CN107946556A - A kind of preparation method of graphene-based Si-C composite material - Google Patents
A kind of preparation method of graphene-based Si-C composite material Download PDFInfo
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- CN107946556A CN107946556A CN201711064440.3A CN201711064440A CN107946556A CN 107946556 A CN107946556 A CN 107946556A CN 201711064440 A CN201711064440 A CN 201711064440A CN 107946556 A CN107946556 A CN 107946556A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 27
- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 30
- 239000010439 graphite Substances 0.000 claims abstract description 30
- -1 graphite alkene Chemical class 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 16
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 16
- 238000002604 ultrasonography Methods 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract description 10
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004005 microsphere Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 9
- 229910001416 lithium ion Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 239000002023 wood Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 239000010703 silicon Substances 0.000 abstract description 7
- 230000004087 circulation Effects 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 238000001694 spray drying Methods 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011806 microball Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
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- Battery Electrode And Active Subsutance (AREA)
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Abstract
The present invention relates to a kind of preparation method of graphene-based Si-C composite material, is 12 first by mass ratio:1 graphene oxide and maleate is distributed in water, and stirring, spray drying, become powdered, high-temperature process, obtain spherical graphite alkene microballoon；Nano-silicon, spherical graphite alkene microballoon are disperseed in a solvent, by ultrasound, stirring, uniformly rear removing solvent to be mixed, high-temperature process, obtains nano-silicon/spherical graphite alkene microsphere compound under an inert gas；Compound and organic carbon source are disperseed in a solvent again, by ultrasound, stirring, uniformly rear removing solvent to be mixed, high-temperature process, obtains graphene-based Si-C composite material under an inert gas.Present invention has the advantages that：Spherical graphite alkene microballoon high degree of dispersion, maleate, silicon and carbon are evenly distributed, and discharge capacity is up to more than 750 first, and coulombic efficiency is up to discharge and recharge under more than 92%, 0.1C first, capacity retention ratio more than 85% after 500 circulations.
Description
Technical field
The present invention relates to the preparation method of graphene-based Si-C composite material, belongs to lithium ion battery negative material and prepares skill
Art field.
Background technology
With the demand of production and the raising of environmental protection consciousness, new energy become various countries fall over each other development emphasis, lithium from
Sub- battery is big with it is bigger than energy, operating voltage is high, self-discharge rate is small, the advantage such as small, light-weight occupies 3C fields already
Market segment.
Current commercialized lithium ion battery negative material is mainly graphite, but theoretical capacity is only 372mAh/g, by
Cannot gradually meet the needs of market is to high-energy-density.
Silicon have superelevation theoretical specific capacity (4200mAh/g) and relatively low embedding de- lithium current potential (<0.5V), and silicon voltage
Platform is slightly above graphite, and more difficult in charging to cause surface to analyse lithium, security performance is more preferable.Silicon is as lithium ion battery negative material
When shortcoming also clearly.First, silicon is semi-conducting material, and the electrical conductivity of itself is relatively low；Secondly, in electrochemistry cyclic process
In, the insertion and abjection of lithium ion can make the expansion and contraction of silica-base material volume generation more than 300%, resulting machinery
Active force can make the gradual dusting of silica-base material, cause structure collapses, ultimately result in electrode active material and depart from collector, lose
Electrical contact, so that the cycle performance of lithium ion battery substantially reduces.
The content of the invention
In order to solve the technical problem that graphite theoretical capacity in the prior art is low, silicon removal lithium embedded causes structure collapses, this hair
Bright purpose is to provide a kind of preparation method of graphene-based Si-C composite material.
The technical scheme is that：
A kind of preparation method of graphene-based Si-C composite material, is 1-2 first by mass ratio:1 graphene oxide and
Maleate is distributed in water, is obtained dispersion liquid after stirring 2h at 70-90 DEG C, is then spray-dried at 150-200 DEG C, makes it
As powdered, after 220-250 DEG C of processing 5h, then after 300-350 DEG C handles 5h, 450-500 DEG C of processing 5h, then in 750-
800 DEG C of processing 5h, obtain spherical graphite alkene microballoon；By nano-silicon, spherical graphite alkene microballoon disperse in a solvent, by ultrasound,
Stirring, uniformly rear removing solvent to be mixed, keeps 10-20min, 200-300 DEG C of holding 20- for 50-100 DEG C under an inert gas
30min, 700-800 DEG C of holding 5-6h, obtain nano-silicon/spherical graphite alkene microsphere compound；Again by compound and organic carbon source
Disperse in a solvent, by ultrasound, to stir, uniformly rear removing solvent to be mixed, under an inert gas 50-100 DEG C of holding 10-
20min, 200-300 DEG C of holding 20-30min, 700-800 DEG C of holding 5-6h, 850-900 DEG C of holding 8-10h, obtains graphene-based
Si-C composite material.
