CN109742363A - One kind may be implemented graphene and closely coats SiO negative materials and preparation method thereof - Google Patents
One kind may be implemented graphene and closely coats SiO negative materials and preparation method thereof Download PDFInfo
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- CN109742363A CN109742363A CN201910017791.1A CN201910017791A CN109742363A CN 109742363 A CN109742363 A CN 109742363A CN 201910017791 A CN201910017791 A CN 201910017791A CN 109742363 A CN109742363 A CN 109742363A
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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 that one kind may be implemented graphene and closely coat SiO negative materials and preparation method thereof, solve the problems, such as that battery cathode silicon substrate raw material theoretical capacity is low in the prior art, poor circulation, a kind of preparation method that graphene may be implemented and closely coats SiO negative materials comprising the steps of: the 1) preparation of the modified graphene oxide solution in surface: the 2) preparation of SiO dispersion liquid；3) preparation of graphene oxide coated Si O composite material；4) preparation of graphene coated SiO composite material, the close ultrathin membrane coated Si O composite material of graphene may be implemented in this method completely, and this method preparation process is simple, and at low cost, the period is short, environmental protection, and magnanimity preparation may be implemented.
Description
Technical field
The present invention relates to cell negative electrode material technical fields, and particularly relating to one kind may be implemented the close coated Si O of graphene
Negative electrode material and preparation method thereof.
Background technique
Lithium ion battery has many advantages, for example, energy density it is high, have extended cycle life, memory-less effect etc., due to it
These advantages, lithium ion battery become the ideal energy storage device in the fields such as mobile electronic device, electric tool.With national
Lithium ion battery is included in the medium-term and long-term scientific and technological development planning outline of 2006~the year two thousand twenty, and to renewable energy and
The great attention of electric car, to performances such as the energy densities of lithium ion battery, more stringent requirements are proposed.
Lithium ion battery is mainly made of cathode, anode, electrolyte, diaphragm etc..Graphite cathode has been carried out business at present
Change.For performances such as the energy densities that improves lithium ion battery, need to research and develop novel negative electrode material.Silicon is in the world
The highest substance of content, the theoretical capacity (4200mAh/g) with superelevation are expected to become next-generation business negative electrode material.
There are some problems, such as huge expansion are poor so as to cause mechanical stability in charge and discharge process for silica-base material
It is low with side reaction increase and powder, conductivity poor so as to cause charge-discharge performance.Carbon coating is to solve silica-base material most to have
The method of effect, because the volume expansion of silica-base material can be limited later by carbon coating to improve mechanical stability and reduction
The generation of side reaction and inhibition powder；Since carbon material has good electric conductivity, silicon substrate can be improved after carbon coating
The conductivity of material improves charge-discharge performance.Graphene is as novel nanometer two dimension carbon material, the specific surface with superelevation
Product, light weight, ultrathin, superelevation conductivity, SiO material surface can be coated on, realize close ultrathin membrane packet
It covers, so that restricted volume expansion and raising conductivity, become SiO and coat optimal carbon source.
Summary of the invention
The present invention proposes that one kind may be implemented graphene and closely coat SiO negative materials and preparation method thereof, solves existing
There is in technology the problem of low battery cathode silicon substrate raw material theoretical capacity, poor circulation.
The technical scheme of the present invention is realized as follows: a kind of graphene that may be implemented closely coats SiO negative materials
Preparation method comprising the steps of:
1) preparation of the modified graphene oxide solution in surface: use natural flake graphite for raw material, by modified
Hummers method prepares graphite oxide, and centrifugation washing obtains graphene oxide slurry, by graphene oxide slurry ultrasonic disperse to water
In, centrifugation removes unstripped graphite and obtains graphene oxide solution, and surfactant is added in graphene oxide solution, surpasses
Sound is uniformly dispersed, and obtains the modified graphene oxide solution in surface；
2) preparation of SiO dispersion liquid: SiO powder is added in organic solvent, by stirring to get finely dispersed SiO
Dispersion liquid；
3) preparation of graphene oxide coated Si O composite material: under agitation, by the modified graphene oxide in surface
Solution is slowly added into SiO dispersion liquid, then heating stirring, is staticly settled, filters pressing separation, and vacuum drying obtains oxidation stone
The SiO composite material of black alkene cladding；
4) preparation of graphene coated SiO composite material: high temperature reduction obtains stone under conditions of protective gas or vacuum
Black alkene coated Si O composite material.
