WO1999040029A1 - Verfahren zur herstellung von lithium-übergangsmetallaten - Google Patents

Verfahren zur herstellung von lithium-übergangsmetallaten Download PDF

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Publication number
WO1999040029A1
WO1999040029A1 PCT/EP1998/005150 EP9805150W WO9940029A1 WO 1999040029 A1 WO1999040029 A1 WO 1999040029A1 EP 9805150 W EP9805150 W EP 9805150W WO 9940029 A1 WO9940029 A1 WO 9940029A1
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WIPO (PCT)
Prior art keywords
compound
transition metal
lithium
calcination
manganese
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/EP1998/005150
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German (de)
English (en)
French (fr)
Inventor
Mathias Benz
Wolfgang Kummer
Evelyn Pross
Josef Schmoll
Wolfgang Schweda
Daniel Duff
Ricarda Leiberich
Christoph Schild
Ulrich Krynitz
Juliane Meese-Marktscheffel
Viktor Stoller
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HC Starck GmbH
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HC Starck GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from PCT/EP1998/000697 external-priority patent/WO1998037023A1/de
Priority to EP98945239A priority Critical patent/EP1058673B1/de
Priority to AU92622/98A priority patent/AU744558B2/en
Priority to DE59811208T priority patent/DE59811208D1/de
Priority to CA002320155A priority patent/CA2320155C/en
Priority to KR1020007008659A priority patent/KR100544541B1/ko
Priority to US09/601,946 priority patent/US6875416B1/en
Priority to AT98945239T priority patent/ATE264271T1/de
Priority to HK01105761.5A priority patent/HK1034952B/xx
Priority to HU0100690A priority patent/HUP0100690A3/hu
Priority to JP2000530464A priority patent/JP4122710B2/ja
Application filed by HC Starck GmbH filed Critical HC Starck GmbH
Priority to IL13735098A priority patent/IL137350A0/xx
Publication of WO1999040029A1 publication Critical patent/WO1999040029A1/de
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G53/82—Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
    • 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
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/12—Complex oxides containing manganese and at least one other metal element
    • C01G45/1221—Manganates or manganites with trivalent manganese, tetravalent manganese 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—Complex oxides containing manganese and at least one other metal element
    • C01G45/1221—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof
    • C01G45/1228—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof of the type (MnO2)-, e.g. LiMnO2 or Li(MxMn1-x)O2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/20—Compounds containing manganese, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G45/22—Compounds containing manganese, with or without oxygen or hydrogen, and containing two or more other elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Complex oxides containing cobalt and at least one other metal element
    • C01G51/42—Complex oxides containing cobalt and at least one other metal element containing alkali metals, e.g. LiCoO2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Complex oxides containing cobalt and at least one other metal element
    • C01G51/42—Complex oxides containing cobalt and at least one other metal element containing alkali metals, e.g. LiCoO2
    • C01G51/44—Complex oxides containing cobalt and at least one other metal element containing alkali metals, e.g. LiCoO2 containing manganese
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/80—Compounds containing cobalt, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G51/82—Compounds containing cobalt, with or without oxygen or hydrogen, and containing two or more other elements
    • 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
    • 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
    • H01M4/58—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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/10—Nitrates
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C01P2006/40—Electric properties
    • 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
    • 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
    • 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
    • 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 method for producing lithium transition metallates of the general formula
  • M 1 denotes nickel, cobalt or manganese
  • M 2 denotes a transition metal different from M 1 and means chromium, cobalt, iron, manganese, molybdenum and / or aluminum,
  • n 2 if M 1 is manganese and n is 1 if M 1 is nickel or cobalt, where
  • x assumes a value from 0.9 to 1.2
  • y takes a value between 0.5 and 1 and
  • z assumes a value between 1.9 and 2.1.
