CN108281634A - A kind of method and its application of graphene coated graphite negative material of lithium ion battery - Google Patents
A kind of method and its application of graphene coated graphite negative material of lithium ion battery Download PDFInfo
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- CN108281634A CN108281634A CN201810076397.0A CN201810076397A CN108281634A CN 108281634 A CN108281634 A CN 108281634A CN 201810076397 A CN201810076397 A CN 201810076397A CN 108281634 A CN108281634 A CN 108281634A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 discloses a kind of method of graphene coated graphite negative material of lithium ion battery, includes the following steps:(1) graphite ultrasonic disperse is obtained into graphite suspension in solvent;(2) graphite oxide ultrasonic dissolution is obtained into graphene oxide solution in solvent;(3) mass ratio for pressing graphene oxide and graphite is 0.01~0.3:1, graphite suspension is added in graphene oxide solution, then ultrasonic mixing removes solvent, obtain dry solid powder;(4) under an inert atmosphere, the solid powder obtained by step (3) handles 1~4h in 600~1000 DEG C, cooling to obtain the graphite negative material of lithium ion battery of graphene coated.This method is simple and practicable, and energy consumption is low, and environmental-friendly, at low cost, covered effect is good, and purity is high, suitable for large batch of industrialized production.Without adding conductive agent when as lithium ion battery negative material, and cycle performance is very excellent, and first charge discharge efficiency is up to 90%.
Description
The application be the applying date be on April 21st, 2015, application No. is 201510190383.8 applications for a patent for invention " one
The divisional application of the method for kind graphene coated graphite negative material of lithium ion battery and application ".
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of graphene coated graphite negative material of lithium ion battery
Method and its application.
Background technology
Lithium ion battery has entered functionization the seventies as a kind of emerging power supply, because of its, electricity high with energy density
The advantages that cell voltage is high, storage life is long, is widely used on various portable electronic products and electric tool, especially exists
It plays an important role in terms of electric vehicle (EV) and hybrid-electric car (HEV) power supply.
Negative material is one of critical material of lithium ion battery, and carbonaceous material is people's early start studies and apply
In the material of negative electrode of lithium ion battery, carbonaceous materials are still received significant attention so far and are mainly had the following advantages:Specific capacity is high
(200~400mAh/g), electrode potential is low, cycle efficieny height (>95%) it, has extended cycle life.It is negative that more carbonaceous is studied at present
Pole material has graphite, mesocarbon microspheres (MCMB), height ratio capacity carbide, petroleum coke etc..These carbonaceous materials respectively have its excellent
Disadvantage, in recent years, as that studies carbonaceous material deepens continuously, it has been found possible to by being tied to all kinds of carbonaceous materials
Structure adjusts, and such as forms nano grade pore structure, is surface modified and modification or doping treatment.It may make lithium wherein
Insertion/deintercalation not only can stoichiometrically LiC6It carries out, and also non-stoichiometric insertion/deintercalation, to make carbonaceous
Material specific capacity is more than the theoretical value 372mAhg of graphite, reaches 700g~1000mAh/g.Meanwhile using nanometer carbon material,
A new research hotspot is had become as lithium ion battery negative material.But because source and the preparation of nanometer carbon material
Method is different.Structure has very big difference and causes to be very different in its embedding lithium capacity and embedding lithium mechanism.
Graphene is the basic unit for constituting other carbon material structures, and graphene wraps up the fullerene that can form zero dimension,
One-dimensional carbon nanotube can be formed by curling, and superposition can form three-dimensional graphite.The theoretical specific surface area of grapheme material is high
Up to 2600m2/ g has heat conductivility outstanding and ultimate strength, and the electron mobility of high speed at room temperature, these are excellent
Property makes it have very big development prospect in terms of energy storage.But as a kind of brand-new material graphene itself agglomeration traits
It can not solve well always.
Current commercialized graphite cathode material has more highly oriented layer structure, sensitive to electrolyte, with solvent phase
Capacitive is poor;The high current charge-discharge ability of graphite cathode material is relatively low, causes power performance poor.Simultaneously as graphite
Interlamellar spacing is less than lithium and is inserted into the compound between graphite layers Li formed after graphite liningsxC6Crystal face interlamellar spacing (d002=0.37nm),
During charge and discharge cycles, graphite layers are away from changing greatly;And also occur that lithium is inserted into graphite layers jointly with organic solvent
And the further decomposition of organic solvent.It is easy to cause that graphite linings are gradually peeled off, graphite particle is burst apart and dusting, to drop
Low negative material cycle life.
