WO2015016648A1 - Procédé de préparation d'un oxyde de composite de métal de transition, oxyde de composite de métal de transition ainsi préparé et oxyde de composite de lithium préparé en l'utilisant - Google Patents

Procédé de préparation d'un oxyde de composite de métal de transition, oxyde de composite de métal de transition ainsi préparé et oxyde de composite de lithium préparé en l'utilisant Download PDF

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WO2015016648A1
WO2015016648A1 PCT/KR2014/007082 KR2014007082W WO2015016648A1 WO 2015016648 A1 WO2015016648 A1 WO 2015016648A1 KR 2014007082 W KR2014007082 W KR 2014007082W WO 2015016648 A1 WO2015016648 A1 WO 2015016648A1
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metal salt
aqueous solution
composite oxide
solution
nickel
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PCT/KR2014/007082
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English (en)
Korean (ko)
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선양국
윤성준
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한양대학교 산학협력단
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Priority to CN201480042956.6A priority Critical patent/CN105594029B/zh
Priority to US14/909,035 priority patent/US10629903B2/en
Priority claimed from KR1020140098660A external-priority patent/KR101903827B1/ko
Publication of WO2015016648A1 publication Critical patent/WO2015016648A1/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
    • 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
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • 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
    • 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 preparing a transition metal composite oxide, and a transition metal composite oxide prepared by the same, and a lithium composite oxide prepared using the same, and more particularly, a basic solution added during preparation of a transition metal composite oxide by a coprecipitation reaction.
  • a method for preparing a transition metal composite oxide, and a transition metal composite oxide prepared by the same, and a lithium composite oxide prepared using the same and more particularly, a basic solution added during preparation of a transition metal composite oxide by a coprecipitation reaction.
  • Li-ion secondary batteries have been widely used as power sources for portable devices since they emerged in 1991 as small, lightweight, and large capacity batteries.
  • lithium ion secondary battery As a power source to drive these portable electronic information communication devices It is increasing day by day.
  • Commercially available small lithium ion secondary batteries use LiCoO 2 for the positive electrode and carbon for the negative electrode.
  • LiNiO 2, LiCo x Ni 1-x O 2 and LiMn 2 O 4 are the anode materials currently being actively researched and developed.
  • LiCoO 2 is an excellent material having stable charging and discharging characteristics and a flat discharge voltage characteristic.
  • CoCo has a low reserve, a high cost, and toxicity to humans.
  • LiNiO 2 is not commercialized because of difficulty in material synthesis and thermal stability, and LiMn 2 O 4 is commercialized in low-cost products.
  • LiMn 2 O 4 having a spinel structure has a theoretical capacity of 148 mAh / g, which is smaller than that of other materials, and has a three-dimensional tunnel structure.
  • LiCoO 2 and LiNiO 2 It is lower than LiCoO 2 and LiNiO 2 , and has poor cycle characteristics due to the Jahn-Teller effect.
  • high temperature characteristics (description) of 55 ° C. are inferior to LiCoO 2 and are not widely used in actual batteries.
  • the nickel-manganese-cobalt composite oxide is manufactured by the co-precipitation method, if the amount of nickel is increased, there is a problem that the density of primary particles decreases during initial seed formation and consequently, the tap density decreases.
  • the present invention to improve the coprecipitation reaction conditions by adjusting the concentration of the initial base added in the reactor according to the nickel content in the particles prepared before the coprecipitation reaction to solve the above problems can improve the particle density and tap density It is an object to provide a method for producing a lithium composite oxide and a lithium composite oxide produced thereby.
  • the present invention to solve the above problems
  • the first metal forming aqueous solution for internal formation, the chelating agent and the basic aqueous solution are continuously mixed with the reactor, and the nickel, cobalt and manganese have a constant concentration and a radius of r1 (0.2 um ⁇ r1 ⁇ 5 um).
  • the mixing ratio of the first aqueous metal salt solution for internal formation and the second aqueous metal salt solution for internal formation is gradually changed from 100 v%: 0 v% to 0 v%: 100 v% while being supplied while mixing and chelating agent and Mixing a basic aqueous solution into a reactor to form particles including a second inside having a radius r2 (r2 ⁇ 10 um) at the first inside periphery;
  • in the second step is to adjust the concentration of the basic aqueous solution in the reaction solution to be 0.25 g / L to 0.5 g / L method for producing a transition metal complex oxide.
