KR100795982B1 - 폴리올 프로세스를 이용한 전극재료 및 그 합성방법 - Google Patents
폴리올 프로세스를 이용한 전극재료 및 그 합성방법 Download PDFInfo
- Publication number
- KR100795982B1 KR100795982B1 KR1020070029199A KR20070029199A KR100795982B1 KR 100795982 B1 KR100795982 B1 KR 100795982B1 KR 1020070029199 A KR1020070029199 A KR 1020070029199A KR 20070029199 A KR20070029199 A KR 20070029199A KR 100795982 B1 KR100795982 B1 KR 100795982B1
- Authority
- KR
- South Korea
- Prior art keywords
- electrode material
- polyol
- mixed solution
- synthesizing
- polyol process
- Prior art date
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- 239000007772 electrode material Substances 0.000 title claims abstract description 47
- 238000004917 polyol method Methods 0.000 title claims abstract description 22
- 238000001308 synthesis method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- 229920005862 polyol Polymers 0.000 claims abstract description 24
- 150000003077 polyols Chemical class 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 12
- 239000002159 nanocrystal Substances 0.000 claims abstract description 11
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 150000002642 lithium compounds Chemical class 0.000 claims abstract description 9
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 32
- 239000010936 titanium Substances 0.000 claims description 26
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 20
- 229920001223 polyethylene glycol Polymers 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims description 11
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052596 spinel Inorganic materials 0.000 claims description 9
- 239000011029 spinel Substances 0.000 claims description 9
- 229910018071 Li 2 O 2 Inorganic materials 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- FDLZQPXZHIFURF-UHFFFAOYSA-N [O-2].[Ti+4].[Li+] Chemical compound [O-2].[Ti+4].[Li+] FDLZQPXZHIFURF-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000007773 negative electrode material Substances 0.000 claims 1
- 239000007774 positive electrode material Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- -1 Ta 2 O 5 Inorganic materials 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- 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
-
- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
Claims (11)
- 폴리올(polyols)용매에 티타늄계 화합물 및 리튬계 화합물용액을 혼합한 혼합용액을 제조하는 단계; 및상기 혼합용액을 리플럭스(reflux)장치에서 반응시켜 반응결과물을 얻어내되, 상기 리플럭스장치내의 온도가 상기 폴리올용매의 끓는점에 도달하게 되면 상기 혼합용액 내의 상기 리튬계화합물이 분해됨과 함께 상기 티타늄계화합물과 반응하여 나노결정의 스피넬(Spinel)구조를 갖는 리튬-티타늄계 산화물인 반응결과물을 얻어내는 단계;를 포함하며,나노결정의 스피넬구조를 갖는 전극재료를 합성하는데에 반응결과물의 열처리공정이 필요하지 않은 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 항에 있어서,상기 나노결정의 스피넬구조를 갖는 반응결과물을 얻어내는 단계; 후에상기 혼합용액을 세정하여 반응하고 남은 폴리올용매을 제거하는 단계:상기 결과물을 필터링하는 단계; 및상기 결과물을 건조시키는 단계;를 더 포함하는 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 또는 제 2 항에 있어서,상기 폴리올용매는 EG(Ethylene Glycol), EOH(Ethanol), DEG(Diethylene Glycol), TEG(Triethylene Glycol), TTEG(Tetraethylene Glycol) 및 TtEg(Tetratethylene Glycol)으로 이루어진 군에서 선택된 어느 하나인 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 또는 제 2 항에 있어서,상기 티타늄계 화합물은 TTIP(Titanium Tetra-isopropoxide) 또는 TiCl인 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 또는 제 2 항에 있어서,상기 리튬계 화합물은 Li2O2 또는 CH3COOLi인 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 또는 제 2 항에 있어서,상기 나노결정구조의 스피넬구조를 갖는 결과물은 Li4Ti5O12인 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 또는 제 2 항에 있어서,상기 혼합용액을 리플럭스장치에서 반응시켜 나노결정의 스피넬구조를 갖는 결과물을 얻어내는 단계;는상기 혼합용액을 상기 폴리올용매의 끓는점에서 가열하여 수행하는 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 7 항에 있어서,상기 혼합용액을 40 내지 50시간 동안 반응시키는 것을 특징으로 하는 폴리올 프로세스를 이용한 전극재료의 합성방법.
