CN105070904A - Cathode active material, preparation method and battery - Google Patents
Cathode active material, preparation method and battery Download PDFInfo
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- CN105070904A CN105070904A CN201510449821.8A CN201510449821A CN105070904A CN 105070904 A CN105070904 A CN 105070904A CN 201510449821 A CN201510449821 A CN 201510449821A CN 105070904 A CN105070904 A CN 105070904A
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- electrode active
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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
- 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
- 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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- 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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- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a cathode active material. The method comprises the following steps: dissolving a lithium salt and an inorganic manganese salt into an alcohol solvent according to the ratio of lithium atoms to manganese atoms being 1 to 2, so as to obtain a first solution; dissolving resorcinol and hexamethylenetetramine into the solvent at the molar ratio of 4 to (0.5-2) to obtain a second solution; mixing the first solution with the second solution at the molar ratio of lithium manganate to the resorcinol being (0.5-2) to 1; sealing the mixed solution, carrying out solvent thermal treatment at 100-180 DEG C, and taking out and drying the mixture, so as to obtain microspheric lithium manganate precursor power; and calcining the lithium manganate precursor power in an air atmosphere at 600-800 DEG C. The invention further provides a cathode active material obtained by the method, and a battery using the cathode active material.
Description
Technical field
The present invention relates to a kind of positive electrode active materials, preparation method and the battery containing this positive electrode active materials, particularly a kind of positive electrode active materials for lithium ion battery and preparation method.
Background technology
Lithium manganate having spinel structure (LiMn
2o
4) operating voltage is 3.8V (vs.Li), theoretical capacity 148mAh/g, because of its there is aboundresources, with low cost, fail safe good, non-environmental-pollution and prepare the ideal material that the advantage such as easy is considered to power lithium-ion battery.LiMn2O4 actual capacity is generally 100-120mAh/g, and lower specific capacity and larger capacity attenuation constrain its application and development in power lithium-ion battery field.
By LiMn
2o
4particle nanometer can significantly improve its specific capacity and high rate performance, but due to solid liquid interface increase, makes Mn
3+easier stripping, causes the rapid decay of capacity.In addition, the nanometer of material also can cause tap density to reduce, and then directly reduces its volume and capacity ratio.In order to the reduction of the decay and volume and capacity ratio that suppress capacity, researcher has prepared spherical lithium manganate particle, effectively improves volume and capacity ratio.But micron-sized spheric granules has longer ion transfer distance, and electrolyte is not easy to penetrate into ball centre, causes high rate performance to reduce.Therefore, the hollow be made up of nanometer or submicron order crystal grain is prepared or porous microsphere causes people's interest widely.Due to hole abundant between primary particle, electrolyte is easy to infiltration wherein, thus can improve the high rate performance of electrode.But, the method of current synthetic lithium manganate porous microsphere mainly first controls the solid or hollow precursor microsphere of carbonate synthesis manganese, calcined and become manganese oxide, or directly synthesize manganese dioxide porous microsphere, again it mixed with lithium salts, calcine and obtain LiMn2O4, technics comparing is complicated, and governing factor is more.For this reason, the simple method for preparing developing a kind of LiMn2O4 porous microsphere is necessary.In addition, in prior art, synthetic lithium manganate hollow ball also there is not been reported.
Summary of the invention
The invention provides a kind of positive electrode active materials, its preparation method and the battery containing this positive electrode active materials, can solve the problem.
A preparation method for positive electrode active materials, comprises the following steps:
Be that 1:2 is dissolved in alcohols solvent by lithium salts and inorganic manganese salt according to lithium atom and manganese atom ratio, obtain the first solution;
Resorcinol and hexamethylenetetramine are dissolved in solvent in 4:0.5 ~ 2 in molar ratio, obtain the second solution;
Be that the first solution mixes with the second solution by 0.5 ~ 2:1 by the mol ratio of LiMn2O4 and resorcinol;
After mixed liquor is sealed, 100-180 DEG C of solvent heat treatment, take out post-drying, obtain microspheroidal LiMn2O4 precursor powder;
By LiMn2O4 precursor powder in air atmosphere in 600 ~ 800 DEG C of calcinings.
Further, described alcohols solvent is methyl alcohol, ethanol, isopropyl alcohol, normal propyl alcohol, ethylene glycol or its mixing.
Further, further, at 100-180 DEG C of solvent heat treatment 4-10h, 60-80 DEG C of oven dry after taking-up.