  • the conditions of the coprecipitation reaction for supplying the aqueous metal salt solution are optimized by adjusting the concentration of the basic aqueous solution in the reactor to be 0.25 g / L to 0.5 g / L before supplying the aqueous metal salt solution into the reactor. do.
  • the basic aqueous solution is then supplied continuously during the preparation of the transition metal complex oxide.
  • the pH of the solution in the reactor in the second step is characterized in that it is adjusted to 11.8 to 12.3.
  • the concentration of nickel in the first aqueous solution for forming metal salts is controlled to 0.8 to 1 mol%.
  • the present inventors have found that the growth rate of seed may be higher than the growth rate of particles from each seem when the pH is 12.3 or more in the reactor before the aqueous metal salt solution is supplied. As a result, as a result, individual particles were not produced, but only a large amount of seeds were generated. As a result, the excessively generated seeds coagulated with each other, and the individual particles were found to have a problem of poor growth. It is a technical feature to adjust the pH in the reactor to 12.3 or less.
  • the basic aqueous solution and ammonia are preferably continuously supplied through the reaction process, and after adjusting the initial pH in the reactor, supplying an aqueous metal salt solution showing acidity to form particles. As the reaction proceeds, the pH in the reactor decreases.
  • D50 is 4 ⁇ m or less in the size distribution of particles formed after the reaction for 30 minutes by the first step to the fourth step. That is, the method for producing a lithium composite oxide according to the present invention controls the formation rate of the individual seed and the growth rate of the particles from the individual seed, by reacting for 30 minutes by the first step to the fourth step of the particles formed
  • the size distribution is characterized by adjusting the D50 to 4 ⁇ m or less.
  • the method further comprises a fifth step of drying or heat-treating the transition metal composite oxide obtained by performing the first step to the fourth step.
  • the average diameter of the transition metal composite oxide particles is characterized in that 5 to 10 ⁇ m.
  • the present invention also provides a transition metal composite oxide prepared by the production method of the present invention.
  • the present invention also provides a method for producing a lithium composite oxide, and a lithium composite oxide prepared thereby further comprising; a fifth step of mixing and heat-treating the lithium salt to the transition metal composite oxide prepared in the fourth step.
  • the average composition of the whole particles of the lithium composite oxide according to the present invention is characterized by the following formula (1).
  • the nickel content in the average composition of the whole particles of the lithium composite oxide produced by the present invention is characterized in that the high nickel to 0.5 or more.
  • the present invention also provides a method for preparing a first aqueous metal salt solution containing nickel, manganese and cobalt;
  • a mixing ratio of the first metal salt aqueous solution and the second metal salt aqueous solution is 0 v% or more and 100 v% or less.
  • the first metal salt aqueous solution and the second metal salt aqueous solution containing nickel, manganese and cobalt may be mixed in a separate reactor with a raw material solution containing nickel, manganese and cobalt, respectively. Can be prepared by the process.
  • the content of nickel in the first metal salt solution is x1
  • the content of manganese is y1
  • the content of cobalt is z1
  • the content of nickel in the solution of the second metal salt is x2.
  • the transition metal composite oxide prepared by the method for producing a transition metal composite oxide according to the present invention may have a structure in which the concentration of any one of nickel, manganese, and cobalt is kept constant.
  • x1 is 0.8 or more and 1.0 or less.
  • x2 is 0.8 or less.
  • a high capacity transition metal composite oxide having a high nickel content may be prepared by adjusting the content of nickel in the first metal salt aqueous solution.
  • the mixing ratio of the aqueous solution of the first metal salt and the aqueous solution of the second metal salt is gradually changed from 100 v%: 0 v% to 0v%: 100 v%. do.
  • the method for producing a transition metal composite oxide according to the present invention is characterized in that at least a part of the transition metal in the particles is produced such that a concentration gradient shows.