Preferably：It is 1.5 first by mass ratio:1 graphene oxide and maleate is distributed in water, is stirred at 80 DEG C
Obtain dispersion liquid after mixing 2h, be then spray-dried at 180 DEG C, become it is powdered, after 240 DEG C of processing 5h, then at 320 DEG C
After handling 5h, 480 DEG C of processing 5h, then 5h is handled at 780 DEG C, obtain spherical graphite alkene microballoon；Nano-silicon, spherical graphite alkene is micro-
Ball disperses in a solvent, by ultrasound, to stir, uniformly rear removing solvent to be mixed, under an inert gas 80 DEG C of holding 10-
20min, 260 DEG C of holding 20-30min, 780 DEG C of holding 5-6h, obtain nano-silicon/spherical graphite alkene microsphere compound；Again will be multiple
Compound and organic carbon source disperse in a solvent, by ultrasound, stirring, it is to be mixed uniformly after remove solvent, under an inert gas 80
DEG C keep 10-20min, 260 DEG C holding 20-30min, 780 DEG C holding 5-6h, 880 DEG C holding 8-10h, obtain graphene-based silicon
Carbon composite.
The present invention also provides a kind of graphene-based Si-C composite material, prepared using the above method.
The present invention also provides a kind of lithium ion battery negative material, using above-mentioned graphene-based Si-C composite material.
The present invention also provides a kind of lithium ion battery, using above-mentioned negative material.
Present invention has the advantages that：Spherical graphite alkene microballoon high degree of dispersion, maleate, silicon and carbon are evenly distributed, first
Discharge capacity is up to more than 750, and coulombic efficiency is up to discharge and recharge under more than 92%, 0.1C first, capacity retention ratio after 500 circulations
More than 85%.
Embodiment
Technical scheme is described in detail below.
Embodiment 1
It is 1 first by mass ratio:1 graphene oxide and maleate is distributed in water, is obtained after stirring 2h at 70 DEG C
Dispersion liquid, is then spray-dried at 150 DEG C, become it is powdered, 220 DEG C processing 5h after, then 300 DEG C handle 5h after,
450 DEG C of processing 5h, then 5h is handled at 750 DEG C, obtain spherical graphite alkene microballoon；Nano-silicon, spherical graphite alkene microballoon are dispersed in
In solvent, by ultrasound, stir, uniformly rear removing solvent to be mixed, under an inert gas 50 DEG C of holding 10min, 200 DEG C keep
20min, 800 DEG C of holding 6h, obtains nano-silicon/spherical graphite alkene microsphere compound；Compound and organic carbon source are dispersed in again
In solvent, by ultrasound, stir, uniformly rear removing solvent to be mixed, under an inert gas 100 DEG C of holding 20min, 300 DEG C are protected
20min is held, 800 DEG C of holding 5h, 850 DEG C of holding 8h, obtain graphene-based Si-C composite material.
Embodiment 2
It is 1.5 first by mass ratio:1 graphene oxide and maleate is distributed in water, is obtained after stirring 2h at 80 DEG C
To dispersion liquid, be then spray-dried at 180 DEG C, become it is powdered, 240 DEG C processing 5h after, then 320 DEG C handle 5h
Afterwards, 480 DEG C of processing 5h, then 5h is handled at 780 DEG C, obtain spherical graphite alkene microballoon；Nano-silicon, spherical graphite alkene microballoon are disperseed
In a solvent, by ultrasound, stirring, it is to be mixed uniformly after remove solvent, under an inert gas 80 DEG C holding 10-20min, 260
DEG C keep 20-30min, 780 DEG C holding 5-6h, obtain nano-silicon/spherical graphite alkene microsphere compound；Again by compound with it is organic
Carbon source disperses in a solvent, by ultrasound, to stir, uniformly rear removing solvent to be mixed, under an inert gas 80 DEG C of holding 10-
20min, 260 DEG C of holding 20-30min, 780 DEG C of holding 5-6h, 880 DEG C of holding 8-10h, obtain graphene-based silicon-carbon composite wood
Material.