Invention content
For the above problem of the prior art, it is negative that the object of the present invention is to provide a kind of lithium ion graphite of graphene coated
The preparation method of pole material.This method is simple and practicable, and energy consumption is low, and environmental-friendly, at low cost, covered effect is good, suitable for large quantities of
The industrialized production of amount.
A kind of method of graphene coated graphite negative material of lithium ion battery, includes the following steps:
(1) graphite ultrasonic disperse is obtained into graphite suspension in solvent;
(2) graphite oxide ultrasonic dissolution is obtained into graphene oxide solution in solvent;
(3) mass ratio for pressing graphene oxide and graphite is (0.01~0.3):1, graphite is added in graphene oxide solution
Suspension obtains mixed liquor;
(4) and then solvent is removed, obtains dry solid powder;
(5) under an inert atmosphere, the solid powder obtained by step (4) handles 1~4h in 600~1000 DEG C, and cooling to obtain the final product
To the graphite negative material of lithium ion battery of graphene coated.
Further, the solvent described in step (1) and/or step (2) is water, ethyl alcohol and/or acetone.
Further, the solvent in the step (1) is water and ethyl alcohol, and graphite ultrasonic agitation is first distributed to a small amount of ethyl alcohol
In, then water is added, ultrasonic disperse obtains graphite suspension.In the step (1), contain in graphite suspension described in every 100mL
The amount of graphite is 10g.
Further, the solvent in the step (2) is water.In the step (2), it is configured to per 0.2g graphene oxides
Graphene oxide solution described in 50mL.
In the step (3), under stiring, slowly graphene oxide water solution is added in graphite suspension, is surpassed
Sound 30min is further continued for stirring 2 hours, obtains mixed liquor.
Further, the process of step (4) removing solvent includes:Filtering, drying;Alternatively, evaporation, drying;Or spraying is dry
It is dry.
Preferably, the method for step (4) the removing solvent is:The mixed liquor that first step 3 is obtained is using filtering, steaming
Hair or the preliminary removal solvent of spray drying, obtained solid powder, then solid powder is first dried overnight in draught cupboard,
Then 10 hours dry in 50 DEG C in vacuum drying chamber.
Further, step (5) described inert atmosphere is nitrogen, argon gas and/or helium.
Further, in step (5), temperature rises to 600~1000 DEG C with the speed of 1~3 DEG C/min.It is preferred that with 2 DEG C/min
Speed rise to 800 DEG C.
It is not necessary that any conductive agent is added when according to material obtained by the above method as lithium ion battery negative material, and follow
Ring performance is very excellent, and first charge discharge efficiency is up to 90%.
Main advantages of the present invention are:
1, graphene oxide removes oxygen-containing group at high temperature, woth no need to separately plus reducing agent, will not introduce any metal from
Son makes product keep very high degree of purity;
2, graphene layer can be effectively coated on to the surface of graphite cathode material, covered effect is good;
3, without adding conductive agent, and cyclicity when the material of present invention gained is used as lithium ion battery negative material
Can be very excellent, first charge discharge efficiency is up to 90% or more;
4, the method for the present invention is simple for process, and mild condition, technological parameter is easily-controllable, and energy consumption is low, environmentally friendly, is conducive to work
Industryization mass produces.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of 1 resulting materials of embodiment.
Fig. 2 is first charge-discharge curve of 1 resulting materials of embodiment as lithium ion battery negative material, and voltage range is
0.005~2.000V, 0.1C.
Fig. 3 is efficiency and cycle performance of 1 resulting materials of embodiment as lithium ion battery negative material.