  • Method for producing a transition metal composite oxide according to the present invention is to prepare a third metal salt aqueous solution containing nickel, manganese and cobalt; And providing a second mixed metal salt solution, ammonia and a basic aqueous solution in which the first mixed metal salt aqueous solution and the third metal salt aqueous solution are mixed in the reactor, wherein the first mixed metal salt aqueous solution and the first mixed metal salt aqueous solution are mixed with each other.
  • the mixing ratio of the third metal salt aqueous solution is more than 0 v% and is characterized by being 100 v% or less.
  • the second mixed metal salt aqueous solution is provided, the mixing ratio of the first mixed metal salt aqueous solution and the third metal salt aqueous solution is 100 v%: 0 v% to 0 v %: 100 incrementally, up to and including v%.
  • transition metal composite oxide having two or more gradients of concentration gradients of nickel, manganese and cobalt in a particle by supplying the second mixed metal salt aqueous solution.
  • the content of nickel in the first mixed metal salt solution is x3, the content of manganese y3, the content of cobalt is z3, and the content of nickel in the third metal salt solution is x4.
  • Lithium composite oxide production method by adjusting the amount of the basic solution added according to the nickel content in the initial reaction conditions in the coprecipitation reaction by adjusting the pH in the reactor to improve the particle density and high tap density of high capacity lithium An ion secondary battery can be manufactured.
  • 1 and 2 show the results of measuring the precursor particle size and the precursor particle size distribution upon completion of the reaction 30 minutes after the start of the coprecipitation reaction according to one embodiment of the present invention.
  • 3 and 4 show the results of measuring a cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • 5 and 6 show the results of measuring the precursor particle size and the precursor particle size distribution upon completion of the reaction 30 minutes after the start of the coprecipitation reaction according to one embodiment of the present invention.
  • 7 and 8 show the results of measuring a cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • 9 and 10 show the results of measuring the precursor particle size and the precursor particle size distribution upon completion of the reaction 30 minutes after the start of the coprecipitation reaction according to one embodiment of the present invention.
  • 11 and 12 show the results of measuring the cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • 13 and 14 show the results of measuring the precursor particle size and the precursor particle size distribution upon completion of the reaction 30 minutes after the start of the coprecipitation reaction.
  • 15 and 16 show the results of measuring the cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • 17 and 18 show the results of measuring the precursor particle size and the precursor particle size distribution upon completion of the reaction 30 minutes after the start of the coprecipitation reaction according to one embodiment of the present invention.
  • 19 and 20 show the results of measuring a cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • 21 and 22 show the results of measuring the precursor particle size and the precursor particle size distribution at the completion of the reaction 30 minutes after the start of the coprecipitation reaction according to one embodiment of the present invention.
  • 23 and 24 show the results of measuring the cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • 25 and 26 show the results of measuring the precursor particle size and the precursor particle size distribution upon completion of the reaction 30 minutes after the start of the coprecipitation reaction according to one embodiment of the present invention.
  • 27 and 28 show the results of measuring a cross-sectional SEM photograph of the precursor and the active material prepared according to an embodiment of the present invention.
  • a surface portion forming solution having a composition ratio of Ni: Co: Mn of 60:15:25 was prepared, and the mixing ratio of the aqueous metal salt solution for forming the center portion and the aqueous metal salt solution for forming the surface portion was 100 v%: 0 v% to 0
  • the chelating agent and the basic aqueous solution were mixed and fed into the reactor while mixing while gradually changing to v%: 100 v% to prepare transition metal composite oxide particles.
  • the precursor and the lithium compound were reacted with each other and then fired to prepare active material particles.
  • SEM photographs of the cross sections of the prepared precursor particles and active material particles were measured and the results are shown in FIGS. 3 and 4. It can be seen from FIG. 3 and FIG. 4 that the inside of the particles forms a dense structure.
  • a central forming solution having a composition ratio of Ni: Co: Mn of 95: 2: 3 was prepared, the initial NaOH was added at a rate of 10 g per 2.5 L of distilled water to adjust the pH of the reaction solution to 11.9, followed by coprecipitation reaction.
  • a transition metal composite oxide particle having a radius of 0.2 ⁇ m was prepared.
  • a second -1 internal forming solution having a composition ratio of Ni: Co: Mn of 85: 6: 9 and a second -2 internal forming solution having a composition ratio of Ni: Co: Mn of 65:10:25 was prepared.
