CN104167542A - Nickel-cobalt-lithium manganate powder of lithium battery positive electrode material and preparation method of nickel-cobalt-lithium manganate powder - Google Patents
Nickel-cobalt-lithium manganate powder of lithium battery positive electrode material and preparation method of nickel-cobalt-lithium manganate powder Download PDFInfo
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- CN104167542A CN104167542A CN201410383729.1A CN201410383729A CN104167542A CN 104167542 A CN104167542 A CN 104167542A CN 201410383729 A CN201410383729 A CN 201410383729A CN 104167542 A CN104167542 A CN 104167542A
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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
- H01M4/50—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
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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
- 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
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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
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Abstract
The invention discloses nickel-cobalt-lithium manganate powder of a lithium battery positive electrode material and a preparation method of the nickel-cobalt-lithium manganate powder. According to the preparation method, reaction raw materials are heated by microwaves, the reaction raw materials consume the energy of an electromagnetic field, so as to generate heat, and electromagnetic energy directly acts on medium molecules, so as to be converted into heat energy. Therefore, the nickel-cobalt-lithium manganate powder can be prepared without high-temperature heating. The preparation method of the nickel-cobalt-lithium manganate powder has the advantages of simplicity in operation and equipment, short heating time, low energy consumption, short synthesizing period, uniformity in heating reaction and easiness in obtaining.
Description
Technical field
The present invention relates to a kind of lithium ion battery field, be specifically related to a kind of nickle cobalt lithium manganate powder and preparation method thereof.
Background technology
Lithium ion battery is new green environment protection power supply, has high energy density, the high advantages such as discharge platform, is widely used in the electronic products such as mobile phone, camera, notebook computer.Along with the development of digital product industry, people increase day by day to the demand of battery.
The positive electrode of lithium battery is the important component part of lithium battery, is the major effect factor of lithium battery performance, and present business-like positive electrode mainly contains cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate and LiFePO4.In recent years, because the price of nickle cobalt lithium manganate is high compared with low and high energy metric density, good cycle, voltage platform, Heat stability is good, have extended cycle life, crystal structure is desirable, self discharge is little, memory-less effect, specific capacity be compared with advantages of higher, the scope of application is more and more wider.
The preparation method of nickle cobalt lithium manganate adopts high temperature solid phase synthesis, coprecipitation, common hydro thermal method, solution-gel method conventionally.At present, use traditional high temperature solid-state method to be difficult to synthesize the nickle cobalt lithium manganate of pure phase; Use the reaction process of the synthetic nickle cobalt lithium manganate of coprecipitation, common hydro thermal method and solution-gel method many, the reaction time is long, and complex operation.
Summary of the invention
The object of this invention is to provide a kind of method of preparing nickle cobalt lithium manganate powder by microwave method.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
The present invention adopts microwave method to prepare nickle cobalt lithium manganate, that dielectric material is comprised of polar molecule and nonpolar molecule, under the effect of electromagnetic field, these polar molecules are the polarity oriented according to electric field from original random distribution state shift, and under the effect of electromagnetic field of high frequency, these orientations constantly change by the frequency of alternating electromagnetism, thereby this process causes the motion of molecule and phase mutual friction to produce heat, now the field energy of alternating electric field is converted into the heat energy in medium, and medium temperature is constantly raise; And transmission performance is heated the inside and outside medium of calandria simultaneously, do not need heat conduction, and the inner radiating condition that lacks causes internal temperature higher than outside temperature gradient distribution.
The present invention proposes a kind of preparation method of anode material of lithium battery nickle cobalt lithium manganate powder, and concrete steps are as follows:
A, the preparation of solution
By analyzing pure cerium hydroxide lithium, be dissolved in and in deionized water, be mixed with the lithium hydroxide solution that the ratio of lithium hydroxide amount of substance and deionized water amount of substance is 0.1-0.15:1; By nickelous sulfate, cobaltous sulfate, manganese sulfate and potassium permanganate are dissolved in deionized water with the ratio 4-5.5:4-6:1.5-2.5:2-4 mixing of amount of substance, and preparation is called mixed solution;
B, microwave method reaction
The ratio that is 1:1-5 in the ratio of nickel ion, cobalt ions and manganese ion amount of substance sum and the amount of substance of lithium ion slowly joins lithium hydroxide solution in mixed solution, after stirring, in microwave oven, with 150-200 ℃ of temperature, heat 30-60min, naturally cooling, filter, filter residue is with after deionized water washing, dry, obtain nickle cobalt lithium manganate powder sample.