  • Such lithium transition metallates are used as electrode material, in particular as cathode material, for non-aqueous lithium secondary battery systems, so-called lithium-ion batteries.
  • LiCoO 2 has prevailed in recent years, but due to the limited availability and the associated high price of cobalt it is extremely expensive and is therefore out of the question for mass production (e.g. for the electric drive of vehicles). Therefore, there have already been intensive efforts to use LiCoO 2 as cathode material, for example using LiNiO 2 and / or
  • LiMn 2 ⁇ 4 to replace in whole or in part.
  • the intimate mixture is prepared by coprecipitating soluble lithium and transition metal salts from the solution, drying the solution and calcining.
  • relatively finely divided crystals of the lithium transition metallates are obtained at comparatively low calcination temperatures and within comparatively short times.
  • Lithium transition metalates are formed by solid diffusion during the calcination. Solid-state diffusion requires comparatively high temperatures with comparatively long calcination times and generally did not lead to phase-pure lithium metallates with excellent electronic properties. Extensive observations seem to prove that in the case of the nickel system, a longer temperature treatment above 700 ° C begins to decompose LiNiO 2 with the formation of Li O and NiO.
  • EP-A 0 468 942 has therefore already proposed starting with powdery nickel oxide or hydroxide in the production of lithium nickelate, suspending the powder in a saturated lithium hydroxide solution and removing the water from the suspension by spray drying. This should reduce the calcination time and temperature. Because of the relatively low solubility of lithium hydroxide in water, the homogeneity of this mixture is limited.
  • the transition metal compound is used in the form of a powder with a specific surface area of at least 10 m 2 / g (BET), the transition metal ver - Impregnation bond with a large specific surface area before the calcination with the solution of an oxygen-containing lithium compound and the solvent is removed by drying.
  • the transition metal compound powder is able to absorb the lithium compound in such a way that a continuous phase cannot form when heated to a temperature above the melting point of the lithium compound, and the transition metal compound powders coated with the lithium compound both stick with the reactor wall as well as the powder particles with each other is largely avoided.
  • the present invention accordingly relates to a process for the preparation of lithium transition metallates of the general formula Li ⁇ MiyM 2 !. ⁇ ,, where
  • M 1 denotes nickel, cobalt or manganese
  • M 2 is chromium, cobalt, iron, manganese, molybdenum or aluminum and is not equal to M 1 ,
  • n 2 if M 1 is manganese, otherwise 1
  • y is a number between 0.5 and 1.0
  • z is a number between 1.9 and 2.1
  • Lithium compound and drying was obtained, which is characterized in that at least the M 1 compound is used in the form of a powder with a specific surface area of at least 10 m 2 / g (BET) and the calcination is carried out in a moving bed.
  • the Mi compound preferably has a specific surface area of at least 25 m 2 / g, particularly preferably at least 40 m 2 / g.
  • the hydroxides are used as preferred transition metal compounds M 1 .
  • Nickel hydroxide is particularly preferred.
  • ⁇ -Nickel hydroxide with a specific surface area of 60 to 80 m 2 / g is very particularly preferably used, in particular one which is obtainable according to US Pat. No. 5,391,265.
  • the M 2 transition metal compound is preferably at least partially used in the form of a mixed hydroxide of the formula (M 1 y M 2 1. Y ) (OH) 2 .
  • Y should preferably be greater than 0.8, particularly preferably greater than 0.9.
  • Lithium hydroxide and / or lithium nitrate can be used as the oxygen-containing lithium compound. These are preferably mixed with the transition metal compound in aqueous solution and then dried and granulated. Lithium nitrate is used as the preferred oxygen-containing lithium compound.
  • the aqueous solution of the lithium compound is preferably used in concentrated form, in the case of lithium nitrate as a more than 35% aqueous solution.
  • At least part of the M 2 transition metal compound can be used as a solution component of the solution of the lithium compound for impregnating the M 1 transition metal compound.
  • the solid powdery transition metal compound is mixed with the solution of the lithium compound with stirring and then the solvent, in particular water, is dried by spray drying, fluidized bed spray granulation or mixer agglomeration.
  • the solvent in particular water
  • a spray-dried material with an agglomerate size of less than 100 ⁇ m is preferred.
