CN104332599B - The preparation method of a kind of lithium cobalt oxide solid solution presoma - Google Patents
The preparation method of a kind of lithium cobalt oxide solid solution presoma Download PDFInfo
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- CN104332599B CN104332599B CN201410639430.8A CN201410639430A CN104332599B CN 104332599 B CN104332599 B CN 104332599B CN 201410639430 A CN201410639430 A CN 201410639430A CN 104332599 B CN104332599 B CN 104332599B
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- 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
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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
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- 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
Abstract
A preparation method for lithium cobalt oxide solid solution presoma, comprises the following steps: (1) is according to proportioning CoyM1-yOz?xLiO1/2Take cobalt source, lithium source, M source, and it is dissolved in respectively in deionized water, gained solution is mixed; (2) being joined by mixing salt solution in the mixed solution of oleic acid, octadecylene, ethylene glycol, and keep heating and stir, the reaction times is 1-48h; (3) after stopped reaction, taking out filter under the atmosphere of air, collect reaction precipitation thing, then sinter at 100-700 DEG C of temperature, sintering time is 1-48h, to obtain final product. Preparation technology of the present invention is simple, the particle size of generation, morphology controllable, various elements in crystal grain are uniformly distributed, crystalline structure is stablized, the stability of structure when preparing the Lithium-ion embeding of the product in high voltage region and deviate from can be improved, it may also be useful to the cobalt acid lithium material of this precursor power has excellent cycle performance and safety performance.
Description
Technical field
The present invention relates to the preparation method of a kind of lithium cobalt oxide solid solution presoma.
Background technology
In recent years, people deepen continuously for the positive electrode material research of the lithium ion batteries such as cobalt oxidate for lithium, nickel oxidate for lithium, manganese oxidate for lithium, achieve many achievements, but owing to cobalt acid lithium has operating voltage height, and there is good cycle performance and safety performance, and it is easy to the series of advantages such as preparation, still cause the extensive concern of people, it is one of current business-like main lithium cell product.
The cobalt acid traditional production method of lithium be adopt the presoma containing cobalt and containing the presoma of lithium after physical mixed, then obtain through long-time high-temperature calcination. A series of shortcomings such as cobalt acid lithium exists uneven components, sintering temperature height, product reaction is incomplete, sintering time length, crystalline structure are unstable that this kind of method is prepared, finally can produce certain impact to the cycle performance of product and safety performance.
But the requirement of handheld device is constantly improved along with people, energy density and safety performance for lithium ion battery material are had higher requirement, need the preparation technology of cobalt acid lithium and presoma to be improved, ordinary process is all undertaken the presoma of the presoma of cobalt and lithium mixing, sintering preparation, but the sample that this kind of technique is prepared easily causes, and local lithium content is too high or disappearance, with when deviating from, the structural stability of material is deteriorated at high voltage region Lithium-ion embeding, finally affects the cycle performance of material.
Summary of the invention
The technical problem to be solved in the present invention is, overcoming the deficiencies in the prior art, it is provided that the preparation method of the simple lithium cobalt oxide solid solution presoma of a kind of preparation method, gained precursor power becomes battery, Lithium-ion embeding in high voltage region is with, when deviating from, structural stability is better.
It is that the preparation method of a kind of lithium cobalt oxide solid solution presoma, comprises the following steps that the present invention solves the technical scheme of its technical problem employing:
(1) according to proportioning CoyM1-yOz·xLiO1/2Take cobalt source, lithium source, M source, and it is dissolved in respectively in deionized water, be mixed with the solution that concentration is 0.1-1mol/L, gained solution mixed, obtains mixing salt solution;
The general formula Co of described lithium cobalt oxide solid solution presomayM1-yOz·xLiO1/2In, M is alkaline earth ion, for one or more of Ni, Mn, Al, Ti, Zr, Mg, V, Nb, Sb, Y, Yb, Ln (lanthanon), 0.5≤y≤1,0.8≤x≤1.2, z is the adjustment factor of Sauerstoffatom, relevant with sintering temperature, sintering temperature is more high, and z is more big, 1≤z≤1.5;
(2) step (1) gained mixing salt solution is joined in the mixed solution of oleic acid, octadecylene, ethylene glycol, in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:0.5-1.5:1-3 (preferred 2:1:2), and keep heating and stir, computer heating control temperature is 80-160 DEG C (preferred 140-160 DEG C), stirring velocity is 250-350r/min (preferred 300r/min), reaction times is 1-48h (preferred 10-24h), and the form of the precipitation that reaction system generates is lithium cobalt oleate;
(3) after stopped reaction, under the atmosphere of air, take out filter, collect reaction precipitation thing, then sinter at 100-700 DEG C of (preferably 400 DEG C-600 DEG C) temperature, sintering time is 1-48h (preferred 22-24h), obtains lithium cobalt oxide solid solution presoma.
