CN105826552A - Method for producing graphene-composited lithium cobalt oxide positive electrode material - Google Patents
Method for producing graphene-composited lithium cobalt oxide positive electrode material Download PDFInfo
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- CN105826552A CN105826552A CN201510008112.6A CN201510008112A CN105826552A CN 105826552 A CN105826552 A CN 105826552A CN 201510008112 A CN201510008112 A CN 201510008112A CN 105826552 A CN105826552 A CN 105826552A
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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
The invention discloses a method for producing a graphene-composited lithium cobalt oxide positive electrode material. The method comprises the following steps: 1) placing lithium cobalt oxide powder in an atmosphere heating furnace, introducing protection atmosphere, heating the materials, introducing carbon source gas, decomposing the carbon source gas to carbon atoms under catalysis of lithium cobalt oxide, dissolving the decomposed carbon atoms in lithium cobalt oxide to form a carbon atoms-lithium cobalt oxide solid solution; and 2) cooling the materials in protection atmosphere, dialysing the carbon atoms dissolved with the lithium cobalt oxide to the surface of the lithium cobalt oxide to form graphene-coated lithium cobalt oxide to obtain the graphene-composited lithium cobalt oxide positive electrode material. The prepared graphene-composited lithium cobalt oxide positive electrode material has excellent electronic conductivity, high-rate charge-discharge capability and cycle performance.
Description
Technical field
The present invention relates to the technical field that anode material for lithium-ion batteries manufactures, be related specifically to the preparation method of the compound lithium cobaltate cathode material of a kind of Graphene.
Background technology
Along with the fast development of portable electric appts, energy market to reproducible, energy is high, the accumulator demand of life-span length is increasing, and the battery that lithium ion battery is the highest as wherein voltage, energy density is maximum, has good development prospect.
In lithium ion battery, positive electrode is its of paramount importance ingredient, is also the key determining performance of lithium ion battery.Cobalt acid lithium, phosphoric acid vanadium lithium and LiFePO4 are applied the most on a large scale as positive electrode.Wherein cobalt acid lithium (LiCoO2) there is the energy density of 3.7V average output voltage, up to 140mAh/g, and there is the advantage such as cycle performance and good thermal stability.These advantages make cobalt acid lithium be considered as most potential high-tension battery positive electrode, the extremely concern of industry.
But along with the fast development of smart mobile phone, the requirement to battery of mobile phone performance is more and more higher, tradition LiCoO2The energy density of positive electrode the most gradually can not meet demand, so improving LiCoO further2The energy density of positive electrode is the urgent needs of cobalt acid lithium development.Along with people are to lithium ion LiCoO2The understanding of positive electrode, it is found that its surface texture has the biggest impact to its chemical property, due to electric conductivity, electrochemical stability, physical attribute and cheap cost that material with carbon element is excellent, carbon cladding becomes one of most widely used method in lithium ion battery.Carbon cladding combines with nanotechnology, it is possible to provide preferably electric conductivity, faster lithium ion diffusion velocity, thus obtains more preferable high rate performance.
In recent years, Graphene is also used for cladding or cation doping acid lithium as good conductive material, improve the electron conduction of cobalt acid lithium, but the composite of these cobalt acid lithiums and Graphene with and preparation method thereof there is also cobalt acid lithium and graphene dispersion is not enough, contact the problems such as the closest.Therefore, the composite of cobalt acid lithium and Graphene also needs to improve further so that form the most fully dispersed and close contact between the two, ensures that Graphene reduction ratio is relatively abundant simultaneously, and electron conduction is more preferable.
Summary of the invention
It is an object of the invention to provide the preparation method of the compound lithium cobaltate cathode material of a kind of Graphene, prepared positive electrode has excellent electron conduction, high-rate charge-discharge capability and cycle performance.
To this end, the present invention is by the following technical solutions:
The preparation method of the lithium cobaltate cathode material that a kind of Graphene is compound, comprises the steps:
1) in atmosphere heating furnace, load cobalt acid lithium powder, and be passed through protective atmosphere, heating, then it is passed through carbon-source gas, carbon-source gas is decomposed into carbon atom under cobalt acid lithium is catalyzed, and decomposes the carbon atom obtained and dissolves in cobalt acid lithium, forms carbon atom-cobalt acid lithium solid solution；
2) lower the temperature in protective atmosphere, dissolve in the carbon atom dialysis of cobalt acid lithium to cobalt acid lithium surface, form graphene film and be coated with cobalt acid lithium, obtain the lithium cobaltate cathode material that Graphene is compound.
Preferably, described protective atmosphere is argon or nitrogen.
Preferably, the temperature of described heating is 600 DEG C-1000 DEG C, and heat time heating time is 1h-12h.
Preferably, described carbon-source gas is hydrocarbon gas, containing 1-7 carbon atom in each gas molecule of wherein said hydrocarbon gas.
