KR970042275A - Preparation method of ultra fine LiCoO_2 using sol-gel method - Google Patents

Preparation method of ultra fine LiCoO_2 using sol-gel method Download PDF

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KR970042275A
KR970042275A KR1019950052013A KR19950052013A KR970042275A KR 970042275 A KR970042275 A KR 970042275A KR 1019950052013 A KR1019950052013 A KR 1019950052013A KR 19950052013 A KR19950052013 A KR 19950052013A KR 970042275 A KR970042275 A KR 970042275A
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licoo
sol
nitrate
acetate
producing
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KR1019950052013A
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KR0146811B1 (en
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선양국
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윤종용
삼성전관 주식회사
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Priority to US08/768,560 priority patent/US5914094A/en
Priority to JP33914496A priority patent/JP4063350B2/en
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    • 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
    • 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
    • H01M4/52—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
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • 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
    • 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

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

Abstract

Li(CH3COOH)ㆍ2H2O와 Co(NO3)2ㆍ6H20를 1:1의 몰비로 정량하여 증류수에 녹인후 폴리아크릴산(PAA) 대 총 금속 이온 합의 몰비가 0.25 이상인 PAA 수용액을 만들어 상기 용액과 충분히 혼합하고, 혼합 수용애의 pH를 1~2로 조절하고,50~90℃에서 서서히 가열하여 졸로 만든 후 이 졸을 서서히 계속 가열하여 겔전구체를 제조하고, 이 겔젠구체를 300℃ 이상에서 1시간 이상 공기 분위기하에 열처리하여 전구체 분말을 제조하고, 이 전구체 분말을 400~900℃에서 1시간 이상 공기 분위기하에서 소성하여 LiCoO2분말을 제조하는 방법은 공정이 간단하고 경제적이며, 생성된 LiCoO2분말은 입자가 미세하고 비표면적이 커 리튬군 2차 전지의 양극물질로 우수한 물성을 나타낸다.Li (CH 3 COOH) · 2H 2 O and Co (NO 3 ) 2 ㆍ 6H 2 0 were dissolved in distilled water at a molar ratio of 1: 1 and dissolved in distilled water, and then aqueous solution of PAA having a molar ratio of polyacrylic acid (PAA) to total metal ion sum of 0.25 or more. The mixture was sufficiently mixed with the above solution, the pH of the mixed aqueous solution was adjusted to 1 to 2, gradually heated at 50 to 90 ° C. to form a sol, and the sol was gradually heated to prepare a gel precursor. The precursor powder is prepared by heat treatment at 300 ° C. or higher for 1 hour or longer in an air atmosphere, and the precursor powder is calcined at 400 to 900 ° C. for 1 hour or longer in an air atmosphere to prepare LiCoO 2 powder. The resulting LiCoO 2 powder exhibits excellent physical properties as a cathode material of a lithium group secondary battery with fine particles and a large specific surface area.

Description

졸-겔법을 이용한 초미세 LiCoO2의 제조방법Preparation method of ultra fine LiCoO2 using sol-gel method

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

제1도는 본 발명의 일 실시예에 따라 졸-겔법을 이용하여 LiCoO2를 제조하는 공정을 개략적으로 나타낸 제조 공정도.1 is a manufacturing process diagram schematically showing a process for producing LiCoO 2 using the sol-gel method according to an embodiment of the present invention.

제2도는 본 발명의 일 실시예에 따라 졸-겔법을 이용하여 LiCoO2를 제조할때 겔전구체로부터 세라믹스로의 변화 과정을 나타낸 TG-DTA그래프.2 is a TG-DTA graph showing a process of changing from gel precursor to ceramics when preparing LiCoO 2 using a sol-gel method according to an embodiment of the present invention.

Claims (14)