Further, in step (1), described lithium source can be one or more of the carbonate of lithium, oxyhydroxide, acetate, oxalate, oxide compound, fluorochemical, muriate, nitrate or vitriol. Cobalt source can be one or more of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Cobaltous diacetate, cobalt chloride, cobaltous carbonate, cobaltous hydroxide, cobalt oxide or hydroxy cobalt oxide. M source can be one or more of the oxide compound of M, muriate or nitrate.
The present invention, using oleic acid as tensio-active agent, adopts organic solvent ethylene glycol and octadecylene to form uniform solution, adopts the synthesis of thermo-cracking synthesis method.
The size distribution of gained lithium cobalt oxide solid solution presoma of the present invention is at 100nm-25 μm (100 nanometers-25 microns), and shape looks are spherical vesicular structure.
Preparation technology of the present invention is simple, the particle size of generation, morphology controllable, various elements in crystal grain are uniformly distributed, crystalline structure is stablized, particularly prepare in production process at cobalt acid lithium, can effectively simplify and production technique, the stability of structure when can improve the Lithium-ion embeding of the product preparing in high voltage region and deviate from, it may also be useful to the cobalt acid lithium material of this precursor power has excellent cycle performance and safety performance.
Accompanying drawing explanation
Fig. 1 is gained lithium cobalt oxide solid solution presoma CoO in the embodiment of the present invention 14/3·LiO1/2Electronic scanning Electronic Speculum (SEM) photo, magnification is 1000 times;
Fig. 2 is CoO in the embodiment of the present invention 14/3·LiO1/2The cyclic curve of the battery being assembled into as positive electrode material after oversintering, wherein: charge-discharge magnification is 0.5C, charging/discharging voltage is 3.0-4.6V.
Fig. 3 is Co in the embodiment of the present invention 20.95Y0.01Al0.04O·LiO1/2Times rate curve of the battery being assembled into as positive electrode material after oversintering, wherein: rate of charge is 0.2C, and discharge-rate the 1 to 2 week is 0.2C, the 3rd week is 0.5C, and the 4th week is 1C, and the 5th week is 2C, and the 6th week is 5C; Charging/discharging voltage is 3.0-4.5V;
Fig. 4 is Co in the embodiment of the present invention 30.96Mg0.02Ti0.02O1.2·0.9LiO1/2The battery being assembled into as positive electrode material after oversintering cyclic curve, wherein: charge-discharge magnification is 1C, charging/discharging voltage is 3.0-4.5V.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) according to proportioning CoO4/3·LiO1/2Taking cobalt chloride, lithium nitrate, and be dissolved in respectively in deionized water, it is the lithium nitrate solution of 1mol/L, the cobalt chloride solution of 1mol/L that concentration is made in acid, is mixed by gained solution, obtains mixing salt solution;
(2) step (1) gained mixing salt solution is joined in the mixed solution of oleic acid, octadecylene, ethylene glycol, in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:1:2, and keep heating and stir, computer heating control temperature is 160 DEG C, stirring velocity is 300r/min, reaction times is 24h, and the form of the precipitation that reaction system generates is lithium cobalt oleate;
(3) after stopped reaction, taking out filter under the atmosphere of air, collect reaction precipitation thing, then sinter at the temperature of 500 DEG C, sintering time is 15h, obtains lithium cobalt oxide solid solution presoma CoO4/3·LiO1/2。
The present embodiment gained lithium cobalt oxide solid solution presoma CoO4/3·LiO1/2Middle particle diameter is 15.6 microns.