Preferably, when graphene oxide slurry being distributed in water in step 1), the volume of graphene oxide slurry and water
Than being 1: 2~1: 12, ultrasonic power is 80~1000W, and the time is 3~60min, and centrifugal rotational speed is 1000~12000rpm, when
Between be 2~30min, the concentration of graphene oxide solution is 0.5~10mg/mL.
Preferably, centrifugal rotational speed when centrifugation washing obtains graphene oxide slurry in step 1) is 1000~
15000rpm, centrifugation time are 2~30min.
Preferably, the mass ratio of graphene oxide and surfactant is 10: 1~2: 1 in step 1), and surfactant is
One or more of neopelex, dodecyl sodium sulfate, kayexalate, sodium citrate, citric acid,
The power of ultrasound is 80~1000W, and the time is 3~60min.
Preferably, the size of SiO powder is 50nm~100 μm in step (2), and organic solvent is methanol, dehydrated alcohol, different
One of propyl alcohol, ethylene glycol, acetone, pyruvic alcohol, the concentration of SiO powder in organic solvent are 0.5~20mg/mL, stirring
Revolving speed is 50~1000rpm, and the time is 3~60min.
Preferably, speed of agitator is 50~1000rpm in step (3), and the mass ratio of SiO and graphene oxide is 100: 1
~3: 1, the addition rate of the modified graphene oxide solution in surface is 0.1~10mL/min, and heating temperature is 20~70 DEG C, is stirred
Mixing the time is 3~60min.
Preferably, the temperature of step (4) high temperature reduction is 200~2000 DEG C, and the time is 0.5~10h, and heating rate is
1~20 DEG C/min, protective gas is nitrogen or argon gas.
Preferably, the mesh number of natural flake graphite is 32~1000 mesh in step (1).
The present invention also proposes the graphene coated SiO negative materials that thus method of planting is prepared.
The features of the present invention and beneficial effect are:
1. the present invention prepares ultra-thin graphene oxide using modified Hummers method, realizes graphene and SiO is surpassed
Film coated.
2. the present invention is added to surfactant in graphene oxide solution, increase graphene oxide and SiO particle table
The binding force in face, make graphene oxide it is even closer be coated on SiO particle surface, realize graphene to the close of SiO material
Cladding.
3. this method preparation process is simple, organic solvent used is all common solvents, and price is low, and at low cost, the period is short, ring
It protects, magnanimity preparation may be implemented.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Embodiment 1:
A kind of preparation method that graphene may be implemented and closely coats SiO negative materials, comprising the following steps:
1) it the preparation of the modified graphene oxide solution in surface: uses natural flake graphite for raw material, first passes through modified
Hummers method prepares graphite oxide, and 2min is centrifuged under 1000~15000rpm revolving speed and washes to obtain graphene oxide slurry, is pressed
According to volume ratio be 1: 12 ratio under 80W power ultrasound 3min graphene oxide slurry is distributed in water, 1000~
Centrifugation 2min removes unstripped graphite and obtains graphene oxide solution under 12000rpm revolving speed, adds in graphene oxide solution
Enter surfactant, ultrasound 3min is uniformly dispersed under the power of 80W, obtains the modified graphene oxide solution in surface；
2) preparation of SiO dispersion liquid: SiO powder is added in organic solvent, and 3min is stirred under 1000rpm revolving speed and is obtained
To finely dispersed SiO dispersion liquid.
3) preparation of graphene oxide coated Si O composite material: stirring under 50rpm speed conditions, surface is modified
Graphene oxide solution is slowly added into SiO dispersion liquid, then heating stirring 3min, is staticly settled, filters pressing separation, and vacuum is dry
It is dry, obtain the SiO composite material of graphene oxide cladding.
(4) preparation of graphene coated SiO composite material: under vacuum conditions, with 20 DEG C/min heating rate by temperature
It heats 200 DEG C of reduction 0.5h and obtains graphene coated SiO composite material.
Wherein the mesh number of natural flake graphite is 32 mesh, and the concentration of graphene oxide solution is 10mg/mL, graphene oxide
Mass ratio with surfactant is 10:1, and surfactant is citric acid (CA), and the size of SiO powder is 100 μm, You Jirong
Agent is dehydrated alcohol, and the concentration of SiO powder in organic solvent is 20mg/mL, and the mass ratio of SiO and graphene oxide is 100:
1, the addition rate of the modified graphene oxide solution in surface is 10mL/min, and heating temperature is 20 DEG C.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 30%, and cycle performance improves 50%.
Embodiment 2:
The mesh number of natural flake graphite is 500 mesh, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 21%, and cycle performance improves 30%.
Embodiment 3:
The concentration of graphene oxide solution is 5mg/mL, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 26%, and cycle performance improves 38%.
