CN107591538A - A kind of preparation method of graphene-based anode material for lithium-ion batteries - Google Patents
A kind of preparation method of graphene-based anode material for lithium-ion batteries Download PDFInfo
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- CN107591538A CN107591538A CN201710870093.7A CN201710870093A CN107591538A CN 107591538 A CN107591538 A CN 107591538A CN 201710870093 A CN201710870093 A CN 201710870093A CN 107591538 A CN107591538 A CN 107591538A
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- graphene
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- anode material
- ion batteries
- positive electrode
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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 present invention proposes a kind of preparation method of graphene-based anode material for lithium-ion batteries, and its step is as follows：Graphite oxide is made by chemical oxidization method, graphite oxide is dispersed in water, obtains graphene oxide solution；Anode material for lithium-ion batteries is scattered in organic solvent, obtain positive electrode dispersion liquid；Graphene oxide solution is added dropwise in positive electrode dispersion liquid, stirred, is staticly settled, obtained sediment is dried in atmosphere；Dry combined oxidation graphene anode material is subjected to heating reduction under vacuum, obtains composite graphite alkene positive electrode.Beneficial effects of the present invention are as follows：The electronic conductivity of anode material for lithium-ion batteries is improved, improves its cycle performance and high rate performance；Operational procedure is simple, efficiently, and energy consumption is low, green, short preparation period, easily controllable；Organic solvent used in preparation process can recycle, and substantially reduce preparation cost, be produced suitable for large-scale promotion.
Description
Technical field
The present invention relates to technical field of lithium ion battery positive pole material preparation, particularly relates to a kind of graphene-based lithium-ion electric
The preparation method of pond positive electrode.
Background technology
With the continuous development of human society, people are continuously increased to the demand of the energy, and traditional fossil energy excessively makes
With serious environmental pollution is brought, therefore, the development high-efficiency environment friendly energy turns into study hotspot.In a series of energy, lithium ion
Battery is because it has the characteristics that operating voltage is high, energy density is high, has extended cycle life, the environment-friendly extensive pass for causing people
Note.
Lithium ion battery is mainly made up of the part such as electrolyte, barrier film, positive electrode and negative material.Wherein positive electrode
Most important, its characteristic has to the energy storage density of lithium ion battery, cycle life, security, cost etc. to be directly affected, because
This anode material for lithium-ion batteries turns into the emphasis of research.At present, anode material for lithium-ion batteries mainly has cobalt acid lithium, nickel acid
Lithium, the LiMn2O4 of spinel structure, the LiFePO4 and ternary material of olivine structural.These positive electrodes exist in itself
Defect, such as electronic conductivity are low, cycle performance is bad, high rate performance is poor.
Because the electrode reaction of lithium ion battery occurs in electrode electrolyte interface, therefore change lithium ion cell positive material
One effective ways of material chemical property are exactly that surface parcel is carried out to it, and integument can improve the conduction of positive electrode
Property, cycle performance and high rate performance.Graphene has good electric conductivity, uses it for changing anode material for lithium-ion batteries
Enter, the anode composite material of high conductivity can be prepared, improve the chemical property of anode material for lithium-ion batteries.
Has the preparation method of some grapheme composite positive electrode materials on the market at present, still, these methods mostly compare
Complexity, preparation efficiency are low, it is high to prepare cost, are not suitable for large-scale promotion production.Therefore, there is an urgent need to a kind of letter of preparation process
Preparation method that is single, preparing the cheap graphene-based anode material for lithium-ion batteries of cost, this is carried to performance of lithium ion battery
Height possesses significance.
The content of the invention
The present invention proposes a kind of preparation method of graphene-based anode material for lithium-ion batteries, solves lithium in the prior art
The problem of ion battery positive electrode chemical property difference.
The technical proposal of the invention is realized in this way：
A kind of preparation method of graphene-based anode material for lithium-ion batteries, its method and step are as follows：
(1) graphite oxide is made by chemical oxidization method using natural flake graphite, graphite oxide is dispersed in water, obtained
To certain density graphene oxide solution；
(2) anode material for lithium-ion batteries is disperseed in organic solvent, to obtain certain density positive electrode dispersion liquid,
Stir standby；
(3) graphene oxide solution is added dropwise in positive electrode dispersion liquid according to a certain percentage, stirred, it is quiet
Precipitation is put, obtained sediment is dried in atmosphere, obtains combined oxidation graphene anode material；
(4) dry combined oxidation graphene anode material is subjected to heating reduction under vacuum, obtains composite stone
Black alkene positive electrode, i.e., graphene-based anode material for lithium-ion batteries.