Specific implementation mode
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
1. weighing 10g graphite samples (natural spherical plumbago) in 250ml beakers, a small amount of ethyl alcohol is added, with ultrasonic agitation
Dispersion, then water is added, ultrasound is made into the graphite suspension of 100ml;
2. weighing 0.2g graphite oxides in 100ml beakers, add water, under ultrasonic agitation, is made into the graphite oxide of 50ml
Aqueous solution;
3. under stiring, slowly 50ml graphene oxide water solutions are added in 100ml graphite suspensions, then surpass
Sound 30 minutes is further continued for stirring 2 hours, obtains mixed liquor;
4. filtering above-mentioned mixed liquor, obtained solid powder is first dried overnight in draught cupboard, then in vacuum drying chamber
In it is 10 hours dry in 50 DEG C;
5. dried solid powder sample is put into tube furnace, it is passed through N2(flow velocity 50ml/min), then with 2 DEG C/
Min rises to 800 DEG C, is sintered 2 hours postcoolings at such a temperature to room temperature to get to the graphite composite material of graphene coated.
As seen from Figure 1, thin graphene is wrapped in graphite particle surface, has good being evenly coated property.
(300 turns/min) ball milling is after 2 hours under the low speed for the composite material of 1 gained of embodiment, by itself and Kynoar
(PVDF) 92 are pressed:8 mass ratio is made into film after slurry, and cathode selects metal lithium sheet, and electrolyte is that electrolyte is 1mol/L's
LiPF6/ ethylene carbonate+diethyl carbonate (1:1), diaphragm is polypropylene microporous film, and button cell is made, and evaluates its conduct
The performance of lithium cell negative pole material.
Fig. 2 is the first charge-discharge curve of button cell, and charging/discharging voltage section is 0.005~2.000V, and electric current is
(1C=372mAh/g) is arranged in 0.1C, and test temperature is 20 DEG C, graphene modified graphite cathode material charge and discharge specific capacity for the first time
Respectively:372mAh/g (charging) and 410mAh/g (electric discharge), efficiency 90.7%, and non-modified graphite cathode material is for the first time
Charge and discharge specific capacity is respectively:350mAh/g (charging) and 393mAh/g (electric discharge), efficiency 89%.
Fig. 3 is the efficiency and cycle performance figure of battery, as shown, after 20 circle of 0.3C cycles, capacity retention ratio 98%.
Embodiment 2
It is 900 DEG C to change sintering temperature, other conditions such as embodiment 1.
Embodiment 3
It is 4 hours to change sintering time, other conditions such as embodiment 1.
Embodiment 3
The quality for changing graphite oxide is 1.06g, other conditions such as embodiment 1.
Embodiment 4
1. weighing 10g graphite samples (business electrographite) in 250ml beakers, a small amount of ethyl alcohol is added, with ultrasonic agitation
Dispersion, then water is added, ultrasound is made into the graphite suspension of 100ml;
2. weighing 0.2g graphite oxides in 100ml beakers, add water, under ultrasonic agitation, is made into the graphite oxide of 50ml
Aqueous solution;
3. under stiring, slowly 50ml graphene oxide water solutions are added in 100ml graphite suspensions, then surpass
Sound 30 minutes is further continued for stirring 2 hours, obtains mixed liquor;
4. after carefully removing the evaporation of the solvent of above-mentioned mixed liquor, obtained solid powder is again in vacuum drying chamber in 50
DEG C dry 10 hours;
5. dried solid powder sample is put into tube furnace, it is passed through N2(flow velocity 50ml/min), then with 2 DEG C/
Min rises to 800 DEG C, keeps 2 hours postcoolings to room temperature to get to the graphite composite material of graphene coated at such a temperature.
Embodiment 5
1. weighing 10g graphite samples (natural spherical plumbago) in 250ml beakers, a small amount of ethyl alcohol is added, with ultrasonic agitation
Dispersion, then water is added, ultrasound is made into the graphite suspension of 100ml;
2. weighing 0.2g graphite oxides in 100ml beakers, add water, under ultrasonic agitation, is made into the graphite oxide of 50ml
Aqueous solution;
3. under stiring, slowly 50ml graphene oxide water solutions are added in 100ml graphite suspensions, then surpass
Sound 30 minutes is further continued for stirring 2 hours, obtains mixed liquor;
4. above-mentioned mixed liquor is handled using spray drying process, obtained solid powder first stays overnight drying in draught cupboard, so
50 DEG C of dryings 10 hours in vacuum drying chamber afterwards;
5. dried solid powder sample is put into tube furnace, it is passed through N2(flow velocity 50ml/min), then with 2 DEG C/
Min rises to 800 DEG C, keeps 2 hours postcoolings to room temperature to get to the graphite composite material of graphene coated at such a temperature.