  • the mixing ratio of the metal salt aqueous solution for forming the core and the second -1 internal forming solution is gradually changed from 100 v%: 0 v% to 0v%: 100 v% to prepare the first mixed metal aqueous solution and simultaneously chelating
  • the first and basic aqueous solutions were mixed and supplied to the reactor, first to prepare a 2-1 interior on the first inner surface, and the mixing ratio of the first mixed metal aqueous solution and the second -2 internal forming solution was 100 v%: 0 gradually mixing from v% to 0v%: 100 v% to prepare a second mixed metal aqueous solution and supply it to the reactor, and simultaneously supply and supply the chelating agent and the basic aqueous solution to the reactor to provide the 2-1 inner surface with
  • the prepared precursor and the lithium compound were reacted and then fired to prepare active material particles.
  • SEM photographs of the cross-sections of the prepared precursor particles and active material particles were measured and the results are shown in FIGS. 7 and 8. It can be seen from FIG. 7 and FIG. 8 that the internal structure of the particles is compactly formed.
  • a first internal forming solution having a composition ratio of Ni: Co: Mn of 95: 2: 3 was prepared, the initial NaOH was added at a rate of 7 g per 2.5 L of distilled water to adjust the pH to 11.7, and then transferred by coprecipitation reaction.
  • Metal composite oxide particles were prepared.
  • D50 is formed to 4 ⁇ m or more in particle size and particle size distribution when the reaction is completed 30 minutes after the start of the coprecipitation reaction.
  • the prepared transition metal composite oxide particles and the lithium compound were reacted and then fired to prepare active material particles.
  • SEM photographs of the cross sections of the prepared precursor particles and active material particles were measured and the results are shown in FIGS. 11 and 12. It can be seen from FIG. 11 and FIG. 12 that the inside of the particles has a dense structure, and the largest number of particles exhibiting a 10 ⁇ m size in the particle size distribution.
  • a first internal forming solution having a composition ratio of Ni: Co: Mn of 95: 2: 3 was prepared, the initial NaOH was added at a rate of 7 g per 2.5 L of distilled water to adjust the pH to 11.7, and then radiused by coprecipitation. This 0.2 micrometer precursor particle
  • grains were manufactured.
  • a second internal forming solution having a composition ratio of Ni: Co: Mn of 95: 2: 3
  • a first mixed metal aqueous solution which is a mixed solution of the metal salt aqueous solution for forming the center portion and the second internal forming solution.
  • the mixing rate of the metal salt aqueous solution for forming the core and the second internal forming solution is gradually changed from 100 v%: 0 v% to 0v%: 100 v%, while mixing the chelating agent and the basic aqueous solution into the reactor.
  • transition metal composite oxide particles having a concentration gradient of nickel, manganese, and cobalt were prepared in the whole particle.
  • the D50 is adjusted to 4 ⁇ m or less in the particle size and particle size distribution when the reaction is completed 30 minutes after the start of the coprecipitation reaction.
  • the prepared transition metal composite oxide particles and the lithium compound were reacted and then fired to prepare active material particles.
  • SEM photographs of the cross sections of the prepared precursor particles and active material particles were measured and the results are shown in FIGS. 15 and 16. It can be seen from FIG. 15 and FIG. 16 that the inside of the particles has a dense structure.
  • a first internal forming solution having a composition ratio of Ni: Co: Mn of 96: 2: 2 was prepared and fed into the reactor.
  • Precursor particles were prepared by coprecipitation reaction.
  • the precursor and the lithium compound were reacted with each other and then fired to prepare active material particles. SEM photographs of the cross sections of the prepared precursor particles and active material particles were measured and the results are shown in FIGS. 19 and 20.
  • a first internal forming solution having a composition ratio of Ni: Co: Mn of 98: 1: 1 was prepared, the initial NaOH was added at a rate of 12 g per 2.5 L of distilled water, and then the pH was adjusted to 12.
  • a precursor particle having a size of 0.2 ⁇ m was prepared.