Preferably, the described speed lowered the temperature in protective atmosphere is 3 DEG C/min-300 DEG C/min.
Preferably, described method also includes that the amount being passed through carbon-source gas by control controls Graphene mass fraction in the lithium cobaltate cathode material that prepared Graphene is compound.
The lithium cobaltate cathode material that the Graphene prepared according to arbitrary above-mentioned method is combined, the lithium cobaltate cathode material that described Graphene is combined has nucleocapsid structure, kernel is cobalt acid lithium, shell is graphene film, described graphene film is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium nearly, and wherein the mass percent of Graphene is 1%-5%.
The present invention uses above technical scheme, the cobalt acid lithium material that the Graphene formed is compound, there is nucleocapsid structure, kernel is cobalt acid lithium, shell is graphene film, and graphene film is coated with cobalt acid lithium uniformly, and graphene film is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium nearly, as the positive electrode of lithium battery, there is excellent electron conduction, high-rate charge-discharge capability and cycle performance.
Accompanying drawing explanation
Fig. 1 is the preparation method schematic diagram of the lithium cobaltate cathode material that Graphene of the present invention is combined.
Fig. 2 is the electron-microscope scanning figure of the lithium cobaltate cathode material that Graphene of the present invention is combined.
Fig. 3 is the structural representation of the lithium cobaltate cathode material that Graphene of the present invention is combined.
Detailed description of the invention
In order to make objects, features and advantages of the present invention the most clear, below in conjunction with drawings and Examples, the detailed description of the invention of the present invention is made more detailed description, in the following description, elaborate a lot of concrete details so that sufficiently understanding the present invention, but the present invention can implement to be much different from other modes of description.Therefore, the present invention not by following discloses be embodied as limited.
The preparation method of the lithium cobaltate cathode material that a kind of Graphene is compound, as it is shown in figure 1, mainly comprise the steps:
S1, loads cobalt acid lithium powder in atmosphere heating furnace, and is passed through protective atmosphere, heating, then is passed through carbon-source gas, and carbon-source gas is decomposed into carbon atom under cobalt acid lithium is catalyzed, and decomposes the carbon atom obtained and dissolves in cobalt acid lithium, forms carbon atom-cobalt acid lithium solid solution；Wherein, described protective atmosphere is argon or nitrogen；The temperature of described heating is 600 DEG C-1000 DEG C, and heat time heating time is 1h-12h；Described carbon-source gas is hydrocarbon gas, containing 1-7 carbon atom in each gas molecule of wherein said hydrocarbon gas.
S2, lowers the temperature in protective atmosphere, dissolves in the carbon atom dialysis of cobalt acid lithium to cobalt acid lithium surface, forms graphene film and is coated with cobalt acid lithium, obtains the lithium cobaltate cathode material that Graphene is compound；Wherein, the described speed lowered the temperature in protective atmosphere is 3 DEG C/min-300 DEG C/min.
Wherein, described method also includes that the amount being passed through carbon-source gas by control controls Graphene mass fraction in the lithium cobaltate cathode material that prepared Graphene is compound.
The lithium cobaltate cathode material that the Graphene prepared according to said method is combined, as shown in Figure 2 and Figure 3, there is nucleocapsid structure, kernel is cobalt acid lithium 1, shell is graphene film 2, described graphene film 2 is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium 1 nearly, and wherein the mass percent of Graphene is 1%-5%.
Embodiment one:
The lithium cobaltate cathode material that the Graphene prepared according to said method is combined, as shown in Figure 2 and Figure 3, there is nucleocapsid structure, kernel is cobalt acid lithium 1, shell is graphene film 2, described graphene film 2 is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium 1 nearly, and wherein the mass percent of Graphene is 1%.
Embodiment two
The lithium cobaltate cathode material that the Graphene prepared according to said method is combined, as shown in Figure 2 and Figure 3, there is nucleocapsid structure, kernel is cobalt acid lithium 1, shell is graphene film 2, described graphene film 2 is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium 1 nearly, and wherein the mass percent of Graphene is 3%.
Embodiment three
The lithium cobaltate cathode material that the Graphene prepared according to said method is combined, as shown in Figure 2 and Figure 3, there is nucleocapsid structure, kernel is cobalt acid lithium 1, shell is graphene film 2, described graphene film 2 is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium 1 nearly, and wherein the mass percent of Graphene is 5%.
Electrochemical property test:
Lithium cobaltate cathode material powder compound for the Graphene obtained in above-described embodiment carrying out conducting performance test, and compares with the conductivity of cobalt acid lithium powder, result is as follows:
As can be seen here, the lithium cobaltate cathode material that the Graphene that method of the present invention prepares is combined has excellent electron conduction.
