WO2017037179A1 - Oxyde mixte revêtu d'une enveloppe, contenant du lithium et du manganèse - Google Patents

Oxyde mixte revêtu d'une enveloppe, contenant du lithium et du manganèse Download PDF

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Publication number
WO2017037179A1
WO2017037179A1 PCT/EP2016/070620 EP2016070620W WO2017037179A1 WO 2017037179 A1 WO2017037179 A1 WO 2017037179A1 EP 2016070620 W EP2016070620 W EP 2016070620W WO 2017037179 A1 WO2017037179 A1 WO 2017037179A1
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Prior art keywords
core
shell
shell particles
compound
mol
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PCT/EP2016/070620
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German (de)
English (en)
Inventor
Stipan Katusic
Michael Hagemann
Peter Kress
Armin Wiegand
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Evonik Degussa Gmbh
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Publication of WO2017037179A1 publication Critical patent/WO2017037179A1/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—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/12—Manganates manganites or permanganates
    • C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/12—Manganates manganites or permanganates
    • C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
    • C01G45/1242—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]-, e.g. LiMn2O4, Li[MxMn2-x]O4
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
    • C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
    • C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-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
    • H01M4/362—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
    • H01M4/62—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
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • 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
    • 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 sheath surrounded, containing lithium and manganese mixed oxide, its preparation and use.
  • US2005 / 106463 discloses an electrode material for a lithium secondary battery containing mixed lithium / transition metal 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. It is known to produce electrode materials in a simpler way via a flame spray pyrolysis. Thus, in WO 201 1/160940 a process for the preparation of a lithium
  • Metal compound containing as metal component Ag, Al, B, Ca, Cd, Co, Cr, Cu, Fe, Ga, Ge, In, Mg, Mn, Mo, Nb, Ni, Pd, Rh, Ru, Sc, Sn, Ti , V, Y or Zn is atomized by means of a nebulizer gas to an aerosol and burned in an oxygen / hydrogen flame.
  • EP-A-3026019 discloses a powdered cathode material in the form of aggregated primary particles comprising a mixed oxide powder which has a composition corresponding to
  • Lii + x (Ni a CobMn c ) DdO 2, and H and N as a non-metal component, having a content of H 0.01 - 0, 1 wt .-% and a content of N of 0.002-0.05 wt .-% and wherein D Ag, Al, B, Ca, Cr, Cu, Fe, Ga, Ge, In, K, Mg, Mo, Na, Nb, Si, Sn, Ta, Ti, Ti, V, and Zr and 0 ⁇ x ⁇ 0.2; 0 ⁇ a ⁇ 1; 0 ⁇ b ⁇ 1; 0 ⁇ c ⁇ 1, 0 ⁇ d ⁇ 0.2. It is prepared by adding a solution containing a lithium compound and at least one other metal compound selected from the group consisting of Mn, Ni and Co and an ammonia-containing aerosol in one
  • all soluble doping compounds which are oxidizable can be used. These may be inorganic metal compounds or organic metal compounds.
  • a particularly preferred doping component is Al.
  • the doping compound is preferably used in an amount such that the later cathode material does not contain more than 10% by weight of doping component, more preferably 0.1 to 5% by weight.
  • Kalaignan et al. in Journal of Power Sources 196 (201 1) 3640-3645 describe the preparation of silica-clad LiMn204 cathode material via a gel route and subsequent thermal treatment. Accordingly, the crystal structure is not changed by the shell, the electrochemical properties improved.
  • Park et al. in Journal of Power Sources 126 (2004) 150-155 describe the preparation of alumina-clad LiMn2-xZr x 04 via a sol-gel route. Again, the cladding leads to improved electrochemical properties, as compared to the non-clad material.
  • the object of the present invention was to provide cathode materials which have again improved electrochemical properties compared with this prior art. Another object was to provide a method for these cathode materials.
  • the invention relates to core-shell particles (1), wherein the core comprises a mixed oxide containing lithium and manganese, characterized in that
  • the shell largely consists of silica and alumina or
  • the shell consists largely of silica or alumina and
  • the BET surface area is 10 to 30 m 2 / g, preferably 15 to 25 m 2 / g.
  • the silica is an X-ray amorphous silica. Boron should be considered as metal in the context of this invention.
  • the present invention claims two types of core shell particles.
  • the core-shell particles (1) have, for example, a higher BET surface area than the core-shell particles (2).
  • the core-shell particles (1) are the product of flame spray pyrolysis.
  • the core-shell particles (2) can be obtained by thermal aftertreatment of the core-shell particles (1).
  • 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 generally present in the form of aggregated primary particles.
  • Composition contains.
  • the presence of Lio, 78Mno, 8s02 or Lio, 96Mno, 7402 besides the main phase is called LiMri204.
  • the coating constituents contain only conventional, due to the production of these products impurities in conventional amounts.
  • Impurities from silica may be iron oxides, titania, alumina or hydrochloric acid.
  • Impurities from alumina can be iron oxides, titanium oxide,
