CN105845927A - Preparation method of lithium ion battery cathode material lithium cobalt oxide - Google Patents
Preparation method of lithium ion battery cathode material lithium cobalt oxide Download PDFInfo
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- CN105845927A CN105845927A CN201610174790.4A CN201610174790A CN105845927A CN 105845927 A CN105845927 A CN 105845927A CN 201610174790 A CN201610174790 A CN 201610174790A CN 105845927 A CN105845927 A CN 105845927A
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- preparation
- lithium
- cobalto
- roasting
- lithium ion
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 16
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title abstract description 9
- 239000010406 cathode material Substances 0.000 title abstract description 7
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 title abstract 4
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 title abstract 4
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 15
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 26
- 229910052744 lithium Inorganic materials 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 15
- 239000010941 cobalt Substances 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 9
- 239000010405 anode material Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 230000004888 barrier function Effects 0.000 claims description 6
- 150000001868 cobalt Chemical class 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 2
- 239000005030 aluminium foil Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- DLHSXQSAISCVNN-UHFFFAOYSA-M hydroxy(oxo)cobalt Chemical compound O[Co]=O DLHSXQSAISCVNN-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000010416 ion conductor Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
Classifications
-
- 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
- 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
-
- 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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a preparation method of a lithium ion battery cathode material lithium cobalt oxide, wherein cobaltosic oxide is prepared through hydrothermal reaction and then is mixed with lithium carbonate, and finally the mixture is granulated to prepare the lithium cobalt oxide cathode material having excellent performance. The method is simple and convenient and the lithium cobalt oxide cathode material has excellent electrochemical performance.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to the preparation method of a kind of lithium ion cell anode material lithium cobaltate.
Background technology
Lithium ion battery is as a kind of emerging power supply, and it has the plurality of advantages such as voltage high, capacity big, memory-less effect, safety and environmental protection, is therefore extensively applied in secondary cell field.Cobalt acid lithium is owing to having high capacity characteristics, and its gram volume is up to 160 mAhg-1, it is a kind of commonly used anode material for lithium-ion batteries.
Chinese patent application 201510611765 discloses the preparation method of a kind of lithium ion conductor coated lithium ion battery cobalt acid lithium high-voltage positive electrode material, use hydro-thermal method cladding or use stirring at normal temperature method cladding, specifically including three steps: the preparation of oxalate precursor, oxide are coated with preparation and the preparation of lithium ion conductor cladding cobalt acid lithium material of oxalate precursor.The method can improve the bond strength between clad and principal phase cobalt acid lithium, and coating thickness is uniform, makes the high rate performance of lithium ion battery and cyclical stability obtain and significantly improve, especially high rate performance.
Chinese patent application 201310378779 discloses the preparation method of a kind of cobalt acid lithium, including: using cobalt salt solution and alkaline solution is reactant, it is stirred while being reacted in the control crystallization kettle have buffer agent by control crystallization process, prepares spherical hydroxy cobalt oxide；And this spherical hydroxy cobalt oxide is put in lithium hydroxide solution, hydrothermal reaction kettle carries out hydro-thermal reaction, makes the hydrogen in the lithium displacement hydroxy cobalt oxide in Lithium hydrate, generate spherical lithium cobalt.
But in the prior art, or highly desirable can find a kind of the most simple and convenient but also that positive electrode chemical property can be improved preparation method.
Summary of the invention
The invention provides the preparation method of a kind of lithium ion cell anode material lithium cobaltate, the method is implemented simple and convenient, and can be effectively improved the chemical property of cobalt acid lithium.
The present invention adopts the following technical scheme that the preparation method of a kind of lithium ion cell anode material lithium cobaltate, comprises the following steps:
(1) preparation of Cobalto-cobaltic oxide
Cobalt salt it is sequentially added into and containing NH in autoclave4+Solution, then it is incubated in 95 DEG C～105 DEG C of baking ovens 5h～14h, finally gained precipitation is i.e. obtained Cobalto-cobaltic oxide in air atmosphere kiln roasting after filtering, wash, drying；
(2) preparation of cobalt acid lithium
After step (1) gained Cobalto-cobaltic oxide is mixed abundant pelletize with lithium carbonate, in inert atmosphere stove, 800-900 DEG C of roasting 10-15h i.e. obtains lithium ion cell anode material lithium cobaltate.
