'à 50 m2/g et une masse volumique tassée allant de 250 à 700 g/litre, selon lequel a) on fournit une solution qui contient des composés métalliques oxydables et/ou hydrolysables de lithium, de manganèse, de nickel et/ou de sodium et de l'acide borique respectivement dans des proportions correspondant à la formule générale, b) on atomise la solution au moyen d'un gaz d'atomisation pour donner un aérosol, c) on fait réagir l'aérosol dans une chambre de réaction avec une flamme, qui est obtenue à partir d'un mélange d'un gaz combustible et d'air et dont la quantité totale en oxygène suffit au moins à la réaction complète du gaz combustible et des composants métalliques, et d) on refroidit le flux réactionnel et on sépare ensuite la matière solide du flux réactionnel. Oxyde mixte pulvérulent de formule générale Li1 +x(NiaCobMnc)BdNaeO2 avec 0 < x ≤ 0,5; 0 < a ≤ 1; 0 ≤ b ≤ 1; 0 < c ≤ 1; 0,001 ≤ d ≤ 0,1; 0,001 < e ≤ 0,2, ayant une surface BET de 0,1 à 5 m2/g et une masse volumique tassée de 1000 à 2500 g/l et dont la concentration en sodium des particules d'oxyde mixte, déterminée par spectroscopie XPS pour l'analyse chimique est maximale dans une couche proche de la surface, à une profondeur d'environ 5 nm, et diminue vers l'intérieur.
PCT/EP2017/069291 2016-08-05 2017-07-31 Procédé de fabrication d'un matériau de cathode à faible surface bet et à masse volumique tassée élevée et matériau de cathode spécial Ceased WO2018024661A1 (fr)

Applications Claiming Priority (2)

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DE102016214590.8 2016-08-05
DE102016214590.8A DE102016214590A1 (de) 2016-08-05 2016-08-05 Verfahren zur Herstellung eines Kathodenmateriales mit niedriger BET-Oberfläche und hoher Stampfdichte und spezielles Kathodenmaterial

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113215647A (zh) * 2021-04-19 2021-08-06 中南大学 一种高电压单晶三元正极材料的改性研究
US11192794B2 (en) 2017-12-07 2021-12-07 Evonik Operations Gmbh Production of pulverulent, porous crystalline metal silicates by means of flame spray pyrolysis
US11434146B2 (en) 2017-01-09 2022-09-06 Evonik Operations Gmbh Method for producing metal oxides by means of spray pyrolysis
EP4047688A4 (fr) * 2020-03-03 2023-11-29 Beijing Easpring Material Technology Co., Ltd. Matériau riche en lithium-manganèse, son procédé de préparation et applications associées
US12410061B2 (en) 2017-07-05 2025-09-09 Evonik Operations Gmbh Spray evaporation of a liquid raw material for preparation of silicon dioxide and metal oxides

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CN110112410B (zh) * 2019-05-29 2022-05-24 新乡学院 一种改性锂离子电池正极材料及其制备方法

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11434146B2 (en) 2017-01-09 2022-09-06 Evonik Operations Gmbh Method for producing metal oxides by means of spray pyrolysis
US12410061B2 (en) 2017-07-05 2025-09-09 Evonik Operations Gmbh Spray evaporation of a liquid raw material for preparation of silicon dioxide and metal oxides
US11192794B2 (en) 2017-12-07 2021-12-07 Evonik Operations Gmbh Production of pulverulent, porous crystalline metal silicates by means of flame spray pyrolysis
EP4047688A4 (fr) * 2020-03-03 2023-11-29 Beijing Easpring Material Technology Co., Ltd. Matériau riche en lithium-manganèse, son procédé de préparation et applications associées
US11958757B2 (en) 2020-03-03 2024-04-16 Beijing Easpring Material Technology Co., Ltd. Lithium-manganese-rich material, preparation method for same, and applications thereof
CN113215647A (zh) * 2021-04-19 2021-08-06 中南大学 一种高电压单晶三元正极材料的改性研究
CN113215647B (zh) * 2021-04-19 2022-03-15 中南大学 一种高电压单晶三元正极材料

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DE102016214590A1 (de) 2018-02-08

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