Embodiment 4:
The mass ratio of graphene oxide and surfactant is 5: 1, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 28%, and cycle performance improves 54%.
Embodiment 5:
Surfactant is sodium citrate (SC), and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 25%, and cycle performance improves 43%.
Embodiment 6:
The size of SiO powder is 500nm, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 18%, and cycle performance improves 29%.
Embodiment 7:
Organic solvent is acetone, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 26%, and cycle performance improves 41%.
Embodiment 8:
The concentration of SiO powder in organic solvent is 2mg/mL, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 32%, and cycle performance improves 57%.
Embodiment 9:
The mass ratio of SiO and graphene oxide is 10: 1, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 35%, and cycle performance improves 57%.
Embodiment 10:
The addition rate of the modified graphene oxide solution in surface is 5mL/min, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 15%, and cycle performance improves 28%.
Embodiment 11:
Heating temperature is 70 DEG C, and other processes are the same as embodiment 1.
The graphene coated SiO composite material of preparation and the SiO material of not graphene coated are fabricated to electrode slice, so
After be assembled into button cell carry out electrochemical property test.Compared with no graphene coated SiO material, in same test condition
Under, capacity improves 23%, and cycle performance improves 44%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials, which is characterized in that include following step
It is rapid:
1) it the preparation of the modified graphene oxide solution in surface: uses natural flake graphite for raw material, passes through modified Hummers
Method prepares graphite oxide, and centrifugation washing obtains graphene oxide slurry, by graphene oxide slurry ultrasonic disperse into water, centrifugation
It removes unstripped graphite and obtains graphene oxide solution, surfactant, ultrasonic disperse are added in graphene oxide solution
Uniformly, the modified graphene oxide solution in surface is obtained；
2) preparation of SiO dispersion liquid: SiO powder is added in organic solvent, is dispersed by stirring to get finely dispersed SiO
Liquid；
3) preparation of graphene oxide coated Si O composite material: under agitation, by the modified graphene oxide solution in surface
It is slowly added into SiO dispersion liquid, then heating stirring, staticly settles, filters pressing separation, vacuum drying obtains graphene oxide
The SiO composite material of cladding；
4) preparation of graphene coated SiO composite material: high temperature reduction obtains graphene under conditions of protective gas or vacuum
Coated Si O composite material.
2. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
When being distributed to graphene oxide slurry in water in step 1), the volume ratio of graphene oxide slurry and water is 1: 2~1:
12, ultrasonic power be 80~1000W, the time be 3~60min, centrifugal rotational speed be 1000~12000rpm, the time be 2~
30min, the concentration of graphene oxide solution are 0.5~10mg/mL.
3. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
It is 1000~15000rpm that centrifugal rotational speed when obtaining graphene oxide slurry is washed in centrifugation in step 1), and centrifugation time is
2~30min.
4. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
The mass ratio of graphene oxide and surfactant is 10: 1~2: 1 in step 1), and surfactant is detergent alkylate
One or more of sodium sulfonate, dodecyl sodium sulfate, kayexalate, sodium citrate, citric acid, ultrasonic power
For 80~1000W, the time is 3~60min.
5. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
The size of SiO powder is 50nm~100 μm in step (2), and organic solvent is methanol, dehydrated alcohol, isopropanol, second two
One of alcohol, acetone, pyruvic alcohol, the concentration of SiO powder in organic solvent be 0.5~20mg/mL, speed of agitator be 50~
1000rpm, time are 3~60min.
6. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
Speed of agitator is 50~1000rpm in step (3), and the mass ratio of SiO and graphene oxide is 100: 1~3: 1, and surface changes
Property graphene oxide solution addition rate be 0.1~10mL/min, heating temperature be 20~70 DEG C, mixing time be 3~
60min。
7. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
Step (4) high temperature reduction temperature be 200~2000 DEG C, the time be 0.5~10h, heating rate be 1~20 DEG C/
Min, protective gas are nitrogen or argon gas.
8. a kind of preparation method that graphene may be implemented and closely coat SiO negative materials as described in claim 1, feature
It is:
The mesh number of natural flake graphite is 32~1000 mesh in step (1).
9. the graphene coated SiO negative materials being prepared such as the method for any one of claim 1-8.
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| CN111916705A (en) * | 2020-08-05 | 2020-11-10 | 西北师范大学 | Preparation and application of high-performance silicon oxide-based composite material |
| CN114927747A (en) * | 2022-05-26 | 2022-08-19 | 安徽力源新能源有限公司 | High-rate discharge graphene manganese-rich lithium ion battery for fire emergency first aid |
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