In described steps A, lithium hydroxide adds after mixed solution, and with rotating speed, 500-700rpm stirs.
In described steps A, lithium hydroxide adds after mixed solution, at 80-100 ℃, stirs.
In described step B, microwave oven is multimode cavity microwave oven.
After stirring in described step B, in microwave oven, with power 1500W, heat.
In described step B, with filter opening 0.05nm filter membrane, filter.
The deionized water washing of 2-4L for filter residue in described step B.
Dry at 60-80 ℃ in described step B.
Dry 1-4 hour in described step B.
An anode material of lithium battery nickle cobalt lithium manganate powder that adopts described preparation method to prepare, its purity is 90%-96%, specific discharge capacity is 148.7-160.7mAh/g.
To explain the present invention below.
A preparation method for anode material of lithium battery nickle cobalt lithium manganate powder, concrete steps are as follows:
A, the preparation of solution
Lithium hydroxide is dissolved in and in deionized water, is mixed with the lithium hydroxide solution that the ratio of lithium hydroxide amount of substance and deionized water amount of substance is 0.1-0.15:1; By nickelous sulfate, cobaltous sulfate, manganese sulfate and potassium permanganate are dissolved in deionized water with the ratio 4-5.5:4-6:1.5-2.5:2-4 mixing of amount of substance, and preparation is called mixed solution.
B, microwave method reaction
The ratio that is 1:1-5 in the ratio of nickel ion, cobalt ions and manganese ion amount of substance sum and the amount of substance of lithium ion slowly joins lithium hydroxide solution in mixed solution, after stirring, in microwave oven, with 150-200 ℃ of temperature, heat 30-60min, naturally cooling, filter, filter residue is with after deionized water washing, dry, obtain nickle cobalt lithium manganate powder sample.
Analyzing pure is the pureness specifications of chemical reagent, is that main component content is very high, purity is higher, disturbs impurity very low, is applicable to the pureness specifications of proximate analysis and chemical experiment.The pure standard of analysis of different reagent is different; Some are easily purified, not perishable reagent, analyze pure require high.
The molecular formula of nickle cobalt lithium manganate is: LiNi
xco
ymn
1-x-yo
2, therefore, in reaction equation, the ratio of the amount of substance sum of nickel ion, cobalt ions and manganese ion and the amount of substance of lithium ion should be 1:1.But, for abundant reaction, simultaneously in order to guarantee in course of reaction always, in alkaline environment, need the amount of more lithium ion.In the present invention, the ratio of the amount of substance sum of nickel ion, cobalt ions and manganese ion and the amount of substance of lithium ion removes 1:1-5.
Naturally cooling is that other the type of cooling may be destroyed the structure of reactant in order to allow possible low temperature think change fully.
In described steps A, lithium hydroxide adds after mixed solution, and with rotating speed, 500-700rpm stirs.
The too high crystal that easily makes of rotating speed is separated out; Rotating speed is too low can make again to dissolve insufficient.
In described steps A, lithium hydroxide adds after mixed solution, at 80-100 ℃, stirs.
Excess Temperature may cause some volatile substances in raw material; The character of the too low impact reaction of temperature.
Reaction stirred at suitable rotating speed and temperature only, could obtain the nickle cobalt lithium manganate powder of high-purity, high-crystallinity.
In described step B, microwave oven is multimode cavity microwave oven.
Multimode cavity microwave oven refers to that microwave is in the reflection of resonant cavity inside, makes formation multiple work " pattern " in resonant cavity.Pattern in resonant cavity is more, and the distributed architecture of electromagnetic field is just more, and the microwave in resonant cavity is more evenly distributed.One-mode cavity microwave oven will reach the needed power of industrial processes, must adopt powerful microwave generator; But multimode cavity microwave oven can pass through the combination of low power microwave generator, realize the object of HIGH-POWERED MICROWAVES processing.Like this, not only power supply is equipped with and requires to reduce, and can adopt a simple minute cooling system to realize cooling; And the cost of microwave generator also reduces greatly.
After stirring in described step B, in microwave oven, with power 1500W, heat.
In described step B, with filter opening 0.05nm filter membrane, filter.
The deionized water washing of 2-4L for filter residue in described step B.
Dry at 60-80 ℃ in described step B.