Further, described cobalt salt concentration is 1-10 mol/L, containing NH4 +Solution concentration be 20-40 wt%.
Further, described containing NH4 +Solution selected from ammonia, carbamide, NH4One or more in F.
Further, the sintering temperature in step (1) is 300-400 DEG C, and roasting time is 2-5h.
Further, Cobalto-cobaltic oxide is 1:(1-3 with the mol of lithium carbonate).
Further, step (2) is roasted to 850 DEG C of roasting 12h in nitrogen atmosphere stove.
The present invention also protects a kind of button cell; using lithium cobaltate cathode material obtained above as positive electrode; with mass percent as positive electrode: acetylene black conductor: poly-inclined tetrafluoroethene binding agent=95:2.5:2.5 proportional arrangement form slurry, it is evenly applied on aluminium foil make positive plate；Then positive plate, barrier film, graphite cathode sheet are assembled them into button cell in the glove box of full argon gas atmosphere.
Further, its septation is celgard2400 film.
The present invention is mainly prepared for Cobalto-cobaltic oxide by hydro-thermal reaction, is then prepared for having high performance lithium cobaltate cathode material by later stage and lithium carbonate mixing granulation, and the method is implemented simple and convenient, and gained lithium cobaltate cathode material has preferable chemical property.
Detailed description of the invention
Below by embodiment, the present invention will be further described.
Embodiment one
Co (the NO of 10 mmol is added in 50mL polytetrafluoroethylliner liner autoclave3)2Solution 35 mL, is then added dropwise over the ammonia spirit of 25wt% until solution becomes clear solution in the case of stirring, and then autoclave is placed in the baking oven of 100 DEG C reaction 14h.By gained precipitation after filtering, wash, drying in air atmosphere stove 350 DEG C of roasting 2h Cobalto-cobaltic oxide.Then take gained Cobalto-cobaltic oxide 3.7g, 1.85g lithium carbonate mix after abundant pelletize in nitrogen atmosphere stove 850 DEG C of roasting 12h cobalt acid lithium.By gained cobalt acid lithium simulated battery, wherein negative pole is graphite, and barrier film is celgard2400 film, and button cell model is CR2025 type button cell.
Embodiment two
Difference from Example 1 is, take 1.17g Co (NO3) 2,1.2g carbamide and 40 mL distilled water in 50mL polytetrafluoroethylliner liner autoclave, be placed in 95 DEG C of baking ovens reaction 8h wait being sufficiently mixed after uniformly, then by gained precipitation after filtering, wash, drying in air atmosphere stove 350 DEG C of roasting 2h Cobalto-cobaltic oxide.Then it is mixed with 1.85g lithium carbonate after abundant pelletize in nitrogen atmosphere stove 850 DEG C of roasting 12h cobalt acid lithium.By gained cobalt acid lithium simulated battery, wherein negative pole is graphite, and barrier film is celgard2400 film, and button cell model is CR2025 type button cell.
Embodiment three
It is with embodiment 1 and 2 difference, takes 1.4 mmol cobalt nitrate solutions, 2.8 mmol
NH4F solution, 7 mmol
CO (NH2) 2 solution and 35 mL
Distilled water, in polytetrafluoroethylliner liner autoclave, puts it into insulation 5h in 105 DEG C of baking ovens wait being sufficiently mixed after uniformly, then by gained precipitation after filtering, wash, drying in air atmosphere stove 350 DEG C of roasting 2h Cobalto-cobaltic oxide.Then it is mixed with 1.85g lithium carbonate after abundant pelletize in nitrogen atmosphere stove 850 DEG C of roasting 12h cobalt acid lithium.By gained cobalt acid lithium simulated battery, wherein negative pole is graphite, and barrier film is celgard2400 film, and button cell model is CR2025 type button cell.
Above in conjunction with embodiment, the present invention is carried out exemplary description; obviously the realization of the present invention being not restricted to the described embodiments; if the various improvement that the method design that have employed the present invention is carried out with technical scheme; or the most improved design by the present invention and technical scheme directly apply to other occasion, the most within the scope of the present invention.