  • the mixing ratio of the metal salt aqueous solution for forming the core and the second -1 internal forming solution is gradually changed from 100 v%: 0 v% to 0v%: 100 v% to prepare and supply the first mixed metal aqueous solution.
  • the chelating agent and the basic aqueous solution were mixed and supplied to the reactor to first prepare a 2-1 interior on the first inner surface, and the mixing ratio of the second -1 internal forming solution and the second -2 internal forming solution was 100.
  • a third internal formation solution having a composition ratio of Ni: Co: Mn is 57:16:27, and a third interior having a constant concentration of nickel, manganese, and cobalt is formed outside the second-2 by coprecipitation.
  • precursor particles having a composition ratio of Ni: Co: Mn is 57:16:27, and a third interior having a constant concentration of nickel, manganese, and cobalt is formed outside the second-2 by coprecipitation.
  • the transition metal composite oxide particle size prepared at 30 minutes after the start of the coprecipitation reaction and the transition metal composite oxide particle size distribution at the completion of the reaction were measured and the results are shown in FIGS. 21 and 22.
  • the prepared transition metal composite oxide was reacted with a lithium compound and then fired to prepare active material particles.
  • the precursor and the lithium compound were reacted with each other and then fired to prepare active material particles. SEM photographs of the cross sections of the prepared precursor particles and active material particles were measured and the results are shown in FIGS. 27 and 28.
  • Lithium composite oxide production method by adjusting the amount of the basic solution added according to the nickel content in the initial reaction conditions in the coprecipitation reaction by adjusting the pH in the reactor to improve the particle density and high tap density of high capacity lithium An ion secondary battery can be manufactured.

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

Abstract

La présente invention concerne un procédé de préparation d'un oxyde de composite de lithium et un oxyde de composite de lithium ainsi préparé, et plus spécifiquement : un procédé de préparation d'un oxyde de composite de lithium, permettant de préparer une batterie secondaire au lithium-ion à haute capacité en ajustant la quantité d'une solution basique ajoutée en fonction de la teneur en nickel pendant la préparation d'un oxyde de composite de lithium par une réaction de co-précipitation, en ajustant ainsi le pH du réacteur et donc en améliorant la densité de particules et en augmentant la densité après tassement ; et un oxyde de composite de lithium ainsi préparé.
PCT/KR2014/007082 2013-07-31 2014-07-31 Procédé de préparation d'un oxyde de composite de métal de transition, oxyde de composite de métal de transition ainsi préparé et oxyde de composite de lithium préparé en l'utilisant WO2015016648A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201480042956.6A CN105594029B (zh) 2013-07-31 2014-07-31 转移金属复合氧化物的制造方法及根据其制造的转移金属复合氧化物及利用其制造的锂复合氧化物
US14/909,035 US10629903B2 (en) 2013-07-31 2014-07-31 Method for preparing transition metal composite oxide, transition metal composite oxide prepared thereby, and lithium composite oxide prepared using same

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KR10-2013-0091245 2013-07-31
KR20130091245 2013-07-31
KR1020140098660A KR101903827B1 (ko) 2013-07-31 2014-07-31 전이금속 복합 산화물의 제조 방법 및 이에 의하여 제조된 전이금속 복합 산화물 및 이를 이용하여 제조된 리튬 복합 산화물
KR10-2014-0098660 2014-07-31

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KR100752703B1 (ko) * 2006-06-29 2007-08-29 한양대학교 산학협력단 리튬 이차 전지용 양극 활물질, 그 제조 방법 및 그를사용한 리튬 이차 전지
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JP2009137834A (ja) * 2007-11-12 2009-06-25 Toda Kogyo Corp 非水電解液二次電池用Ｌｉ−Ｎｉ系複合酸化物粒子粉末及びその製造方法、並びに非水電解質二次電池
KR20120009891A (ko) * 2010-07-22 2012-02-02 주식회사 에코프로 리튬 이차전지용 양극활물질의 제조방법, 그에 의하여 제조된 리튬 이차전지용 양극활물질 및 그를 이용한 리튬 이차전지
KR20120084585A (ko) * 2011-01-20 2012-07-30 한양대학교 산학협력단 양극 활물질, 이의 제조 방법, 및 이를 포함하는 리튬 이차 전지

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