Preferably, natural flake graphite is aoxidized using modified Hummers methods in the step (1), oxidation temperature
Spend for 0 DEG C~55 DEG C, oxidization time is 2h~4h；Ultrasonic time is 20s~15min, and ultrasonic power is 400W~600W；Centrifugation
Rotating speed is 3000rmp~6000rmp, and centrifugation time is 5min~10min；The size of the natural flake graphite is 1~100 μ
m；The concentration of the graphene oxide solution is 1mg/mL~3mg/mL.
Preferably, organic solvent is acetone, ethanol or methanol in the step (2)；The positive electrode dispersion liquid
Concentration is 1mg/mL~3mg/mL.
Preferably, the weight of graphene oxide and positive electrode ratio is 5: 95~10: 90 in the step (3).
Preferably, the temperature of heating reduction is 250 DEG C~450 DEG C in the step (4), the time is 2h~3.5h.
Used organic solvent, which can pass through, in preparation method of the present invention filters, is isolated clean organic molten
Agent, so as to realize the recycling of organic solvent, reduce cost.
Beneficial effects of the present invention are：
The method of the invention improves lithium ion battery by the way that graphene is compounded on anode material for lithium-ion batteries
The electronic conductivity of positive electrode, improve its cycle performance and high rate performance.
The method of the invention operational procedure is simple, efficiently, and energy consumption is low, green, short preparation period, easily controllable；
Organic solvent used in preparation process can recycle, and substantially reduce preparation cost, be produced suitable for large-scale promotion.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the anode material for lithium-ion batteries of non-composite graphite alkene and the lithium ion cell positive after composite graphite alkene
Lithium electricity data comparison figure of the material under 0.2 multiplying power；
Fig. 2 is the anode material for lithium-ion batteries of non-composite graphite alkene and the lithium ion cell positive after composite graphite alkene
Lithium electricity data comparison figure of the material under 0.5 multiplying power.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
Embodiment 1
Anode material for lithium-ion batteries LiFePO4 is scattered in ethanol for 2mg/mL by concentration, stir.With modification
Hummers methods prepare graphite oxide, and then prepare graphene oxide solution (wherein the size of graphene is 1 μm~50 μm), and
Diluted concentration is 2mg/mL.
Under agitation, by weight for the ratio of 10: 90 (graphene oxides: positive electrode) that graphene oxide is molten
Liquid is added dropwise in positive electrode dispersion liquid, is stirred, and is staticly settled, and obtained sediment is dried in atmosphere；
Further by dry sediment under vacuum, 3.5h is reduced under 450 DEG C of reduction temperatures, obtains required composite graphite alkene
Positive electrode.
Used ethanol is by filtering, separation, obtains clean ethanol, recycles.
Electron microscopic observation result shows：Positive electrode LiFePO4 particles are wrapped up by graphene on this condition, and wrap up
Closely.
Assembling lithium ion battery test result shows：Positive electrode capacity boost 16% after composite graphite alkene, circulation
Performance boost 23%, high rate performance improve 21%.
Embodiment 2
Anode material for lithium-ion batteries LiFePO4 is scattered in ethanol for 2mg/mL by concentration, stir.With modification
Hummers methods prepare graphite oxide, and then prepare graphene oxide solution (wherein the size of graphene is 50 μm~100 μm),
And diluted concentration is 2mg/mL.
Under agitation, by weight for the ratio of 5: 95 (graphene oxides: positive electrode) that graphene oxide is molten
Liquid is added dropwise in positive electrode dispersion liquid, is stirred, and is staticly settled, and obtained sediment is dried in atmosphere；
Further by dry sediment under vacuum, 3.5h is reduced under 450 DEG C of reduction temperatures, obtains required composite graphite alkene
Positive electrode.
Used ethanol is by filtering, separation, obtains clean ethanol, recycles.
Electron microscopic observation result shows：Positive electrode LiFePO4 particles are wrapped up by graphene on this condition, and wrap up
Closely.
Assembling lithium ion battery test result shows：Positive electrode capacity boost 27% after composite graphite alkene, circulation
Performance boost 35%, high rate performance improve 33%.
