CN106784654A - A kind of preparation method of graphene coated cobalt acid lithium material - Google Patents
A kind of preparation method of graphene coated cobalt acid lithium material Download PDFInfo
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- CN106784654A CN106784654A CN201611065529.7A CN201611065529A CN106784654A CN 106784654 A CN106784654 A CN 106784654A CN 201611065529 A CN201611065529 A CN 201611065529A CN 106784654 A CN106784654 A CN 106784654A
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- 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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- 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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Abstract
The present invention is a kind of preparation method of graphene coated cobalt acid lithium material, and method and step includes, Graphene is prepared using hummers methods；By obtained graphene dispersion in ethanol, then ball milling, obtains the ethanol solution of Graphene；Add cobalt acid lithium and a small amount of water to continue ball milling in the ethanol solution of Graphene, obtain the mixed solution of cobalt acid lithium and Graphene；Then the mixed solution of filtering graphite alkene and cobalt acid lithium, take filtrate drying, obtain the composite of graphene coated cobalt acid lithium, in the present invention, in dispersing graphene in ethanol, and because ethanol has certain polarity, dissolved each other with a small amount of water, the dispersiveness of cobalt acid lithium can be improved, simultaneously, the dissociation amount of cobalt acid lithium can be reduced again, so most cobalt acid lithium is scattered in ethanol with molecular forms, it is well mixed with Graphene, form the material of graphene coated cobalt acid lithium, this method, ensure that the chemical property of cobalt acid lithium, improve the utilization rate of cobalt acid lithium.
Description
Technical field
The present invention relates to the preparation method of anode material for lithium-ion batteries, a kind of particularly graphene coated cobalt acid lithium material
The preparation method of material.
Background technology
The actual capacity of cobalt acid lithium is low compared with theoretical capacity, because during repeated charge, active material is more
Volumetric expansion after secondary discharge and recharge, causes internal resistance to increase, and capacity reduces；In addition, cobalt is dissolved in electrolyte, active material is caused to lose.
Cobalt acid lithium can be modified by doping and cladding, unwanted surface can be avoided to react, inhibitory activity material it is molten
Solution.The stabilized protection course that Surface coating is formed, will not suppress lattice dilatation and phase transformation of the cobalt acid lithium in charge and discharge process, thus
Electrode, the chemistry of electrolyte interface and structural stability are improved, so as to the charge-discharge performance and circulation that effectively improve them can
Inverse property.
The coating layer material requirement of cobalt acid lithium has certain mechanical strength, could suppress LixCoO2Lattice is followed in discharge and recharge
Expansion and contraction during ring.The mechanical tensile strength of metal oxide is not the optimal selection for coating cobalt acid lithium not enough.
Graphene has excellent mechanical performance and good electric conductivity property, can be used as the preferable covering material of cobalt acid lithium.
At present, the technique of graphene coated cobalt acid lithium mainly has two major classes：
The first kind is that advance scattered graphene oxide solution carries out ultrasound with cobalt acid lithium or stirring mixes, Ran Houjin
Row centrifugation, washing, dried process, you can prepare the cobalt acid lithium of graphene oxide cladding, then carrying out reduction can prepare
Go out the cobalt acid lithium of graphene coated.There are following some deficiencies in this preparation technology：First, graphene oxide/cobalt acid lithium is answered
After carrying out reduction, can make the ratio of oxygen in cobalt acid lithium reduces compound, reduces the chemical property of active material；Secondly, stone is aoxidized
Black alkene/cobalt acid lithium surface reduction is not comprehensive enough, and the oxygen of graphenic surface residual can reduce its electric conductivity, the speed for causing electronics to conduct
Rate is slack-off；Finally, using water as the dispersant of cobalt acid lithium, cobalt acid lithium dissolution of partial fiber surface can be made, surface produces substantial amounts of hydroxyl,
Can not be removed by follow-up simple dried process, so that the chemical property reduction of cobalt acid lithium.
Equations of The Second Kind is, with oxygen-bearing organic matter as carbon source, in an inert atmosphere, carbon is produced by being pyrolyzed oxygen-bearing organic matter, sinks
Product forms Graphene on cobalt acid lithium surface.This cladding process has the following disadvantages：First, discrete Graphene can not be complete
The surface of cobalt acid lithium is coated, still can there is the dissolving of active material；Secondly, by the method for chemical meteorology deposition directly non-
The Graphene of metal surface deposition, defect is more, influences the mechanical performance and electric conductivity of Graphene, causes its chemical property to drop
It is low；Finally, the temperature of technique thermal decomposition is high, it is impossible to reach the purpose of energy-conservation.