  • the subsequent calcination in a moving bed can be carried out in a rotary kiln, in a fluidized bed or in a chute reactor (downer).
  • a rotary kiln is particularly preferred.
  • the granules are introduced continuously or batchwise into a preferably electrically heated rotary kiln and for a residence time of 0.5 to 10 hours, preferably 1 to 5 hours, at a temperature of 500 to 800 ° C., preferably 550 to 650 ° C. , particularly preferably 580 to 620 ° C, treated. - 7 -
  • the temperature range from below the melting temperature of the lithium compound to the calcination temperature should be passed as quickly as possible. Accordingly, the intimate mixture is introduced into the rotary kiln which is already at the calcining temperature or into the moving bed which is at the calcining temperature.
  • the intimate mixture can be preheated to a temperature of up to 200 ° C., preferably 150 to 180 ° C.
  • the preheating can be carried out up to a temperature of 350 ° C.
  • the calcination can be carried out in an atmosphere containing up to 50% oxygen, for example air. Calcination is preferred, at least for two thirds of the calcination time, under essentially oxygen-free inert gas, for example argon, with an oxygen content of less than 5%, in particular less than 3%. In this case, calcination is preferably carried out under an oxygen-containing gas atmosphere during the remaining calcination time.
  • the atmosphere can be exchanged for an oxygen-containing atmosphere after at least two thirds of the calcination time.
  • an oxygen-containing atmosphere or oxygen is preferably introduced into the furnace in the last third of the furnace by means of a lance.
  • the lithium transition metallate emerging in powder form from the moving bed is cooled to room temperature (below 100 ° C.) and subjected to gentle grinding.
  • Suitable grinding devices are, for example, those which take advantage of the shear effect of high gas velocity profiles, the size reduction being carried out by particle-particle impact, such as fluidized bed counter-jet mills or micro-vortex mills.
  • the grinding is preferably carried out (after separation of the fine fraction) up to an average grain size of 15 to 25 ⁇ m in diameter.
  • the fine fraction of the grinding is either returned to the moving bed or mixed with the powdery, oxygen-containing transition metal compound and then treated and dried together with the solution of the oxygen-containing lithium compound, i.e. impregnated.
  • Lithium nitrate is particularly preferably used as the oxygen-containing lithium compound.
  • the NO x gas released in this case during the calcination is preferably absorbed in an aqueous lithium hydroxide solution and the resulting lithium nitrate solution is used to impregnate the powdery transition metal compounds.
  • the premix preparation A consists of a stirred container in which a 40% aqueous lithium nitrate solution is placed, into which powdered ⁇ -nickel hydroxide with an average particle size of 10 ⁇ m and a specific surface area of 65 m 2 / g is stirred. The received
  • Slurry is dried by spray drying and introduced into rotary kiln B as granules with an average particle diameter of about 100 ⁇ m.
  • the furnace material is preferably kept under an inert gas at sintering temperature for 1 to 3 hours.
  • the argon atmosphere can then be replaced (in batch mode) by an atmosphere containing 20 to 50% oxygen. Then the
  • the rotary kiln was cooled and the lithium nickelate obtained was ground in a fluidized bed counter-jet mill C to a particle diameter below 40 ⁇ m and the fine fraction with particle sizes below 3 ⁇ m separated by sighting or in a cyclone and collected for return to oven B.
  • the furnace atmosphere containing NO x is washed in a scrubber D with aqueous lithium hydroxide solution and the lithium nitrate obtained is obtained for the renewed premix production.
  • BET is stirred into an approximately 40% aqueous solution of lithium nitrate.
  • the molar ratio of LiNO 3 to Ni (OH) 2 is 1.03.
  • the suspension is dried in a spray tower.
  • the dried powder with an average grain size of about 60 ⁇ m is mixed with 5% by weight lithium nickelate with a grain size ⁇ 5 ⁇ m.
  • 500 g of the powder mixture are placed in the hot zone of a laboratory rotary kiln heated to 620 ° C, through which a stream of nitrogen flows at a speed of 84 m / h.
  • the rotary kiln has an inner diameter of 55 mm and is rotated at 1/4 rpm.
  • the rotary kiln After one hour the rotary kiln is cooled to less than 100 ° C and samples are taken from the oven.
  • Example 1 was repeated with the difference that the rotary kiln is kept at 600 ° C. and the cooling takes place after two hours. - 11 -
  • Example 2 was repeated, first annealing at 640 ° C. under nitrogen and then 30 minutes at 640 ° C. in air.
  • Half-width 003 reflex 0.17
  • Half-width 004-reflex 0.19