Further, by LiMn2O4 precursor powder in air atmosphere, heating rate is that 1 ~ 2 DEG C/min is heated to 600 ~ 800 DEG C and temperature retention time 2 ~ 12h.
Further, described inorganic manganese salt is manganese acetate or manganese chloride, and described lithium salts is lithium acetate, lithium nitrate or lithium chloride, and the purity of described inorganic manganese salt and lithium salts is at more than 98wt.%.
Further, described resorcinol and more than hexamethylenetetramine purity 99wt.%.
The present invention also provides a kind of positive electrode active materials obtained by above-mentioned preparation method, and wherein, described positive electrode active materials is hollow LiMn2O4 microballoon.
Further, the diameter of described hollow LiMn2O4 microballoon is at 0.5 ~ 2 μm, and the thickness of ball wall is 50nm ~ 150nm.
The present invention also provides a kind of battery comprising above-mentioned positive electrode active materials further, comprising: positive pole; Negative pole; And electrolyte; Wherein, described positive pole comprises above-mentioned positive electrode active materials.
The preparation method of positive electrode active materials provided by the invention, by the process of resorcinol and the balling-up of hexamethylenetetramine solvent thermal polymerization, by manganese salt and the direct load of lithium salts on organic micro-spheres, then make burning till of LiMn2O4 synchronously complete in calcining with the removal of organic micro-spheres template, thus provide a kind of simple method for preparing of LiMn2O4 porous hollow sphere.This technique is simple, and cost is low, is extremely conducive to large-scale production.In addition, the diameter of positive electrode active materials provided by the invention is at about 0.5-2 μm, and hollow ball wall is made up of the LiMn2O4 nano particle of about 50nm ~ 150nm, and purity is high, good crystallinity, shows excellent specific capacity and high rate performance as anode material for lithium-ion batteries.
Accompanying drawing explanation
Preparation method's flow chart of the positive electrode active materials that Fig. 1 provides for the embodiment of the present invention.
The stereoscan photograph of the positive electrode active materials that Fig. 2 provides for the embodiment of the present invention 1.
The X ray diffracting spectrum of the positive electrode active materials that Fig. 3 provides for the embodiment of the present invention 1.
When the positive electrode active materials that Fig. 4 provides for the embodiment of the present invention 1 is as Snap-type cell positive, the cyclic curve under different multiplying.
Fig. 5 for the positive electrode active materials that provides for the embodiment of the present invention 1 as Snap-type cell positive time, the charging and discharging curve under different multiplying.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.Be understandable that, specific embodiment described herein is only for explaining the present invention, but not limitation of the invention.It also should be noted that, for convenience of description, illustrate only part related to the present invention in accompanying drawing but not entire infrastructure.
Please refer to Fig. 1, a kind of preparation method of positive electrode active materials, comprises the following steps:
S1: be that 1:2 is dissolved in alcohols solvent according to lithium atom and manganese atom ratio by lithium salts and inorganic manganese salt, obtains the first solution;
S2: resorcinol and hexamethylenetetramine are dissolved in solvent in 4:0.5 ~ 2 in molar ratio, obtain the second solution;
S3: be that the first solution mixes with the second solution by 0.5 ~ 2:1 by the mol ratio of LiMn2O4 and resorcinol;
S4: after mixed liquor is sealed, 100-180 DEG C of solvent heat treatment, take out post-drying, obtain microspheroidal LiMn2O4 precursor powder;
S5: by LiMn2O4 precursor powder in air atmosphere in 600 ~ 800 DEG C of calcinings.
In step sl, described inorganic manganese salt is manganese acetate or manganese chloride, and its purity is at more than 98wt.%.Described lithium salts is lithium acetate, lithium nitrate or lithium chloride, and its purity is at more than 98wt.%.Described alcohols solvent can be methyl alcohol, ethanol, isopropyl alcohol, normal propyl alcohol, ethylene glycol or its mixing.Preferably, be that 1:2 is dissolved in ethanol by lithium salts and inorganic manganese salt according to lithium atom and manganese atom ratio.
In step s 2, resorcinol and hexamethylenetetramine can be dissolved in deionized water or other can dissolve in the solvent of described applicable resorcinol and hexamethylenetetramine in 4:0.5 ~ 2 in molar ratio.Described resorcinol and hexamethylenetetramine purity are all at more than 99wt.%.