The content of the invention
To solve above technical problem, the invention provides a kind of preparation method of graphene coated cobalt acid lithium material, side
Step is simple in method, optimizes cobalt acid lithium surface oxygen distribution, improves the chemical property of composite.This law is using such as lower section
What case was realized：
A kind of preparation method of graphene coated cobalt acid lithium material, step includes,
Step one, Graphene is prepared using hummers methods；
Step 2, by obtained graphene dispersion in ethanol, then ball milling, obtains the ethanol solution of Graphene；
Step 3, adds cobalt acid lithium and water in the ethanol solution of Graphene, continues ball milling, obtains cobalt acid lithium and Graphene
Mixed solution；
Step 4, filtering graphite alkene and the mixed solution of cobalt acid lithium, take filtrate drying, obtain graphene coated cobalt acid lithium
Composite.
Preferably, step also includes, the composite of obtained graphene coated cobalt acid lithium in step 3 is placed in into air
The heating of atmosphere high temperature obtains graphene coated cobalt acid lithium material.
It is highly preferred that composite is placed in the heating of air atmosphere high temperature, the temperature of heating is 200~500 DEG C, during heating
Between be 1~4h.
Preferably, in step 2, in ethanol solution, the time of ball milling is 1~2h to graphene dispersion.
Preferably, in step 3, the amount of the water of addition is 0~1 with the ratio of amount of alcohol:10.
Preferably, in step 3, cobalt acid lithium and water are added in the ethanol solution of Graphene, the time of ball milling is 1~2h.
Preferably, in step 4, the drying time of filtrate is 1~2h, and drying temperature is 60~90 DEG C.
In the technical solution adopted in the present invention, wherein, in dispersing graphene in ethanol, and because ethanol has one
Fixed polarity, dissolves each other with a small amount of water, can improve the dispersiveness of cobalt acid lithium, meanwhile, the dissociation amount of cobalt acid lithium can be reduced again, this
The most cobalt acid lithium of sample is scattered in ethanol with molecular forms, is well mixed with Graphene, forms graphene coated cobalt
The material of sour lithium, this method, it is ensured that the chemical property of cobalt acid lithium, improve the utilization rate of cobalt acid lithium.
Further, the material of obtained graphene coated cobalt acid lithium heats in air atmosphere again, enables to stone
Black alkene surface has a small amount of defect, increases a small amount of hydroxyl, and a small amount of hydroxyl is combined with cobalt acid lithium by hydrogen bond and Van der Waals force
More closely, the material of uniform graphene coated cobalt acid lithium is formed.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
The preparation of Graphene：
It is that Graphene is prepared using hummers methods in the present embodiment, concretely comprises the following steps, graphite powder and sodium nitrate is added
In the concentrated sulfuric acid of ice bath, below 4 DEG C, wherein the mass ratio of sodium nitrate bath graphite powder is 1 to the temperature of the ice bath concentrated sulfuric acid:2, reaction
After a period of time, potassium permanganate is slow added into, be well mixed, the temperature in control reaction solution is below 10 DEG C；Reaction one
After the section time, then tepidarium is carried out, the temperature of tepidarium is no more than 40 DEG C；After tepidarium for a period of time, add in solution
Enter deionized water, raise bath temperature, control the temperature in reaction solution for 95 DEG C or so, carry out hot bath, period stirring is anti-
Answer solution；After reaction a period of time, deionized water stopped reaction is added, hydrogen peroxide is then slowly added to this again and hydrochloric acid is molten
Liquid.The reacted solution of low-speed centrifugal and filtration washing sediment, as graphene film.
Graphene is combined with cobalt acid lithium：
By obtained graphene dispersion in ethanol, and after the ultrasonic ball milling 1h of use, graphene film is uniformly disperseed, obtained
To Graphene ethanol solution.
Cobalt acid lithium is sequentially added in Graphene ethanol solution, after ball milling 1h, cobalt acid lithium is uniformly scattered in ethanol, and
With the ethanol solution that Graphene is compounded to form cobalt acid lithium and Graphene.
The ethanol solution of cobalt acid lithium obtained above and Graphene is filtered, is removed removing and is formed the undispersed of aggregation
Graphene and cobalt acid lithium, the filtrate that will be obtained are placed in baking oven and dry, and oven temperature is 90 DEG C, and drying time is 1h, will
Ethanol and moisture evaporation are clean, obtain the composite of graphene coated cobalt acid lithium.