Product in the present embodiment is obtained positive active material through 950 DEG C of high temperature sintering 10h, positive electrode active materials, PVDF and acetylene black is pressed the mass ratio mixing of 94:3:3, adds NMP, stir and make slurry. Slurry is coated on aluminium foil, dry at 120 DEG C, make positive plate; Using metal lithium sheet as negative plate; Barrier film is the polypropylene microporous membrane (Celgard2400) of import; Electrolytic solution is 1mol/LLiPF6/ ethylene carbonate (EC)+dimethyl carbonate (DMC) (volume ratio 1:1), is assembled into CR2032 experimental button cell in glove box. The charge-discharge performance test of battery at room temperature carries out, the mode of first constant current constant voltage again is adopted to charge, charge cutoff voltage is 4.6V, adopt constant-current discharge, stopping potential is 3.0V, charging and discharging currents density is 0.5C multiplying power (contrast sample is that technique traditionally prepares presoma tricobalt tetroxide, and mixes with Quilonum Retard, adopts same method sintering and prepares battery).
Accompanying drawing 1 is CoO4/3·LiO1/2Electronic scanning Electronic Speculum (SEM) picture.
Fig. 2 is CoO in the present embodiment4/3·LiO1/2The cyclic curve of the battery being assembled into as positive electrode material after oversintering, wherein: charge-discharge magnification is 0.5C, charging/discharging voltage is 3.0-4.6V.
Embodiment 2
The present embodiment comprises the following steps:
(1) according to proportioning Co0.95Y0.01Al0.04O·LiO1/2Take lithium chloride, Cobaltous diacetate, aluminum nitrate, Yttrium trinitrate, and it is dissolved in respectively in deionized water, be mixed with the lithium chloride solution of 1mol/L, the cobalt acetate solution of 1mol/L, the aluminum nitrate solution of 0.1mol/L, the yttrium nitrate solution of 0.1mol/L, gained solution is mixed, obtains mixing salt solution;
(2) step (1) gained mixing salt solution is joined in the mixed solution of oleic acid, octadecylene, ethylene glycol, in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:1:3, and keep heating and stir, computer heating control temperature is 100 DEG C, stirring velocity is 320r/min, reaction times is 5h, and the form of the precipitation that reaction system generates is lithium cobalt oleate;
(3) after stopped reaction, taking out filter under the atmosphere of air, collect reaction precipitation thing, then sinter at the temperature of 300 DEG C, sintering time is 2h, obtains lithium cobalt oxide solid solution presoma.
The present embodiment gained lithium cobalt oxide solid solution presoma Co0.95Y0.01Al0.04O·LiO1/2Middle particle diameter is 0.35 micron, spherical porous structure.
Product in the present embodiment is obtained positive active material through 850 DEG C of high temperature sintering 10h, positive electrode active materials, PVDF and acetylene black is pressed the mass ratio mixing of 94:3:3, adds NMP, stir and make slurry. Slurry is coated on aluminium foil, dry at 120 DEG C, make positive plate; Using metal lithium sheet as negative plate; Barrier film is the polypropylene microporous membrane (Celgard2400) of import; Electrolytic solution is 1mol/LLiPF6/ ethylene carbonate (EC)+dimethyl carbonate (DMC) (volume ratio 1:1), is assembled into CR2032 experimental button cell in glove box.The charge-discharge performance test of battery at room temperature carries out, and adopts the mode of first constant current constant voltage again to charge, and charge cutoff voltage is 4.5V, adopts constant-current discharge, and stopping potential is 3.0V, and charging current density is 0.2C multiplying power. (contrast sample is that technique traditionally prepares presoma tricobalt tetroxide, and mixes with Quilonum Retard, aluminum nitrate, Yttrium trinitrate, adopts same method sintering and prepares battery)
Fig. 3 is Co in the present embodiment0.95Y0.01Al0.04O·LiO1/2The cyclic curve of the battery being assembled into as positive electrode material after oversintering, wherein: rate of charge is 0.2C, and discharge-rate the 1 to 2 week is 0.2C, the 3rd week is 0.5C, and the 4th week is 1C, and the 5th week is 2C, and the 6th week is 5C. Charging/discharging voltage is 3.0-4.5V.
Embodiment 3
The present embodiment comprises the following steps:
(1) according to proportioning Co0.96Mg0.02Ti0.02O1.2·0.9LiO1/2Take lithium nitrate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, magnesium chloride, Titanium Nitrate, and it is dissolved in respectively in deionized water, be configured to the lithium nitrate solution of 1mol/L, the cobalt nitrate solution of 1mol/L, the magnesium chloride solution of 0.1mol/L, the Titanium Nitrate solution of 0.1mol/L, gained solution is mixed, obtains mixing salt solution;
(2) step (1) gained mixing salt solution is joined in the mixed solution of oleic acid, octadecylene, ethylene glycol, in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:0.8:1.5, and keep heating and stir, control temperature is 160 DEG C, stirring velocity is 300r/min, reaction times is 24h, and the form of the precipitation that reaction system generates is lithium cobalt oleate;
(3) after stopped reaction, taking out filter under the atmosphere of air, collect reaction precipitation thing, then sinter at the temperature of 500 DEG C, sintering time is 7h, obtains lithium cobalt oxide solid solution presoma.