In step s 4 which, by solvent thermal reaction, described resorcinol and hexamethylenetetramine can be polymerized balling-up, and described manganese salt and lithium salts depend on spheroid simultaneously.Wherein, the time of described solvent heat treatment is 4-10h, and the temperature of taking out oven dry is 60-80 DEG C.Preferred, the temperature of described solvent heat treatment is 150-180 DEG C., thus described resorcinol and hexamethylenetetramine can fully be reacted.
In step s 5, burning till of LiMn2O4 synchronously can complete with the removal of organic micro-spheres template in calcination process.Concrete, can by LiMn2O4 precursor powder in air atmosphere, be that 1 ~ 2 DEG C/min is heated to 600 ~ 800 DEG C with heating rate, and temperature retention time 2 ~ 12h.Preferably, can in 600 ~ 800 DEG C of temperature ranges calcine by steps, preferred, in three temperature ranges such as 600 ~ 700 DEG C, 700 ~ 750 DEG C and 750 ~ 800 DEG C, calcine 2 ~ 12h respectively, thus more good crystallinity can be obtained.
The present invention also provides a kind of positive electrode active materials obtained by above-mentioned preparation method, and wherein, described positive electrode active materials is hollow LiMn2O4 microballoon.The diameter of described hollow LiMn2O4 microballoon is at 0.5 ~ 2 μm, and the thickness of ball wall is 50nm ~ 150nm.Preferably, the diameter of described hollow LiMn2O4 microballoon is at 0.5 ~ 1 μm, and the thickness of ball wall is 100nm ~ 150nm.
The present invention also provides a kind of battery comprising above-mentioned positive electrode active materials further, comprising: positive pole; Negative pole; And electrolyte; Wherein, described positive pole comprises above-mentioned positive electrode active materials.
Embodiment 1:
Under stirring, be 1:2 by lithium atom and manganese atom number ratio, appropriate two acetate hydrate lithiums and manganese acetate be dissolved in 40ml ethanol, obtain the first solution; By resorcinol and hexamethylenetetramine in molar ratio 4:2 be dissolved in 20ml deionized water, obtain the second solution; By the mol ratio 0.5:1 of LiMn2O4 and resorcinol, the first solution is mixed with the second solution, then being transferred to volume is in the stainless steel cauldron of 100ml, after sealing, at 180 DEG C of solvent heat treatment 10h, take out directly 80 DEG C of oven dry, namely obtain microspheroidal LiMn2O4 precursor powder; LiMn2O4 precursor powder is calcined 5h at 650,750 and 800 DEG C respectively with Muffle furnace in atmosphere, obtains lithium cell anode material lithium manganate hollow ball.
Please refer to Fig. 2, as seen from Figure 2, the lithium manganate hollow ball diameter obtained is at about 1 μm, and hollow ball wall is made up of the LiMn2O4 nano particle of about 100nm.Please refer to Fig. 3, as seen from Figure 3, its crystal phase and spinel lithium manganate (JCPDF card number: 35-0782, space group Fd3m) fit like a glove, and what prove synthesis is spinel lithium manganese oxide anode material.Please refer to Fig. 4-5, can see from Fig. 4-5, specific discharge capacity is at 10C(1C=120mA/g) time still can reach more than 100mAh/g, prove that it has excellent specific capacity and high rate performance.
Embodiment 2:
Substantially the same manner as Example 1, difference is, replaces manganese acetate as manganese source using manganese chloride.
Embodiment 3
Substantially the same manner as Example 1, difference is, replaces lithium acetate as lithium source using lithium nitrate.
Embodiment 4
Substantially the same manner as Example 1, difference is, replaces lithium acetate as lithium source using lithium chloride.
Embodiment 5
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using methyl alcohol.
Embodiment 6
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using isopropyl alcohol.
Embodiment 7
Substantially the same manner as Example 1, difference is, replaces ethanol as solvent using normal propyl alcohol.
Experiment proves, it is high that embodiment 2-7 all can obtain purity, good crystallinity, excellent specific capacity and high rate performance positive electrode active materials.
Note, above are only preferred embodiment of the present invention and institute's application technology principle.Skilled person in the art will appreciate that and the invention is not restricted to specific embodiment described here, various obvious change can be carried out for a person skilled in the art, readjust and substitute and can not protection scope of the present invention be departed from.Therefore, although be described in further detail invention has been by above embodiment, the present invention is not limited only to above embodiment, when not departing from the present invention's design, can also comprise other Equivalent embodiments more, and scope of the present invention is determined by appended right.