The heat treatment of graphene coated cobalt acid lithium：
In the above-mentioned composite by graphene coated cobalt acid lithium, it is placed in air atmosphere and is heated, heating temperature
Degree is maintained at 500 DEG C, and then heat time 1h anneals, until being cooled to room temperature, is being made the battery of graphene coated cobalt acid lithium just
Pole material.
Embodiment 2,
The preparation of Graphene：It is same as Example 1, same Graphene is obtained using hummers methods.
Graphene is combined with cobalt acid lithium：
By obtained graphene dispersion in ethanol, be scattered in graphene film in ethanol and obtain Graphene by ball milling 2h
Ethanol solution.
Cobalt acid lithium and a small amount of water are sequentially added in Graphene ethanol solution, the amount of water is the 0.03 of amount of alcohol, ball milling 2h
Afterwards, Graphene and cobalt acid lithium form compound solution.
The ethanol solution of cobalt acid lithium obtained above and Graphene is filtered, is removed removing and is formed the undispersed of aggregation
Graphene and cobalt acid lithium, the filtrate of acquisition are placed under conditions of 60 DEG C and dry 2h, obtain dry graphene coated cobalt acid
The composite of lithium.
The heat treatment of graphene coated cobalt acid lithium：
The composite of dry graphene coated cobalt acid lithium is placed in air atmosphere and is heated, heating-up temperature is maintained at
200 DEG C, the heat time is 3h, is then annealed, cooling, and the cell positive material of graphene coated cobalt acid lithium is obtained.
Embodiment 3
In the present embodiment, the preparation of Graphene uses identical preparation process with embodiment 1.
Graphene is combined with cobalt acid lithium：
By obtained graphene dispersion in ethanol, 2h is mixed in high-speed mixer, graphene film is scattered in ethanol
In obtain the ethanol solution of Graphene.
Cobalt acid lithium and a small amount of water are sequentially added in Graphene ethanol solution, the amount of water is 0.08 times of amount of alcohol, ball milling
After 1.5h, Graphene and cobalt acid lithium form compound solution.
The ethanol solution of cobalt acid lithium obtained above and Graphene is filtered, is removed removing and is formed the undispersed of aggregation
Graphene and cobalt acid lithium, the filtrate of acquisition are placed under conditions of 80 DEG C and dry 1.5h, obtain dry graphene coated cobalt
The composite of sour lithium.
The heat treatment of graphene coated cobalt acid lithium：
The composite of dry graphene coated cobalt acid lithium is placed in air atmosphere and is heated, heating-up temperature is maintained at
300 DEG C, the heat time is 1.5h, is then annealed, cooling, and the cell positive material of graphene coated cobalt acid lithium is obtained.
The cell positive material of graphene coated cobalt acid lithium obtained in embodiment 1,2,3 is made battery, battery is measured
Performance is superior to existing cobalt acid lithium battery, and cycle performance is significantly improved, and in circulation more than 1500 times, capacitance does not see below battery
Drop.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
Should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with scope of the claims
It is defined.
Claims (7)
1. a kind of preparation method of graphene coated cobalt acid lithium material, it is characterised in that：Method and step includes,
Step one, Graphene is prepared using hummers methods；
Step 2, by obtained graphene dispersion in ethanol, then ball milling, obtains the ethanol solution of Graphene；
Step 3, adds cobalt acid lithium and a small amount of water in the ethanol solution of Graphene, continues ball milling, obtains cobalt acid lithium and Graphene
Mixed solution；
Step 4, filtering graphite alkene and the mixed solution of cobalt acid lithium, take filtrate drying, obtain the compound of graphene coated cobalt acid lithium
Material.
2. the preparation method of graphene coated cobalt acid lithium material according to claim 1, it is characterised in that：Step is also wrapped
Include, the composite of obtained graphene coated cobalt acid lithium in step 4 is placed in into the heating of air atmosphere high temperature obtains Graphene
Cladding cobalt acid lithium material.
3. the preparation method of graphene coated cobalt acid lithium material according to claim 2, it is characterised in that：Composite is put
In the heating of air atmosphere high temperature, the temperature of heating is 200~500 DEG C, and the heat time is 1~4h.
4. the preparation method of graphene coated cobalt acid lithium material according to claim 1 and 2, it is characterised in that：Step 2
In, in ethanol solution, the time of ball milling is 1~2h to graphene dispersion.