  • Be silica or hydrochloric acid The usual amount is understood to mean that the proportion of the coating constituents silicon dioxide and aluminum oxide is at least 98% by weight, generally at least 99% by weight or 99.5% by weight.
  • the core-shell particles (1) generally have an acceptable tamped density of 300-600 g / l.
  • the BET surface area is determined according to DIN ISO 9277.
  • the tamped density is determined according to DIN EN ISO 787/1 1.
  • the shell consists essentially of silica and alumina
  • a ratio Si / Al of 0, 1-100 mol / mol has been found to be preferred and 0.2-10 mol / mol is particularly preferred.
  • the ratio M / (Li + Mn) is preferably 0.001-0.5 mol / mol, and more preferably 0.005-0.03 mol / mol.
  • Alumina and / or boria are the preferred additional metal oxides in the core.
  • the core may also contain nickel and / or cobalt.
  • Another object of the invention is a process for the preparation of the core-shell particles (1), wherein
  • metal M Al, B, Ca, Nb, Ta, Ti and V,
  • the aerosol can be prepared by co-sputtering a metal compound and a
  • Atomizing gas can be obtained by means of one or more nozzles.
  • Lithium, manganese, nickel and cobalt compound, and the metal compound can be used as such even in liquid form or in the form of a solution.
  • the nature of the metal compounds is not limited as long as they are hydrolyzable or pyrolyzable under the reaction conditions to form the metal oxides.
  • chlorides, nitrates or organometallic compounds can be used.
  • the solution contains different metal compounds of one metal or more metal compounds with different metal components. In the latter case mixed metal oxides are formed.
  • air, oxygen-enriched air and / or an inert gas such as nitrogen can be used as sputtering gas.
  • Cobalt compound as well as the metal compound in a solution.
  • the solution can be heated. Particular preference may be given to using water or a mixture of water and an organic solvent.
  • organic solvents include water or a mixture of water and an organic solvent.
  • alcohols such as methanol, ethanol, n-propanol, isopropanol, n-butanol or tert-butanol
  • diols such as ethanediol, pentanediol, 2-methyl-2,4-pentanediol
  • C1- C12 carboxylic acids such as acetic, propionic, butanoic, hexanoic, oxalic, malonic, succinic, glutaric, adipic, octanoic, 2-ethylhexanoic, valeric, capric,
  • Lauric acid can be used. Furthermore, benzene, toluene, naphtha and / or gasoline can be used. Preferably, an aqueous solvent is used.
  • a silicon compound and / or aluminum compound each of which is hydrolyzable or pyrolyzable, is added to the reaction mixture from the first zone.
  • SiCU preferably selected from the group consisting of SiCU, CH 3 SCl 3 , (Ch 2 SiCk, (CH 2 SiCl, HSiCIs, (CH 3 ) 2 HSiCl and CH 3 C 2 H 5 SCl 2, H 4 Si, Si (OC 2 H 5 ) 4 and Si (OCH 3 ) 4 and the
  • the timing of addition of the silicon compound and / or aluminum compound is to be chosen so that the particle formation of the core constituents in the first zone is well advanced or already completed. This time depends among other things on the execution of the
  • the average residence time in the first zone and the second zone is independently 0.1 - 10 s.
  • a particular embodiment provides that ammonia is introduced into the reaction space. This can be achieved, for example, by adding ammonia to the aerosol.
  • concentration of ammonia is preferably 0.01-2 Nm 3 / mol (Li + Mn), more preferably 0.05-1.5 Nim 3 / mol (Li + Mn). The addition of ammonia seems to affect the
  • Another object of the invention are core-shell particles (2), wherein the core comprises a lithium and manganese-containing mixed oxide, and
  • the shell largely consists of silica and alumina or
  • the shell consists largely of silica or alumina and
  • the BET surface area is less than 10 m 2 / g.
  • core-shell particles (2) These particles are to be referred to in the context of the present invention as core-shell particles (2). They differ from the core-shell particles (1), inter alia, in a lower BET surface area and a higher crystallinity.
  • the further metal oxide is alumina and the tamped density of the core-shell particles (2) is 700-1500 g / l.
  • Another object of the invention is a process for the preparation of the core-shell particles (2) in which the core-shell particles (1) are thermally treated. Preferably, this is done at 800 to 1000 ° C and over a period of 1 to 10 hours.
  • the production of the core-shell particles (2) comprises the process steps for the production of the core-shell particles (1).
  • the production of the core-shell particles (2) includes a
  • metal M Al, B, Ca, Nb, Ta, Ti and V,
  • Another object of the invention is the use of the core-shell particles (2) produced by the novel process as the 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 mean residence time of the reaction mixture in the first zone is 0.75 s in Examples 1 and 2 and 1.75 s in Examples 3-6.
  • vapor Si (OC2Hs) 4 and / or vaporous Al (OiBu) 3 is added to the stream of the reaction mixture from the first zone, in each case together with nitrogen, and separately 2.5 kg / h of steam.
  • the average residence time of the reaction mixture in the second zone is 0.9 s in Examples 3-6.
  • the solid After cooling, the solid is separated on a filter of gaseous substances.
  • Comparative Example 1 has neither a shell nor an additional metal oxide.
  • Comparative Example 2 has a SiC shell, but no additional metal oxide in the core.
  • Inventive Example 3 has an SiC shell and Al 2 O 3 as an additional metal oxide in the core.
  • Inventive Examples 4-6 have a shell of S1O2 and Al2O3 and Al2O3 as an additional metal oxide in the core.
  • the proportion of Al2O3 in Examples 4-6 increases.
  • Table 2 shows that the shell and the additional AI2O3 in the core leads to an improvement of the electrochemical data.
  • Table 1 Starting materials and reaction conditions