Claims (10)
1. a preparation method for positive electrode active materials, is characterized in that, comprises the following steps:
Be that 1:2 is dissolved in alcohols solvent by lithium salts and inorganic manganese salt according to lithium atom and manganese atom ratio, obtain the first solution;
Resorcinol and hexamethylenetetramine are dissolved in solvent in 4:0.5 ~ 2 in molar ratio, obtain the second solution;
Be that the first solution mixes with the second solution by 0.5 ~ 2:1 by the mol ratio of LiMn2O4 and resorcinol;
After mixed liquor is sealed, 100-180 DEG C of solvent heat treatment, take out post-drying, obtain microspheroidal LiMn2O4 precursor powder;
By LiMn2O4 precursor powder in air atmosphere in 600 ~ 800 DEG C of calcinings.
2. the preparation method of positive electrode active materials according to claim 1, is characterized in that, described alcohols solvent is methyl alcohol, ethanol, isopropyl alcohol, normal propyl alcohol, ethylene glycol or its mixing.
3. the preparation method of positive electrode active materials according to claim 1, is characterized in that, described in, the step of taking out post-drying comprises: 60-80 DEG C of oven dry.
4. the preparation method of positive electrode active materials according to claim 1, is characterized in that, the described step 100-180 DEG C of solvent heat treatment comprises:
At 100-180 DEG C of solvent heat treatment 4-10h.
5. the preparation method of positive electrode active materials according to claim 1, is characterized in that, described by LiMn2O4 precursor powder in air atmosphere in 600 ~ 800 DEG C calcining step be:
By LiMn2O4 precursor powder in air atmosphere, heating rate is that 1 ~ 2 DEG C/min is heated to 600 ~ 800 DEG C and temperature retention time 2 ~ 12h.
6. the preparation method of positive electrode active materials according to claim 1, is characterized in that, described inorganic manganese salt is manganese acetate or manganese chloride, and described lithium salts is lithium acetate, lithium nitrate or lithium chloride, and the purity of described inorganic manganese salt and lithium salts is at more than 98wt.%.
7. the preparation method of positive electrode active materials according to claim 1, is characterized in that, described resorcinol and more than hexamethylenetetramine purity 99wt.%.
8., by a positive electrode active materials for preparation method's acquisition as described in the appended claim 1, it is characterized in that, described positive electrode active materials is hollow LiMn2O4 microballoon.
9. a positive electrode active materials according to claim 8, is characterized in that, the diameter of described hollow LiMn2O4 microballoon is at 0.5 ~ 2 μm, and the thickness of ball wall is 50nm ~ 150nm.
10. a battery, comprising:
Positive pole;
Negative pole; And
Electrolyte,
It is characterized in that, described positive pole comprises the positive electrode active materials as described in any one of claim 8-9.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428847A (en) * | 2008-12-15 | 2009-05-13 | 吉林大学 | Process for producing nanostructured tin dioxide lithium ion battery negative pole material |
| CN101898799A (en) * | 2010-07-28 | 2010-12-01 | 复旦大学 | Method for preparing lithium manganate hollow ball material |
| CN102655231A (en) * | 2012-05-08 | 2012-09-05 | 广州市香港科大霍英东研究院 | Novel preparation method of anode material LiMn2O4 of high-power-performance lithium ion battery |
| CN104600286A (en) * | 2015-01-29 | 2015-05-06 | 扬州大学 | Preparation method of positive active material hollow spherical lithium manganate of lithium ion battery |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428847A (en) * | 2008-12-15 | 2009-05-13 | 吉林大学 | Process for producing nanostructured tin dioxide lithium ion battery negative pole material |
| CN101898799A (en) * | 2010-07-28 | 2010-12-01 | 复旦大学 | Method for preparing lithium manganate hollow ball material |
| CN102655231A (en) * | 2012-05-08 | 2012-09-05 | 广州市香港科大霍英东研究院 | Novel preparation method of anode material LiMn2O4 of high-power-performance lithium ion battery |
| CN104600286A (en) * | 2015-01-29 | 2015-05-06 | 扬州大学 | Preparation method of positive active material hollow spherical lithium manganate of lithium ion battery |
Non-Patent Citations (2)
| Title |
|---|
| QIANG SUN,ET AL: ""Controlled hydrothermal synthesis of 1D nanocarbons by surfactant templated assembly for use as anodes for rechargeable lithium-ion batteries"", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| YINGCHAO CHEN,ET AL: ""Nano-sized LiMn2O4 spinel cathode materials exhibiting high rate discharge capability for lithium-ion batteries"", 《JOURNAL OF POWER SOURCES》 * |
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