5. the preparation method of graphene coated cobalt acid lithium material according to claim 1 and 2, it is characterised in that step 3
In, the amount of the water of addition is 0~1 with the ratio of amount of alcohol:10.
6. the preparation method of graphene coated cobalt acid lithium material according to claim 5, it is characterised in that：In step 3,
Cobalt acid lithium and water are added in the ethanol solution of Graphene, the time of ball milling is 1~2h.
7. the preparation method of graphene coated cobalt acid lithium material according to claim 5, it is characterised in that：In step 3,
The drying time of filtrate is 1~2h, and drying temperature is 60~90 DEG C.
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| CN107579247A (en) * | 2017-09-17 | 2018-01-12 | 长沙仲善新能源科技有限公司 | Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof |
| CN107634189A (en) * | 2017-08-08 | 2018-01-26 | 华东理工大学 | A kind of modified nickel cobalt aluminium tertiary cathode material and its preparation method and application |
| CN107742705A (en) * | 2017-10-03 | 2018-02-27 | 长沙仲善新能源科技有限公司 | Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof |
| CN107910532A (en) * | 2017-11-20 | 2018-04-13 | 复旦大学 | A kind of preparation method of graphene coated nickle cobalt lithium manganate composite 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 |
| CN109728269A (en) * | 2018-12-18 | 2019-05-07 | 南京理工大学 | The preparation method of graphene coated cobalt lithium aluminate electrode material |
| CN110828780A (en) * | 2019-11-01 | 2020-02-21 | 长沙矿冶研究院有限责任公司 | graphene/TiO2Preparation method of composite positive electrode |
| CN112103477A (en) * | 2019-06-17 | 2020-12-18 | 中兴通讯股份有限公司 | Single-layer reduced graphene oxide lithium cobaltate composite material and preparation method and application thereof |
| CN112103478A (en) * | 2019-06-17 | 2020-12-18 | 中兴通讯股份有限公司 | Porous graphene lithium cobaltate composite material and preparation method and application thereof |
| CN112635732A (en) * | 2020-12-17 | 2021-04-09 | 中国电子科技集团公司第十八研究所 | Preparation method of graphene/lithium cobaltate composite positive electrode material |
| CN113716623A (en) * | 2021-08-27 | 2021-11-30 | 中国地质大学（武汉） | High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of |
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| CN107634189A (en) * | 2017-08-08 | 2018-01-26 | 华东理工大学 | A kind of modified nickel cobalt aluminium tertiary cathode material and its preparation method and application |
| CN107579247A (en) * | 2017-09-17 | 2018-01-12 | 长沙仲善新能源科技有限公司 | Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof |
| CN107742705A (en) * | 2017-10-03 | 2018-02-27 | 长沙仲善新能源科技有限公司 | Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof |
| CN107910532A (en) * | 2017-11-20 | 2018-04-13 | 复旦大学 | A kind of preparation method of graphene coated nickle cobalt lithium manganate composite material |
| CN107910532B (en) * | 2017-11-20 | 2020-09-01 | 复旦大学 | Preparation method of graphene-coated nickel cobalt lithium manganate composite 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 |
| CN109728269A (en) * | 2018-12-18 | 2019-05-07 | 南京理工大学 | The preparation method of graphene coated cobalt lithium aluminate electrode material |
| CN109728269B (en) * | 2018-12-18 | 2022-02-15 | 南京理工大学 | Preparation method of graphene-coated cobalt lithium aluminate electrode material |
| CN112103478A (en) * | 2019-06-17 | 2020-12-18 | 中兴通讯股份有限公司 | Porous graphene lithium cobaltate composite material and preparation method and application thereof |
| CN112103477A (en) * | 2019-06-17 | 2020-12-18 | 中兴通讯股份有限公司 | Single-layer reduced graphene oxide lithium cobaltate composite material and preparation method and application thereof |
| CN110828780A (en) * | 2019-11-01 | 2020-02-21 | 长沙矿冶研究院有限责任公司 | graphene/TiO2Preparation method of composite positive electrode |
| CN112635732A (en) * | 2020-12-17 | 2021-04-09 | 中国电子科技集团公司第十八研究所 | Preparation method of graphene/lithium cobaltate composite positive electrode material |
| CN113716623A (en) * | 2021-08-27 | 2021-11-30 | 中国地质大学（武汉） | High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of |
| CN113716623B (en) * | 2021-08-27 | 2022-07-19 | 中国地质大学（武汉） | High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of |
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Application publication date: 20170531 |