Li의 질산염 또는 초산염과, Co의 질산염 또는 초산염을 물에 용해시켜 제조한 금속염 수용액과 폴리아크릴산 수용액을 혼합하는 공정과; 혼합 수용액의 pH를 1~2로 조절하는 공정과; 혼합 수용액을 50~90℃에서 가열하여 졸을 형성하는 공정과; 형성된 졸을 50~90℃에서 가열하여 겔전구체를 형성하는 공정과; 형성된 겔전구체를 300℃ 이상에서 열처리하여 전구체 분말을 형성하는 공정과; 전구체 분말을 400~900℃에서 소성하는 공정을; 포함하는 LiCoO2의 제조방법.Mixing a nitrate or acetate of Li, a metal salt solution prepared by dissolving Co nitrate or acetate in water and an aqueous polyacrylic acid solution; Adjusting the pH of the mixed aqueous solution to 1-2; Heating the mixed aqueous solution at 50 ° C. to 90 ° C. to form a sol; Heating the formed sol at 50 ° C. to 90 ° C. to form a gel precursor; Heat-treating the formed gel precursor at 300 ° C. or higher to form precursor powder; Baking the precursor powder at 400 to 900 ° C; Method for producing LiCoO 2 comprising. 제 1 항에 있어서, 금속염 수용액은 Li(CH3COOH)ㆍ2H2O와 Co(NO3)2ㆍ6H20을 물에 녹인 것인 LiCoO2의 제조방법.The method for producing LiCoO 2 according to claim 1, wherein the aqueous metal salt solution dissolves Li (CH 3 COOH) .2H 2 O and Co (NO 3 ) 2 .6H 2 0 in water. 제 1 항에 있어서, Li의 질산염 또는 초산염과, Co의 질산염 또는 초산염과의 혼합 몰비는 1:1인 LiCoO2의 제조방법.The method for producing LiCoO 2 according to claim 1, wherein the mixing molar ratio of nitrate or acetate of Li and nitrate or acetate of Co is 1: 1. 제 1 항에 있어서, 전구체 분말의 소성온도는 400~600℃인 LiCoO2의 제조방법.The method of claim 1 wherein the firing temperature of the precursor powder A method of manufacturing a LiCoO 2 400 ~ 600 ℃. 제 1 항에 있어서, 상기한 혼합 용액에서 폴리아크릴산 대 총 금속 이온의 몰비는 0.25 이상인 LiCoO2의 제조방법.The method of claim 1, wherein the process for producing a mole ratio of polyacrylic acid ion to total metal in the mixed solution is LiCoO 2 not less than 0.25. 제 1 항에 있어서, 상기한 소성은 산화성 분위기에서 실시하는 것인 LiCoO2의 제조방법.The method for producing LiCoO 2 according to claim 1, wherein the firing is performed in an oxidizing atmosphere. 제 1 항에 있어서, 상기한 pH의 조절은 질산을 서서히 적가하여 실시하는 것인 LiCoO2의 제조방법.The method of claim 1, wherein the adjustment of the pH is a method of producing a LiCoO 2 to carried out slowly added dropwise nitric acid. Li의 질산염 또는 초산염과, Co의 질산염 또는 초산염을 물에 용해시켜 제조한 금속염 수용액과 폴리아크릴산 수용액을 혼합하는 공정과; 혼합 수용액의 pH를 1~2로 조절하는 공정과; 혼합 수용액을 50~90℃에서 가열하여 졸을 형성하는 공정을; 포함하는 LiCoO2졸의 제조방법.Mixing a nitrate or acetate of Li, a metal salt solution prepared by dissolving Co nitrate or acetate in water and an aqueous polyacrylic acid solution; Adjusting the pH of the mixed aqueous solution to 1-2; Heating the mixed aqueous solution at 50 ° C. to 90 ° C. to form a sol; Method for producing a LiCoO 2 sol comprising. Li의 질산염 또는 초산염과, Co의 질산염 또는 초산염을 물에 용해시켜 제조한 금속염 수용액과 폴리아크릴산 수용액을 혼합하는 공정과; 혼합 수용액의 pH를 1~2로 조절하는 공정과; 혼합 수용액을 50~90℃에서 가열하여 졸을 형성하는 공정과; 형성된 졸을 50~90℃에서 가열하여 겔전구체를 형성하는 공정을; 포함하는 LiCoO2겔전구체의 제조방법.Mixing a nitrate or acetate of Li, a metal salt solution prepared by dissolving Co nitrate or acetate in water and an aqueous polyacrylic acid solution; Adjusting the pH of the mixed aqueous solution to 1-2; Heating the mixed aqueous solution at 50 ° C. to 90 ° C. to form a sol; Heating the formed sol at 50 ° C. to 90 ° C. to form a gel precursor; Method for producing a LiCoO 2 gel precursor comprising. Li의 질산염 또는 초산염과, Co의 질산염 또는 초산염을 물에 용해시켜 제조한 금속염 수용액과 폴리아크릴산 수용액을 혼합하는 공정과; 혼합 수용액의 pH를 1~2로 조절하는 공정과; 혼합 수용액을 50~90℃에서 가열하여 졸을 형성하는 공정과; 상기 형성된 졸을 50~90℃에서 가열하여 겔전구체를 형성하는 공정과; 상기 형성된 겔전구체를 300℃ 이상에서 열처리하여 전구체 분말을 형성하는 공정을; 포함하는 LiCoO2전구체 분말의 제조방법.Mixing a nitrate or acetate of Li, a metal salt solution prepared by dissolving Co nitrate or acetate in water and an aqueous polyacrylic acid solution; Adjusting the pH of the mixed aqueous solution to 1-2; Heating the mixed aqueous solution at 50 ° C. to 90 ° C. to form a sol; Heating the formed sol at 50 ° C. to 90 ° C. to form a gel precursor; Heat treating the formed gel precursor at 300 ° C. or higher to form precursor powder; Method for producing a LiCoO 2 precursor powder comprising. 제 1 항의 방법에 의하여 생성된 LiCoO2. LiCoO produced by the method of claim 1 2. 제 7항의 방법에 의하여 생성된 LiCoO2졸.LiCoO 2 sol produced by the method of claim 7. 제8 항의 방법에 의하여 생성된 LiCoO2겔전구체.LiCoO 2 gel precursor produced by the method of claim 8. 제 9 항의 방법에 의하여 생성된 LiCoO2전구체 분말.LiCoO 2 precursor powder produced by the method of claim 9.
KR1019950052013A 1995-12-19 1995-12-19 Process for preparing lico02 using sol-gel method KR0146811B1 (en)

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KR1019950052013A KR0146811B1 (en) 1995-12-19 1995-12-19 Process for preparing lico02 using sol-gel method
US08/768,560 US5914094A (en) 1995-12-19 1996-12-17 Process for preparing cathode active material by a sol-gel method
JP33914496A JP4063350B2 (en) 1995-12-19 1996-12-19 Method for producing composite oxide using sol-gel method

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100485335B1 (en) * 2002-10-29 2005-04-27 한국과학기술연구원 Fabrication of lithium-cobalt oxide nano powder by surface modification of precursor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100485335B1 (en) * 2002-10-29 2005-04-27 한국과학기술연구원 Fabrication of lithium-cobalt oxide nano powder by surface modification of precursor

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