Embodiment 3
Anode material for lithium-ion batteries LiNi0.5Co0.2Mn0.3O2 is scattered in methyl alcohol for 2mg/mL by concentration, stir
Mix uniformly.Graphite oxide is prepared with modified Hummers methods, and then (wherein the size of graphene is 1 to preparation graphene oxide solution
μm~50 μm), and diluted concentration is 2mg/mL.
Under agitation, by weight for the ratio of 5: 95 (graphene oxides: positive electrode) that graphene oxide is molten
Liquid is added dropwise in positive electrode dispersion liquid, is stirred, and is staticly settled, and obtained sediment is dried in atmosphere；
Further by dry sediment under vacuum, 3h is reduced under 350 DEG C of reduction temperatures, is obtaining required composite graphite alkene just
Pole material.
Used methanol is by filtering, separation, obtains clean methanol, recycles.
Electron microscopic observation result shows：Positive electrode LiNi0.5Co0.2Mn0.3O2 particles are by graphene bag on this condition
Wrap up in, its small particles is completely wrapped, and bulky grain is portion envelops.
Assembling lithium ion battery test result shows：Positive electrode capacity boost 20% after composite graphite alkene, circulation
Performance boost 17%, high rate performance improve 19%.
Embodiment 4
Anode material for lithium-ion batteries LiNi0.5Co0.2Mn0.3O2 is scattered in methyl alcohol for 2mg/mL by concentration, stir
Mix uniformly.Graphite oxide is prepared with modified Hummers methods, and then (wherein the size of graphene is 1 to preparation graphene oxide solution
μm~50 μm), and diluted concentration is 2mg/mL.
Under agitation, by weight for the ratio of 10: 90 (graphene oxides: positive electrode) that graphene oxide is molten
Liquid is added dropwise in positive electrode dispersion liquid, is stirred, and is staticly settled, and obtained sediment is dried in atmosphere；
Further by dry sediment under vacuum, 3h is reduced under 350 DEG C of reduction temperatures, is obtaining required composite graphite alkene just
Pole material.
Used methanol is by filtering, separation, obtains clean methanol, recycles.
Electron microscopic observation result shows：Positive electrode LiNi0.5Co0.2Mn0.3O2 particles are by graphene bag on this condition
Wrap up in, its small particles is completely wrapped, and bulky grain is portion envelops.
Assembling lithium ion battery test result shows：Positive electrode capacity boost 35% after composite graphite alkene, circulation
Performance boost 31%, high rate performance improve 32%.
Embodiment 5
Anode material for lithium-ion batteries LiNi0.5Co0.2Mn0.3O2 is scattered in ethanol for 2mg/mL by concentration, stir
Mix uniformly.Graphite oxide is prepared with modified Hummers methods, and then prepares graphene oxide solution (size of wherein graphene is
50 μm~100 μm), and diluted concentration is 2mg/mL.
Under agitation, by weight for the ratio of 5: 95 (graphene oxides: positive electrode) that graphene oxide is molten
Liquid is added dropwise in positive electrode dispersion liquid, is stirred, and is staticly settled, and obtained sediment is dried in atmosphere；
Further by dry sediment under vacuum, 3h is reduced under 450 DEG C of reduction temperatures, is obtaining required composite graphite alkene just
Pole material.
Used ethanol is by filtering, separation, obtains clean ethanol, recycles.
Electron microscopic observation result shows：Positive electrode LiNi0.5Co0.2Mn0.3O2 particles are by graphene bag on this condition
Wrap up in, its small particles is completely wrapped, and bulky grain is portion envelops.
Assembling lithium ion battery test result shows：Positive electrode capacity boost 21% after composite graphite alkene, circulation
Performance boost 23%, high rate performance improve 29%.
Embodiment 6
Anode material for lithium-ion batteries LiFePO4 is scattered in acetone for 2mg/mL by concentration, stir.With modification
Hummers methods prepare graphite oxide, and then prepare graphene oxide solution (wherein the size of graphene is 1 μm~50 μm), and
Diluted concentration is 2mg/mL.
Under agitation, by weight for the ratio of 5: 95 (graphene oxides: positive electrode) that graphene oxide is molten
Liquid is added dropwise in positive electrode dispersion liquid, is stirred, and is staticly settled, and obtained sediment is dried in atmosphere；
Further by dry sediment under vacuum, 3.5h is reduced under 450 DEG C of reduction temperatures, obtains required composite graphite alkene
Positive electrode.