Claims (8)
1. the preparation method of a lithium ion cell anode material lithium cobaltate, it is characterised in that comprise the following steps:
(1) preparation of Cobalto-cobaltic oxide
Cobalt salt it is sequentially added into and containing NH in autoclave4 +Solution, then it is incubated in 95 DEG C～105 DEG C of baking ovens 5h～14h, finally gained precipitation is i.e. obtained Cobalto-cobaltic oxide in air atmosphere kiln roasting after filtering, wash, drying；
(2) preparation of cobalt acid lithium
After step (1) gained Cobalto-cobaltic oxide is mixed abundant pelletize with lithium carbonate, in inert atmosphere stove, 800-900 DEG C of roasting 10-15 i.e. obtains lithium ion cell anode material lithium cobaltate.
Preparation method the most according to claim 1, it is characterised in that described cobalt salt concentration is 1-10 mol/L, containing NH4 +Solution concentration be 20-40
wt%。
Preparation method the most according to claim 1, it is characterised in that described containing NH4 +Solution selected from ammonia, carbamide, NH4One or more in F.
Preparation method the most according to claim 1, it is characterised in that the sintering temperature in step (1) is 300-400 DEG C, roasting time is 2-5h.
Preparation method the most according to claim 1, it is characterised in that Cobalto-cobaltic oxide is 1:(1-3 with the mol of lithium carbonate).
Preparation method the most according to claim 1, it is characterised in that be roasted to 850 DEG C of roasting 12h in nitrogen atmosphere stove in step (2).
7. a button cell, it is characterized in that, cobalt acid lithium preparation method according to any one of claim 1-6 prepared is as positive electrode, with mass percent as positive electrode: acetylene black conductor: poly-inclined tetrafluoroethene binding agent=95:2.5:2.5 proportional arrangement form slurry, it is evenly applied on aluminium foil make positive plate；Then positive plate, barrier film, graphite cathode sheet are assembled them into button cell in the glove box of full argon gas atmosphere.
Button cell the most according to claim 7, it is characterised in that described barrier film is celgard2400 film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610174790.4A CN105845927A (en) | 2016-03-25 | 2016-03-25 | Preparation method of lithium ion battery cathode material lithium cobalt oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610174790.4A CN105845927A (en) | 2016-03-25 | 2016-03-25 | Preparation method of lithium ion battery cathode material lithium cobalt oxide |
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| Publication Number | Publication Date |
|---|---|
| CN105845927A true CN105845927A (en) | 2016-08-10 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610174790.4A Pending CN105845927A (en) | 2016-03-25 | 2016-03-25 | Preparation method of lithium ion battery cathode material lithium cobalt oxide |
Country Status (1)
| Country | Link |
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| CN (1) | CN105845927A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
| CN114702080A (en) * | 2022-03-17 | 2022-07-05 | 宜昌邦普时代新能源有限公司 | Preparation method and application of sea urchin-shaped lithium cobalt oxide |
| WO2023207247A1 (en) * | 2022-04-25 | 2023-11-02 | 广东邦普循环科技有限公司 | Porous spherical cobalt oxide particle and preparation method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1361061A (en) * | 2000-12-26 | 2002-07-31 | ***电子第十八研究所 | Prepn of cobalt-lithium oxide material |
| CN1485278A (en) * | 2002-09-27 | 2004-03-31 | 北京圣比和科技有限公司 | Preparation method for secondary crystal lithium cobalt acid of positive electrode material of lithium ion cell |
| CN1583576A (en) * | 2004-06-03 | 2005-02-23 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
-
2016
- 2016-03-25 CN CN201610174790.4A patent/CN105845927A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1361061A (en) * | 2000-12-26 | 2002-07-31 | ***电子第十八研究所 | Prepn of cobalt-lithium oxide material |
| CN1485278A (en) * | 2002-09-27 | 2004-03-31 | 北京圣比和科技有限公司 | Preparation method for secondary crystal lithium cobalt acid of positive electrode material of lithium ion cell |
| CN1583576A (en) * | 2004-06-03 | 2005-02-23 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
Non-Patent Citations (1)
| Title |
|---|
| XIAOLING XIAO等: ""Facile Synthesis of LiCoO2 Nanowires with High Electrochemical Performance"", 《NANO RES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
| CN114702080A (en) * | 2022-03-17 | 2022-07-05 | 宜昌邦普时代新能源有限公司 | Preparation method and application of sea urchin-shaped lithium cobalt oxide |
| WO2023207247A1 (en) * | 2022-04-25 | 2023-11-02 | 广东邦普循环科技有限公司 | Porous spherical cobalt oxide particle and preparation method therefor |
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