The ion cathode material lithium of graphene coated graphite made from embodiment 2,3,4,5 is similar to 1 pattern of embodiment, material
Excellent charging and discharging capacity and cycle performance are embodied after material assembly battery.
Conclusion:
The ion cathode material lithium product purity of graphene coated graphite made from method provided by the invention is high.Material fills
With embodying excellent charging and discharging capacity and cycle performance after battery.Simple production process is easy, and energy consumption is low, environment friend
It is good, it is at low cost, suitable for large batch of industrialized production.
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (10)
1. a kind of method of graphene coated graphite negative material of lithium ion battery, includes the following steps:
(1) graphite ultrasonic disperse is obtained into graphite suspension in solvent;
(2) graphite oxide ultrasonic dissolution is obtained into graphene oxide solution in solvent;
(3) mass ratio for pressing graphene oxide and graphite is (0.01~0.3):1, graphite is added in graphene oxide solution and is suspended
Liquid obtains mixed liquor;
(4) and then solvent is removed, obtains dry solid powder;
(5) under an inert atmosphere, the solid powder obtained by step (4) handles 1~4h in 600~1000 DEG C, cooling to obtain stone
The graphite negative material of lithium ion battery of black alkene cladding.
2. according to the method described in claim 1, it is characterized in that, molten described in the step (1) and/or the step (2)
Agent is water, ethyl alcohol and/or acetone.
3. according to the method described in claim 2, it is characterized in that, the solvent in the step (1) is water and ethyl alcohol, first by stone
Ink ultrasonic agitation is distributed in a small amount of ethyl alcohol, then adds water, and ultrasonic disperse obtains graphite suspension;
Preferably, in the step (1), the amount containing graphite is 10g in graphite suspension described in every 100mL.
4. according to the method described in claim 2, it is characterized in that, the solvent in the step (2) is water;
Preferably, in the step (2), graphene oxide solution described in 50mL is configured to per 0.2g graphene oxides.
5. according to the method described in claim 1, it is characterized in that, in the step (3), under stiring, will slowly aoxidize
Graphene aqueous solution is added in graphite suspension, ultrasonic 30min, is further continued for stirring 2 hours, is obtained mixed liquor.
6. according to the method described in claim 1, it is characterized in that, the process that step (4) removes solvent includes:Filtering, drying;
Alternatively, evaporation, drying;Or spray drying;
Preferably, the method for step (4) the removing solvent is:The mixed liquor that first step 3 is obtained using filtering, evaporation or
The preliminary removal solvent of person's spray drying, obtained solid powder, then solid powder is first dried overnight in draught cupboard, then exist
It is 10 hours dry in 50 DEG C in vacuum drying chamber.
7. according to the method described in claim 1, it is characterized in that, step (5) described inert atmosphere be nitrogen, argon gas and/or
Helium.
8. according to the method described in claim 1, it is characterized in that, in step (5), temperature is risen to the speed of 1~3 DEG C/min
600~1000 DEG C, preferable temperature rises to 800 DEG C with the speed of 2 DEG C/min.
9. the material obtained according to any methods of claim 1-5.
10. application of the material described in claim 6 as lithium ion battery negative material.
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CN201510190383.8A CN104868106A (en) | 2015-04-21 | 2015-04-21 | Method for coating graphite anode material of lithium ion battery with graphene and application thereof |
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CN114551830A (en) * | 2022-02-21 | 2022-05-27 | 海城申合科技有限公司 | Preparation method of graphene oxide coated artificial graphite lithium ion negative electrode material |
CN114804094A (en) * | 2022-04-15 | 2022-07-29 | 广东凯金新能源科技股份有限公司 | Nitrogen-graphene doped composite graphite negative electrode material and preparation method thereof |
CN115000371A (en) * | 2022-06-06 | 2022-09-02 | 深圳材启新材料有限公司 | Preparation method of graphene-coated graphite powder |
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