The present embodiment gained lithium cobalt oxide solid solution presoma Co0.96Mg0.02Ti0.02O1.2·0.9LiO1/2Middle particle diameter is 9.2 microns, spherical porous structure.
Product in the present embodiment is obtained positive active material through 900 DEG C of high temperature sintering 10h, positive electrode active materials, PVDF and acetylene black is pressed the mass ratio mixing of 94:3:3, adds NMP, stir and make slurry. Slurry is coated on aluminium foil, dry at 120 DEG C, make positive plate; Using metal lithium sheet as negative plate; Barrier film is the polypropylene microporous membrane (Celgard2400) of import; Electrolytic solution is 1mol/LLiPF6/ ethylene carbonate (EC)+dimethyl carbonate (DMC) (volume ratio 1:1), is assembled into CR2032 experimental button cell in glove box. The charge-discharge performance test of battery at room temperature carries out, and adopts the mode of first constant current constant voltage again to charge, and charge cutoff voltage is 4.5V, adopt constant-current discharge, stopping potential is 3.0V, and to be 1C multiplying power, first charge-discharge efficiency and specific discharge capacity be charging current density 93.8% and 188.8mAh/g. (contrast sample is that technique traditionally prepares presoma tricobalt tetroxide, and mixes with Quilonum Retard, magnesium chloride, Titanium Nitrate, adopts same method sintering and prepares battery).
Fig. 4 is Co in the present embodiment0.96Mg0.02Ti0.02O1.2·0.9LiO1/2The cyclic curve of the battery being assembled into as positive electrode material after oversintering, wherein: charge-discharge magnification is 1C, charging/discharging voltage is 3.0-4.5V.
Embodiment 4
The present embodiment comprises the following steps:
(1) according to proportioning Co0.94Zr0.01Yb0.01Ni0.04O4/3·1.1LiO1/2Take lithium nitrate, cobalt chloride, nickelous nitrate, zirconium nitrate, ytterbium nitrate, and be dissolved in respectively in deionized water, it is configured to the lithium nitrate solution of 1mol/L, the cobalt chloride solution of 1mol/L, the nickel nitrate solution of 0.1mol/L, the ytterbium nitrate solution of 0.1mol/L, the zirconium nitrate solution of 0.1mol/L, gained solution is mixed, obtains mixing salt solution;
(2) step (1) gained mixing salt solution is joined in the mixed solution of oleic acid, octadecylene, ethylene glycol, in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:1:1, and keep heating and stir, computer heating control temperature is 160 DEG C, stirring velocity is 300r/min, reaction times is 24h, and the form of the precipitation that reaction system generates is lithium cobalt oleate;
(3) after stopped reaction, taking out filter under the atmosphere of air, collect reaction precipitation thing, then sinter at the temperature of 600 DEG C, sintering time is 24h, obtains lithium cobalt oxide solid solution presoma Co0.94Zr0.01Yb0.01Ni0.04O4/3·1.1LiO1/2。
The present embodiment gained lithium cobalt oxide solid solution presoma Co0.94Zr0.01Yb0.01Ni0.04O4/3·1.1LiO1/2Co, Zr, Y, Ni, Li in crystal grain are uniformly distributed, and middle particle diameter is 11.62 microns.