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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)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)
PCT/EP1998/005150 1998-02-09 1998-08-13 Verfahren zur herstellung von lithium-übergangsmetallaten Ceased WO1999040029A1 (de)

Priority Applications (11)

Application Number Priority Date Filing Date Title
IL13735098A IL137350A0 (en) 1998-02-09 1998-08-13 Method for producing lithium-transition metal mixtures
AT98945239T ATE264271T1 (de) 1998-02-09 1998-08-13 Verfahren zur herstellung von lithium- übergangsmetallaten
DE59811208T DE59811208D1 (de) 1998-02-09 1998-08-13 Verfahren zur herstellung von lithium-übergangsmetallaten
CA002320155A CA2320155C (en) 1998-02-09 1998-08-13 Process for preparing lithium transition metallates
KR1020007008659A KR100544541B1 (ko) 1998-02-09 1998-08-13 리튬-전이 금속 혼합물의 제조 방법
US09/601,946 US6875416B1 (en) 1998-02-09 1998-08-13 Method for producing lithium-transition metal mixtures
HU0100690A HUP0100690A3 (en) 1998-02-09 1998-08-13 Method for producing lithium-transition metal mixtures
EP98945239A EP1058673B1 (de) 1998-02-09 1998-08-13 Verfahren zur herstellung von lithium-übergangsmetallaten
HK01105761.5A HK1034952B (en) 1998-02-09 1998-08-13 Method for producing lithium-transition metal mixtures
JP2000530464A JP4122710B2 (ja) 1998-02-09 1998-08-13 リチウム−遷移金属混合物の調製法
AU92622/98A AU744558B2 (en) 1998-02-09 1998-08-13 Method for producing lithium-transition metal mixtures

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PCT/EP1998/000697 WO1998037023A1 (de) 1997-02-19 1998-02-09 Verfahren zur herstellung von lithium-übergangsmetallaten
EPPCT/EP98/00697 1998-02-09

Publications (1)

Publication Number Publication Date
WO1999040029A1 true WO1999040029A1 (de) 1999-08-12

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PCT/EP1998/005150 Ceased WO1999040029A1 (de) 1998-02-09 1998-08-13 Verfahren zur herstellung von lithium-übergangsmetallaten

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US (1) US6875416B1 (https=)
EP (1) EP1058673B1 (https=)
JP (1) JP4122710B2 (https=)
KR (1) KR100544541B1 (https=)
CN (1) CN1191994C (https=)
AT (1) ATE264271T1 (https=)
AU (1) AU744558B2 (https=)
CA (1) CA2320155C (https=)
DE (1) DE59811208D1 (https=)
HU (1) HUP0100690A3 (https=)
IL (1) IL137350A0 (https=)
WO (1) WO1999040029A1 (https=)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004034489A3 (en) * 2002-09-13 2005-03-03 Max Planck Ges Zur Novel electrodes for li-based electrochemical energy storage devices and a li-based electrochemical storage device
CN1300868C (zh) * 2003-04-30 2007-02-14 杨永平 锂离子电池用结构稳定的尖晶石锰酸锂的制备方法
US7648693B2 (en) 2005-04-13 2010-01-19 Lg Chem, Ltd. Ni-based lithium transition metal oxide
EP2463942A1 (en) 2006-05-10 2012-06-13 LG Chem, Ltd. Material for lithium secondary battery of high performance
US8426066B2 (en) 2005-04-13 2013-04-23 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US8450013B2 (en) 2005-04-13 2013-05-28 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US8540961B2 (en) 2005-04-13 2013-09-24 Lg Chem, Ltd. Method of preparing material for lithium secondary battery of high performance
WO2020224020A1 (zh) * 2019-05-06 2020-11-12 山东泽石新材料科技有限公司 一种过渡金属锂氧化物的制备方法及装置