Used acetone is by filtering, separation, obtains clean acetone, recycles.
Electron microscopic observation result shows：Positive electrode LiFePO4 particles are wrapped up by graphene on this condition, and wrap up
Closely.
Assembling lithium ion battery test result shows：Positive electrode capacity boost 10% after composite graphite alkene, circulation
Performance boost 17%, high rate performance improve 13%.
As shown in figure 1, assembling test, under 0.2 multiplying power, the lithium-ion electric of non-composite graphite alkene are carried out to lithium ion battery
Pond positive electrode LiNi0.5Co0.2Mn0.3O2 discharge capacity first is 148.2mAh/g, and capacity is after circulating 50 times
123.9mAh/g, capability retention 83.6%.Anode material for lithium-ion batteries after composite graphite alkene
LiNi0.5Co0.2Mn0.3O2 discharge capacity first is 171.5mAh/g, capacity boost 23.3mAh/g；After circulation 50 times
Capacity is 148.4mAh/g, capacity boost 24.5mAh/g；Capability retention is 86.5%.
As shown in Fig. 2 assembling test, under 0.5 multiplying power, the lithium-ion electric of non-composite graphite alkene are carried out to lithium ion battery
Pond positive electrode LiNi0.5Co0.2Mn0.3O2 discharge capacity first is 108.9mAh/g, and capacity is after circulating 100 times
68.6mAh/g, capability retention 63%.Anode material for lithium-ion batteries after composite graphite alkene
LiNi0.5Co0.2Mn0.3O2 discharge capacity first is 132.2mAh/g, capacity boost 23.3mAh/g；After circulation 100 times
Capacity is 101.5mAh/g, capacity boost 32.9mAh/g；Capability retention is 76.8%.
In summary, the method for the invention is improved by the way that graphene is compounded on anode material for lithium-ion batteries
The electronic conductivity of anode material for lithium-ion batteries, improve its cycle performance and high rate performance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (5)
1. a kind of preparation method of graphene-based anode material for lithium-ion batteries, it is characterised in that its method and step is as follows：
(1) graphite oxide is made by chemical oxidization method using natural flake graphite, graphite oxide is dispersed in water, obtain one
Determine the graphene oxide solution of concentration；
(2) anode material for lithium-ion batteries is disperseed in organic solvent, to obtain certain density positive electrode dispersion liquid, stirred
It is uniformly standby；
(3) graphene oxide solution is added dropwise in positive electrode dispersion liquid according to a certain percentage, stirred, it is heavy to stand
Form sediment, obtained sediment is dried in atmosphere, obtains combined oxidation graphene anode material；
(4) dry combined oxidation graphene anode material is subjected to heating reduction under vacuum, obtains composite graphite alkene
Positive electrode, i.e., graphene-based anode material for lithium-ion batteries.
A kind of 2. preparation method of graphene-based anode material for lithium-ion batteries according to claim 1, it is characterised in that
Natural flake graphite is aoxidized using modified Hummers methods in the step (1), oxidizing temperature is 0 DEG C~55 DEG C, oxidation
Time is 2h~4h；Ultrasonic time is 20s~15min, and ultrasonic power is 400W~600W；Centrifugal rotational speed be 3000rmp~
6000rmp, centrifugation time are 5min~10min；The size of the natural flake graphite is 1~100 μm；The graphene oxide
The concentration of solution is 1mg/mL~3mg/mL.
A kind of 3. preparation method of graphene-based anode material for lithium-ion batteries according to claim 2, it is characterised in that
Organic solvent is acetone, ethanol or methanol in the step (2)；The concentration of the positive electrode dispersion liquid is 1mg/mL~3mg/
mL。
A kind of 4. preparation method of graphene-based anode material for lithium-ion batteries according to claim 3, it is characterised in that
The weight of graphene oxide and positive electrode ratio is 5: 95~10: 90 in the step (3).
A kind of 5. preparation method of graphene-based anode material for lithium-ion batteries according to claim 1, it is characterised in that
The temperature of heating reduction is 250 DEG C~450 DEG C in the step (4), and the time is 2h~3.5h.
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Cited By (1)
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Application publication date: 20180116 |