Again using lithium cobaltate cathode material compound for the Graphene in above-described embodiment as positive active material, it is sufficiently mixed in nmp solvent according to active substance, acetylene black, PVDF, it is coated on aluminium foil, at 100 DEG C, it is vacuum dried 10h, after being cooled to room temperature, is washed into the positive plate of a diameter of 10mm.With lithium paper tinsel as negative pole, with Celgard2400 as barrier film, electrolyte uses 1.0molL-1LiPF6EC/DMC/DEC solution.In water, Control for Oxygen Content within 10ppm, it is full of in the glove box of Ar gas and is assembled into 2025 type button cells.The new 2025 type button cells assembled are carried out performance test, and result is as follows:
It follows that the lithium cobaltate cathode material that the Graphene that method of the present invention prepares is combined has excellent electron conduction, high-rate charge-discharge capability and cycle performance.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (7)
1. the preparation method of the lithium cobaltate cathode material that a Graphene is compound, it is characterised in that: comprise the steps:
1) in atmosphere heating furnace, load cobalt acid lithium powder, and be passed through protective atmosphere, heating, then it is passed through carbon-source gas, carbon-source gas is decomposed into carbon atom under cobalt acid lithium is catalyzed, and decomposes the carbon atom obtained and dissolves in cobalt acid lithium, forms carbon atom-cobalt acid lithium solid solution；
2) lower the temperature in protective atmosphere, dissolve in the carbon atom dialysis of cobalt acid lithium to cobalt acid lithium surface, form graphene film and be coated with cobalt acid lithium, obtain the lithium cobaltate cathode material that Graphene is compound.
The preparation method of the lithium cobaltate cathode material that a kind of Graphene the most according to claim 1 is compound, it is characterised in that: described protective atmosphere is argon or nitrogen.
The preparation method of the lithium cobaltate cathode material that a kind of Graphene the most according to claim 1 is compound, it is characterised in that: the temperature of described heating is 600 DEG C-1000 DEG C, and heat time heating time is 1h-12h.
The preparation method of the lithium cobaltate cathode material that a kind of Graphene the most according to claim 1 is compound, it is characterised in that: described carbon-source gas is hydrocarbon gas, containing 1-7 carbon atom in each gas molecule of wherein said hydrocarbon gas.
The preparation method of the lithium cobaltate cathode material that a kind of Graphene the most according to claim 1 is compound, it is characterised in that: the described speed lowered the temperature in protective atmosphere is 3 DEG C/min-300 DEG C/min.
The preparation method of the lithium cobaltate cathode material that a kind of Graphene the most according to claim 1 is compound, it is characterised in that: described method also includes that the amount being passed through carbon-source gas by control controls Graphene mass fraction in the lithium cobaltate cathode material that prepared Graphene is compound.
7. the lithium cobaltate cathode material that the Graphene prepared according to the arbitrary described method of claim 1-6 is combined, it is characterized in that: the lithium cobaltate cathode material that described Graphene is combined has nucleocapsid structure, kernel is cobalt acid lithium, shell is graphene film, described graphene film is evenly distributed on cobalt acid lithium surface and is coated with cobalt acid lithium nearly, and wherein the mass percent of Graphene is 1%-5%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106206064A (en) * | 2016-08-24 | 2016-12-07 | 张伟 | Ultracapacitor High-performance graphene electrode material and preparation method thereof |
| CN106450277A (en) * | 2016-11-01 | 2017-02-22 | 江苏海四达电源股份有限公司 | Electrode system used in low-temperature rate type lithium ion battery |
| CN106784654A (en) * | 2016-11-28 | 2017-05-31 | 荆门市格林美新材料有限公司 | A kind of preparation method of graphene coated cobalt acid lithium material |
| CN107959014A (en) * | 2017-11-21 | 2018-04-24 | 中山市电赢科技有限公司 | A kind of production method of extra-high voltage multiplying power lithium battery anode system |
-
2015
- 2015-01-07 CN CN201510008112.6A patent/CN105826552A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106206064A (en) * | 2016-08-24 | 2016-12-07 | 张伟 | Ultracapacitor High-performance graphene electrode material and preparation method thereof |
| CN106206064B (en) * | 2016-08-24 | 2019-02-12 | 苏州欢颜电气有限公司 | Supercapacitor High-performance graphene electrode material and preparation method thereof |
| CN106450277A (en) * | 2016-11-01 | 2017-02-22 | 江苏海四达电源股份有限公司 | Electrode system used in low-temperature rate type lithium ion battery |
| CN106784654A (en) * | 2016-11-28 | 2017-05-31 | 荆门市格林美新材料有限公司 | A kind of preparation method of graphene coated cobalt acid lithium material |
| CN107959014A (en) * | 2017-11-21 | 2018-04-24 | 中山市电赢科技有限公司 | A kind of production method of extra-high voltage multiplying power lithium battery anode system |
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Application publication date: 20160803 |