Dry 1-4 hour in described step B.
Adopt at present high temperature solid phase synthesis, coprecipitation, common hydro thermal method, solution-gel method or some improved methods as the method that sol-gel process and template combine, all want to calcine 5-20h at 600-900 ℃; And preparation method of the present invention only need to react 30-60min at 150-200 ℃, reaction temperature is low, and the reaction time is short.
An anode material of lithium battery nickle cobalt lithium manganate powder that adopts described preparation method to prepare, its purity is 90%-96%, specific discharge capacity is 148.7-160.7mAh/g.
The nickle cobalt lithium manganate purity that the present invention obtains is greater than 90%.
Performance Detection mode of the present invention is as follows:
Take lithium metal as negative pole, and nickle cobalt lithium manganate prepared by the present invention of take, as anodal, is assembled into battery, carries out discharge test, electric discharge specific capacity with 0.1C multiplying power.
The present invention compared with prior art, has following beneficial effect:
1, the present invention heats that synthesis temperature is low, firing rate is fast, heating uniformity is good, efficient energy-saving, synthesis cycle are short;
2, material of the present invention is simple and easy to get, and reactions steps is simple, greatly reduces complex operation degree, is conducive to promote the production development of nickle cobalt lithium manganate; And consersion unit of the present invention is simple, has saved production cost;
3, reaction easy operating of the present invention, pollution-free, alternative heating;
4, the nickle cobalt lithium manganate purity that the present invention obtains is up to 96%.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates that embodiment 1 makes nickle cobalt lithium manganate powder;
Fig. 2 is the SEM collection of illustrative plates that embodiment 1 makes nickle cobalt lithium manganate powder.
Embodiment
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
By analyzing pure cerium hydroxide lithium, be dissolved in and in deionized water, be mixed with the lithium hydroxide solution that the ratio of lithium hydroxide amount of substance and deionized water amount of substance is 0.1:1; By nickelous sulfate, cobaltous sulfate, manganese sulfate and potassium permanganate are dissolved in deionized water with the ratio 5.5:4:2.5:2 mixing of amount of substance, and preparation is called mixed solution;
The ratio that is 1:5 in the ratio of nickel ion, cobalt ions and manganese ion amount of substance sum and the amount of substance of lithium ion slowly joins lithium hydroxide solution in mixed solution, after stirring with 700rpm at 100 ℃ in multimode cavity microwave oven with 200 ℃ of heating 40min of power 1500W, temperature, naturally cooling, 0.05nm membrane filtration, after the deionized water washing of filter residue with 4L, 80 ℃ are dried 1 hour, obtain nickle cobalt lithium manganate powder sample.
The nickle cobalt lithium manganate powder sample purity obtaining is 94%, and specific discharge capacity is 160.7mAh/g.
Use DX2700X x ray diffractometer x test gained nickle cobalt lithium manganate powder, result is as shown in the XRD collection of illustrative plates of Fig. 1, peak position by collection of illustrative plates is calculated with least square method, the lattice constant obtaining is a=0.285nm, c=1.4251nm, similar with the lattice constant of nickle cobalt lithium manganate, therefore can confirm that sample is nickle cobalt lithium manganate; And the nickle cobalt lithium manganate powder obtaining does not have dephasign, and the very high diffraction maximum of purity is very sharp-pointed, thereby nickle cobalt lithium manganate good crystallinity.
Use scanning electron microscope observation sample topography, result is as shown in the SEM collection of illustrative plates of Fig. 2, and the nickle cobalt lithium manganate powder of gained mostly is sheet and class is spherical, and this pattern is more conducive to the performance of its chemical property, has better capacity and cycle performance.
Embodiment 2
By analyzing pure cerium hydroxide lithium, be dissolved in and in deionized water, be mixed with the lithium hydroxide solution that the ratio of lithium hydroxide amount of substance and deionized water amount of substance is 0.15:1; By nickelous sulfate, cobaltous sulfate, manganese sulfate and potassium permanganate are dissolved in deionized water with the ratio 4:5:2:4 mixing of amount of substance, and preparation is called mixed solution;
The ratio that is 1:1 in the ratio of nickel ion, cobalt ions and manganese ion amount of substance sum and the amount of substance of lithium ion slowly joins lithium hydroxide solution in mixed solution, after stirring with 500rpm at 80 ℃ in multimode cavity microwave oven with 150 ℃ of heating 60min of power 1500W, temperature, naturally cooling, 0.05nm membrane filtration, after the deionized water washing of filter residue with 3L, 70 ℃ are dried 3 hours, obtain nickle cobalt lithium manganate powder sample.