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Catalysts (AREA)

Abstract

Particule cœur-écorce (1) dont le cœur comprend un oxyde mixte contenant du lithium et du manganèse, et se caractérisant en ce que a) l'enveloppe se compose majoritairement de dioxyde de silicium et d'oxyde d'aluminium ou b) l'enveloppe se compose majoritairement de dioxyde de silicium ou d'oxyde d'aluminium et le noyau contient en complément au moins un autre oxyde d'un métal M tel que M = AI, B, Ca, Nb, Ta, Ti et V, et c) la surface BET vaut 10-30 m2/g.
PCT/EP2016/070620 2015-09-03 2016-09-01 Oxyde mixte revêtu d'une enveloppe, contenant du lithium et du manganèse WO2017037179A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015216901.4 2015-09-03
DE102015216901.4A DE102015216901A1 (de) 2015-09-03 2015-09-03 Mit einer Hülle umgebenes Lithium und Mangan enthaltendes Mischoxid

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111193019A (zh) * 2020-01-13 2020-05-22 惠州亿纬锂能股份有限公司 一种补锂添加剂及其制备方法和锂离子电池

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2399867A1 (fr) * 2010-06-25 2011-12-28 Evonik Degussa GmbH Procédé de fabrication d'oxydes mixtes contenant du lithium
US20120040247A1 (en) * 2010-07-16 2012-02-16 Colorado State University Research Foundation LAYERED COMPOSITE MATERIALS HAVING THE COMPOSITION: (1-x-y)LiNiO2(xLi2Mn03)(yLiCoO2), AND SURFACE COATINGS THEREFOR
WO2014142803A1 (fr) * 2013-03-12 2014-09-18 Sachem, Inc. Formation d'une coque d'oxyde sur des substrats inorganiques par déposition de sel de polyoxoanion de lithium

Family Cites Families (2)

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Publication number Priority date Publication date Assignee Title
US7241532B2 (en) 2002-03-28 2007-07-10 Mitsubishi Chemical Corporation Positive-electrode material for lithium secondary battery, secondary battery employing the same, and process for producing positive-electrode material for lithium secondary battery
EP3026019A1 (fr) 2014-11-25 2016-06-01 Evonik Degussa GmbH Procédé de fabrication d'un matériau de cathode et matériau de cathode spécial

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2399867A1 (fr) * 2010-06-25 2011-12-28 Evonik Degussa GmbH Procédé de fabrication d'oxydes mixtes contenant du lithium
US20120040247A1 (en) * 2010-07-16 2012-02-16 Colorado State University Research Foundation LAYERED COMPOSITE MATERIALS HAVING THE COMPOSITION: (1-x-y)LiNiO2(xLi2Mn03)(yLiCoO2), AND SURFACE COATINGS THEREFOR
WO2014142803A1 (fr) * 2013-03-12 2014-09-18 Sachem, Inc. Formation d'une coque d'oxyde sur des substrats inorganiques par déposition de sel de polyoxoanion de lithium

Non-Patent Citations (1)

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Title
J.-S. KIM ET AL: "The Electrochemical Stability of Spinel Electrodes Coated with ZrO[sub 2], Al[sub 2]O[sub 3], and SiO[sub 2] from Colloidal Suspensions", JOURNAL OF THE ELECTROCHEMICAL SOCIETY, vol. 151, no. 10, 1 January 2004 (2004-01-01), US, pages A1755, XP055310521, ISSN: 0013-4651, DOI: 10.1149/1.1793713 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111193019A (zh) * 2020-01-13 2020-05-22 惠州亿纬锂能股份有限公司 一种补锂添加剂及其制备方法和锂离子电池

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