Families Citing this family (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7217406B2 (en) * 2002-02-21 2007-05-15 Tosoh Corporation Lithium-manganese composite oxide granular secondary particle, method for production thereof and use thereof
NZ520452A (en) * 2002-10-31 2005-03-24 Lg Chemical Ltd Anion containing mixed hydroxide and lithium transition metal oxide with gradient of metal composition
US7381496B2 (en) * 2004-05-21 2008-06-03 Tiax Llc Lithium metal oxide materials and methods of synthesis and use
JP2009193745A (ja) 2008-02-13 2009-08-27 Sony Corp 正極活物質の製造方法
US8333950B2 (en) * 2009-08-27 2012-12-18 Honeywell International Inc. Process for the preparation of lithium metal oxides involving fluidized bed techniques
US20140004473A1 (en) * 2011-03-16 2014-01-02 Hanwha Chemical Corporation Method for calcining electrode materials using a rotary kiln
US8992794B2 (en) * 2011-06-24 2015-03-31 Basf Corporation Process for synthesis of a layered oxide cathode composition
JP5365711B2 (ja) * 2012-02-21 2013-12-11 住友金属鉱山株式会社 ニッケルコバルトマンガン複合水酸化物及びその製造方法
US10086351B2 (en) * 2013-05-06 2018-10-02 Llang-Yuh Chen Multi-stage process for producing a material of a battery cell
JP6702969B2 (ja) 2014-11-26 2020-06-03 ビーエーエスエフ ソシエタス・ヨーロピアＢａｓｆ Ｓｅ リチウム化遷移金属酸化物の製造方法
US9979022B2 (en) * 2015-03-31 2018-05-22 Denso Corporation Positive electrode material, positive electrode for non-aqueous electrolyte secondary battery, and non-aqueous electrolyte secondary battery
CN105047869A (zh) * 2015-06-16 2015-11-11 田东 一种锂离子正极材料LiNiO2/C的合成方法
CN107068963A (zh) * 2016-12-28 2017-08-18 中国电子科技集团公司第十八研究所 一种铝电极的表面处理方法
CN110494394A (zh) * 2017-03-15 2019-11-22 尤米科尔公司 用于制造过渡金属氢氧化物前体的硝酸盐方法
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CN110697801B (zh) * 2019-10-29 2020-12-04 山东泽石新材料科技有限公司 一种过渡金属锂氧化合物的制备方法及装置
KR20220127517A (ko) * 2021-03-11 2022-09-20 에스케이온 주식회사 리튬 이차 전지용 양극 활물질의 제조 방법
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994025398A1 (fr) * 1993-04-23 1994-11-10 Centre National De La Recherche Scientifique Procede de preparation d'oxydes mixtes de lithium et de metaux de transition, les oxydes obtenus et leur utilisaton comme materiau d'electrode
EP0643430A1 (en) * 1993-07-15 1995-03-15 Sumitomo Chemical Company, Limited Cathode material for lithium secondary battery and method for producing lithiated nickel dioxide and lithium secondary battery
EP0806397A1 (en) * 1995-11-24 1997-11-12 Fuji Chemical Industry Co., Ltd. Lithium-nickel composite oxide, process for preparing the same, and positive active material for secondary battery

Family Cites Families (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4567031A (en) * 1983-12-27 1986-01-28 Combustion Engineering, Inc. Process for preparing mixed metal oxides
CA1265580A (en) 1985-05-10 1990-02-06 Akira Yoshino Secondary battery
US4770960A (en) 1986-04-30 1988-09-13 Sony Corporation Organic electrolyte cell
US4980080A (en) * 1988-06-09 1990-12-25 Societe Anonyme Dite: Saft Process of making a cathode material for a secondary battery including a lithium anode and application of said material
US5264201A (en) 1990-07-23 1993-11-23 Her Majesty The Queen In Right Of The Province Of British Columbia Lithiated nickel dioxide and secondary cells prepared therefrom
US5180574A (en) * 1990-07-23 1993-01-19 Moli Energy (1990) Limited Hydrides of lithiated nickel dioxide and secondary cells prepared therefrom
DE4239295C2 (de) 1992-11-23 1995-05-11 Starck H C Gmbh Co Kg Verfahren zur Herstellung von reinem Nickelhydroxid sowie dessen Verwendung
JPH07105950A (ja) 1993-10-07 1995-04-21 Dowa Mining Co Ltd 非水溶媒リチウム二次電池用正極活物質とその製造法およびリチウム二次電池
JP3067531B2 (ja) 1994-07-13 2000-07-17 松下電器産業株式会社 非水電解液二次電池の正極活物質およびそれを用いた電池
JP3606290B2 (ja) 1995-04-28 2005-01-05 日本電池株式会社 非水系電池の正極活物質用コバルト含有ニッケル酸リチウムの製造方法
US5591548A (en) 1995-06-05 1997-01-07 Motorola, Inc. Electrode materials for rechargeable electrochemical cells and method of making same
US5702679A (en) * 1995-10-06 1997-12-30 Kerr-Mcgee Chemical Corp. Method of preparing Li1+X- Mn2-X O4 for use as secondary battery
IT1285922B1 (it) * 1996-05-06 1998-06-26 Gd Spa Metodo e dispositivo per la piegatura di lembi di estremita' di involucri tubolari
US5728367A (en) * 1996-06-17 1998-03-17 Motorola, Inc. Process for fabricating a lithiated transition metal oxide
JPH10152327A (ja) 1996-11-19 1998-06-09 Seimi Chem Co Ltd リチウム含有複合酸化物の製造方法及びそれを実施するための焼成炉
EP1017627B1 (de) * 1997-02-19 2002-09-11 H.C. Starck GmbH Verfahren zur herstellung von lithium-übergangsmetallaten