Product in the present embodiment is obtained positive active material through 900 DEG C of high temperature sintering 10h, it is assembled into 063048 type rectangular cell, table 1 is that active material, PVDF and graphitized carbon black (are mixed by the mass ratio of 95.5:2.3:2.2, add NMP, stir and make slurry by battery testing data. Slurry is coated on aluminium foil, dry at 120 DEG C, make positive plate; It is assembled into 063048 type battery with negative plate, barrier film, electrolytic solution etc. The charge-discharge performance test of battery at room temperature carries out, and adopts the mode of first constant current constant voltage again to charge, and charge cutoff voltage is 4.35V, adopts constant-current discharge, and stopping potential is 3.0V, and charging current density is 0.5C multiplying power. Contrast sample is that technique traditionally prepares presoma tricobalt tetroxide, and mixes with Quilonum Retard, nickelous nitrate, zirconium nitrate, ytterbium nitrate, adopts same method sintering and the preparation of battery. In table, the detection method of hot case test preserves 0.5h under the high temperature of 150 DEG C, battery explosion or on fire, is NG, otherwise is then Pass. The detection method overcharging test is charged to 5V with the charging current of 1A, battery tympanites on fire or blast be then NG, otherwise be Pass. )
The full battery performance test data of products obtained therefrom in table 1 embodiment 4
Claims (10)
1. the preparation method of a lithium cobalt oxide solid solution presoma, it is characterised in that, comprise the following steps:
(1) according to proportioning CoyM1-yOz·xLiO1/2Take cobalt source, lithium source, M source, and it is dissolved in respectively in deionized water, be mixed with the solution that concentration is 0.1-1mol/L, gained solution mixed, obtains mixing salt solution;
The general formula Co of described lithium cobalt oxide solid solution presomayM1-yOz·xLiO1/2In, M is alkaline earth ion, is one or more of Ni, Mn, Al, Ti, Zr, Mg, V, Nb, Sb, Y, Yb, Ln, 0.5≤y≤1,0.8≤x≤1.2,1≤z≤1.5;
(2) step (1) gained mixing salt solution is joined in the mixed solution of oleic acid, octadecylene, ethylene glycol, in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:0.5-1.5:1-3, and keep heating and stir, control Heating temperature is 80-160 DEG C, stirring velocity is 250-350r/min, reaction times is 1-48h, and the form of the precipitation that reaction system generates is lithium cobalt oleate;
(3) after stopped reaction, taking out filter under the atmosphere of air, collect reaction precipitation thing, then sinter at 100-700 DEG C of temperature, sintering time is 1-48h, obtains lithium cobalt oxide solid solution presoma.
2. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1, it is characterised in that, in step (2), in described mixed solution, the mass ratio of oleic acid, octadecylene, ethylene glycol is 2:1:2.
3. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterised in that, in step (2), control Heating temperature is 140-160 DEG C.
4. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterised in that, in step (2), control stirring velocity is 300r/min.
5. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterised in that, in step (2), the control reaction times is 10-24h.
6. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterised in that, in step (3), sintering temperature is 400 DEG C-600 DEG C.
7. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterised in that, in step (3), sintering time is 22-24h.
8. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterized in that, in step (1), described lithium source is one or more of the carbonate of lithium, oxyhydroxide, acetate, oxalate, oxide compound, fluorochemical, muriate, nitrate or vitriol.
9. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterized in that, in step (1), cobalt source is one or more of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Cobaltous diacetate, cobalt chloride, cobaltous carbonate, cobaltous hydroxide, cobalt oxide or hydroxy cobalt oxide.
10. the preparation method of lithium cobalt oxide solid solution presoma according to claim 1 and 2, it is characterised in that, in step (1), M source is one or more of the oxide compound of M, muriate or nitrate.
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| CN107863526A (en) * | 2017-10-23 | 2018-03-30 | 兰州金川新材料科技股份有限公司 | A kind of preparation method for adulterating cobalt acid lithium |
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| CN1763997A (en) * | 2004-10-21 | 2006-04-26 | 北京化工大学 | Cobalt acid lithium battery material adulterated alkaline-earth metal between layers and its preparing method |
| CN101659447A (en) * | 2009-09-27 | 2010-03-03 | 武汉理工大学 | Method for synthesizing manganese oxide nano-particles in one step |
| CN101770868A (en) * | 2009-01-06 | 2010-07-07 | 中国科学院化学研究所 | Compound of metal/metal oxide and preparation method and application thereof |
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| CN1763997A (en) * | 2004-10-21 | 2006-04-26 | 北京化工大学 | Cobalt acid lithium battery material adulterated alkaline-earth metal between layers and its preparing method |
| CN101770868A (en) * | 2009-01-06 | 2010-07-07 | 中国科学院化学研究所 | Compound of metal/metal oxide and preparation method and application thereof |
| CN101659447A (en) * | 2009-09-27 | 2010-03-03 | 武汉理工大学 | Method for synthesizing manganese oxide nano-particles in one step |
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