- 제 1 항 또는 제 2 항의 합성방법에 의해 합성되는 전극재료.
- 제 9 항에 있어서,상기 합성된 전극재료의 입자의 직경은 5 내지 50nm인 것을 특징으로 하는 전극재료.
- 제 9 항에 있어서,상기 합성된 전극재료는 2차 전지의 양극 또는 음극재료로 이용되는 것을 특징으로 하는 전극재료.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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KR1020070029199A KR100795982B1 (ko) | 2007-03-26 | 2007-03-26 | 폴리올 프로세스를 이용한 전극재료 및 그 합성방법 |
Applications Claiming Priority (1)
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KR1020070029199A KR100795982B1 (ko) | 2007-03-26 | 2007-03-26 | 폴리올 프로세스를 이용한 전극재료 및 그 합성방법 |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
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KR1020050105353 Division | 2005-11-04 |
Publications (2)
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KR20070048675A KR20070048675A (ko) | 2007-05-09 |
KR100795982B1 true KR100795982B1 (ko) | 2008-01-21 |
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KR1020070029199A KR100795982B1 (ko) | 2007-03-26 | 2007-03-26 | 폴리올 프로세스를 이용한 전극재료 및 그 합성방법 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100999163B1 (ko) * | 2010-04-15 | 2010-12-07 | 전남대학교산학협력단 | 초급속연소법을 이용한 나노전극재료 합성방법 및 그 방법으로 합성된 나노전극재료 |
WO2012138158A2 (ko) * | 2011-04-05 | 2012-10-11 | 전남대학교산학협력단 | 폴리올 프로세스를 이용한 리튬화된 전극재료제조방법, 그 방법으로 제조된 리튬화된 전극재료 및 상기 전극재료를 포함하는 2차전지 |
KR101533770B1 (ko) * | 2012-12-05 | 2015-07-03 | (주)에너지와공조 | 화염 분무 방사 열 합성 방법을 이용한 나노 전극 재료 합성 방법 및 이 방법을 의한 화염 분무 방사 합성 장치 |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101134474B1 (ko) | 2009-12-03 | 2012-04-13 | 전남대학교산학협력단 | 급속 충방전이 가능한 리튬 이차전지용 고용량 음극소재 및 그 제조 방법 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH1167204A (ja) * | 1997-08-08 | 1999-03-09 | Fine Ceramics Gijutsu Kenkyu Kumiai | 非水電解液二次電池の正極活物質の製造方法 |
-
2007
- 2007-03-26 KR KR1020070029199A patent/KR100795982B1/ko active IP Right Grant
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH1167204A (ja) * | 1997-08-08 | 1999-03-09 | Fine Ceramics Gijutsu Kenkyu Kumiai | 非水電解液二次電池の正極活物質の製造方法 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100999163B1 (ko) * | 2010-04-15 | 2010-12-07 | 전남대학교산학협력단 | 초급속연소법을 이용한 나노전극재료 합성방법 및 그 방법으로 합성된 나노전극재료 |
WO2012138158A2 (ko) * | 2011-04-05 | 2012-10-11 | 전남대학교산학협력단 | 폴리올 프로세스를 이용한 리튬화된 전극재료제조방법, 그 방법으로 제조된 리튬화된 전극재료 및 상기 전극재료를 포함하는 2차전지 |
WO2012138158A3 (ko) * | 2011-04-05 | 2013-03-28 | 전남대학교산학협력단 | 폴리올 프로세스를 이용한 리튬화된 전극재료제조방법, 그 방법으로 제조된 리튬화된 전극재료 및 상기 전극재료를 포함하는 2차전지 |
KR101533770B1 (ko) * | 2012-12-05 | 2015-07-03 | (주)에너지와공조 | 화염 분무 방사 열 합성 방법을 이용한 나노 전극 재료 합성 방법 및 이 방법을 의한 화염 분무 방사 합성 장치 |
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KR20070048675A (ko) | 2007-05-09 |
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