The nickle cobalt lithium manganate powder sample purity obtaining is 92%, and specific discharge capacity is 155.1mAh/g.
Embodiment 3
By analyzing pure cerium hydroxide lithium, be dissolved in and in deionized water, be mixed with the lithium hydroxide solution that the ratio of lithium hydroxide amount of substance and deionized water amount of substance is 0.13:1; By nickelous sulfate, cobaltous sulfate, manganese sulfate and potassium permanganate are dissolved in deionized water with the ratio 5:6:1.5:3 mixing of amount of substance, and preparation is called mixed solution;
The ratio that is 1:4 in the ratio of nickel ion, cobalt ions and manganese ion amount of substance sum and the amount of substance of lithium ion slowly joins lithium hydroxide solution in mixed solution, after stirring with 650rpm at 95 ℃ in multimode cavity microwave oven with 180 ℃ of heating 32min of power 1500W, temperature, naturally cooling, 0.05nm membrane filtration, after the deionized water washing of filter residue with 4L, 60 ℃ are dried 4 hours, obtain nickle cobalt lithium manganate powder sample.
The nickle cobalt lithium manganate powder sample purity obtaining is 96%, and specific discharge capacity is 148.7mAh/g.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only preferably execution mode of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and execution modes, and these are revised and within execution mode will drop on the disclosed principle scope and spirit of the application.
Claims (10)
1. a preparation method for anode material of lithium battery nickle cobalt lithium manganate powder, is characterized in that concrete steps are as follows:
A, the preparation of solution
By analyzing pure cerium hydroxide lithium, be dissolved in and in deionized water, be mixed with the lithium hydroxide solution that the ratio of lithium hydroxide amount of substance and deionized water amount of substance is 0.1-0.15:1; Ratio 4-5.5:4-6:1.5-2.5:2-4 mixing by nickelous sulfate, cobaltous sulfate, manganese sulfate and potassium permanganate with amount of substance is dissolved in deionized water, and preparation is called mixed solution;
B, microwave method reaction
The ratio that is 1:1-5 in the ratio of nickel ion, cobalt ions and manganese ion amount of substance sum and the amount of substance of lithium ion slowly joins lithium hydroxide solution in mixed solution, after stirring, in microwave oven, with 150-200 ℃ of temperature, heat 30-60min, naturally cooling, filter, filter residue is with after deionized water washing, dry, obtain nickle cobalt lithium manganate powder sample.
2. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that in steps A, lithium hydroxide adds after mixed solution, and with rotating speed, 500-700rpm stirs.
3. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that in steps A, lithium hydroxide adds after mixed solution, at 80-100 ℃, stirs.
4. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that in step B, microwave oven is multimode cavity microwave oven.
5. the preparation method of nickle cobalt lithium manganate powder according to claim 1 heats with power 1500W after it is characterized in that stirring in step B in microwave oven.
6. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that with filter opening 0.05nm filter membrane, filtering in step B.
7. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that the deionized water washing of 2-4L for filter residue in step B.
8. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that in step B dry at 60-80 ℃.
9. the preparation method of nickle cobalt lithium manganate powder according to claim 1, is characterized in that dry 1-4 hour in step B.
10. the anode material of lithium battery nickle cobalt lithium manganate powder that prepared by the preparation method described in claim 1-9 any one claim, the purity that it is characterized in that this powder is 90%-96%, specific discharge capacity is 148.7-160.7mAh/g.
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| CN103137962A (en) * | 2013-03-11 | 2013-06-05 | 佛山市邦普循环科技有限公司 | Method for preparing nickel-cobalt-manganese hydroxide |
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Patent Citations (3)
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| CN101830451A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Microwave hydro-thermal synthesis method of olivine type lithium ion battery positive pole material manganese lithium phosphate |
| CN101699639A (en) * | 2009-07-01 | 2010-04-28 | 北京高盟化工有限公司 | Method for preparing carbon-coated nano-grade lithium iron phosphate composite anode material |
| CN103137962A (en) * | 2013-03-11 | 2013-06-05 | 佛山市邦普循环科技有限公司 | Method for preparing nickel-cobalt-manganese hydroxide |
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Application publication date: 20141126 |