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994025398A1 (fr) * 1993-04-23 1994-11-10 Centre National De La Recherche Scientifique Procede de preparation d'oxydes mixtes de lithium et de metaux de transition, les oxydes obtenus et leur utilisaton comme materiau d'electrode
EP0643430A1 (en) * 1993-07-15 1995-03-15 Sumitomo Chemical Company, Limited Cathode material for lithium secondary battery and method for producing lithiated nickel dioxide and lithium secondary battery
EP0806397A1 (en) * 1995-11-24 1997-11-12 Fuji Chemical Industry Co., Ltd. Lithium-nickel composite oxide, process for preparing the same, and positive active material for secondary battery

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2214230A1 (en) * 2002-09-13 2010-08-04 Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Novel electrodes for Li-based electrochemical energy storage devices and Li-based electrochemical storage device including such an electrode
WO2004034489A3 (en) * 2002-09-13 2005-03-03 Max Planck Ges Zur Novel electrodes for li-based electrochemical energy storage devices and a li-based electrochemical storage device
CN1300868C (zh) * 2003-04-30 2007-02-14 杨永平 锂离子电池用结构稳定的尖晶石锰酸锂的制备方法
US8540961B2 (en) 2005-04-13 2013-09-24 Lg Chem, Ltd. Method of preparing material for lithium secondary battery of high performance
US8784770B2 (en) 2005-04-13 2014-07-22 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US7939203B2 (en) 2005-04-13 2011-05-10 Lg Chem, Ltd. Battery containing Ni-based lithium transition metal oxide
US7943111B2 (en) 2005-04-13 2011-05-17 Lg Chem, Ltd. Process of making cathode material containing Ni-based lithium transition metal oxide
US9590243B2 (en) 2005-04-13 2017-03-07 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US8426066B2 (en) 2005-04-13 2013-04-23 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US8450013B2 (en) 2005-04-13 2013-05-28 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US7648693B2 (en) 2005-04-13 2010-01-19 Lg Chem, Ltd. Ni-based lithium transition metal oxide
US8574541B2 (en) 2005-04-13 2013-11-05 Lg Chem, Ltd. Process of making cathode material containing Ni-based lithium transition metal oxide
US7939049B2 (en) 2005-04-13 2011-05-10 Lg Chem, Ltd. Cathode material containing Ni-based lithium transition metal oxide
US8795897B2 (en) 2005-04-13 2014-08-05 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US8815204B2 (en) 2005-04-13 2014-08-26 Lg Chem, Ltd. Method of preparing material for lithium secondary battery of high performance
US9412996B2 (en) 2005-04-13 2016-08-09 Lg Chem, Ltd. Material for lithium secondary battery of high performance
US9416024B2 (en) 2005-04-13 2016-08-16 Lg Chem, Ltd. Method of preparing material for lithium secondary battery of high performance
US9590235B2 (en) 2005-04-13 2017-03-07 Lg Chem, Ltd. Material for lithium secondary battery of high performance
EP2463942A1 (en) 2006-05-10 2012-06-13 LG Chem, Ltd. Material for lithium secondary battery of high performance
WO2020224020A1 (zh) * 2019-05-06 2020-11-12 山东泽石新材料科技有限公司 一种过渡金属锂氧化物的制备方法及装置
US11757095B2 (en) 2019-05-06 2023-09-12 Shandong Zstone New Material Technology Co., Ltd. Method and apparatus for preparing transition metal lithium oxide

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IL137350A0 (en) 2001-07-24
CN1191994C (zh) 2005-03-09
HUP0100690A3 (en) 2005-03-29
AU9262298A (en) 1999-08-23
HUP0100690A1 (hu) 2001-06-28
JP4122710B2 (ja) 2008-07-23
EP1058673B1 (de) 2004-04-14
EP1058673A1 (de) 2000-12-13
KR20010040770A (ko) 2001-05-15
DE59811208D1 (de) 2004-05-19
CA2320155A1 (en) 1999-08-12
AU744558B2 (en) 2002-02-28
CN1284932A (zh) 2001-02-21
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