Embodiment 3
It is 2 first by mass ratio:1 graphene oxide and maleate is distributed in water, is obtained after stirring 2h at 90 DEG C
Dispersion liquid, is then spray-dried at 200 DEG C, become it is powdered, 250 DEG C processing 5h after, then 350 DEG C handle 5h after,
500 DEG C of processing 5h, then 5h is handled at 800 DEG C, obtain spherical graphite alkene microballoon；Nano-silicon, spherical graphite alkene microballoon are dispersed in
In solvent, by ultrasound, stir, uniformly rear removing solvent to be mixed, under an inert gas 50 DEG C of holding 20min, 200 DEG C keep
30min, 800 DEG C of holding 6h, obtains nano-silicon/spherical graphite alkene microsphere compound；Compound and organic carbon source are dispersed in again
In solvent, by ultrasound, stirring, uniformly rear removing solvent to be mixed, keeps 20min, 200-300 for 100 DEG C under an inert gas
DEG C keep 20min, 700 DEG C holding 5h, 850 DEG C holding 8h, obtain graphene-based Si-C composite material.
Material prepared by Example 1~3 is as negative material, and binding agent (LA132), conductive agent (Super-P) and
Dispersant (water and ethanol, volume ratio position 1：3) it is tuned into slurry, coated on copper foil, and vacuum dried, roll-in, it is prepared into negative
Pole piece；Cathode uses metal lithium sheet, and the organic electrolyte used is 1MLiPF6/EC+PC+DEC (molar ratios 1：1：1), membrane
For polypropylene, CR2025 type button cells are made.Test condition is room temperature, and discharge and recharge under 0.1C, charging/discharging voltage is limited to
0.005~1.5V.
1 half-cell test performance of table
Claims (5)
- A kind of 1. preparation method of graphene-based Si-C composite material, it is characterised in that：It is 1-2 first by mass ratio:1 oxidation Graphene and maleate are distributed in water, are obtained dispersion liquid after stirring 2h at 70-90 DEG C, are then sprayed at 150-200 DEG C It is dry, become it is powdered, after 220-250 DEG C of processing 5h, then after 300-350 DEG C handles 5h, 450-500 DEG C of processing 5h, 5h is handled at 750-800 DEG C again, obtains spherical graphite alkene microballoon；Nano-silicon, spherical graphite alkene microballoon are disperseed in a solvent, warp Ultrasonic, stirring is crossed, uniformly rear removing solvent to be mixed, keeps 10-20min, 200-300 DEG C of guarantor for 50-100 DEG C under an inert gas 20-30min is held, 700-800 DEG C of holding 5-6h, obtains nano-silicon/spherical graphite alkene microsphere compound；Again by compound with it is organic Carbon source is disperseed in a solvent, by ultrasound, stirring, uniformly rear removing solvent to be mixed, and 50-100 DEG C of holding under an inert gas 10-20min, 200-300 DEG C of holding 20-30min, 700-800 DEG C of holding 5-6h, 850-900 DEG C of holding 8-10h, obtains graphite Alkenyl Si-C composite material.
- A kind of 2. preparation method of graphene-based Si-C composite material as claimed in claim 1, it is characterised in that：First by quality Than for 1.5:1 graphene oxide and maleate is distributed in water, dispersion liquid is obtained after stirring 2h at 80 DEG C, then 180 Be spray-dried at DEG C, become it is powdered, 240 DEG C processing 5h after, then 320 DEG C handle 5h after, 480 DEG C processing 5h, then 780 DEG C of processing 5h, obtain spherical graphite alkene microballoon；By nano-silicon, spherical graphite alkene microballoon disperse in a solvent, by ultrasound, Stirring, it is to be mixed uniformly after remove solvent, under an inert gas 80 DEG C holding 10-20min, 260 DEG C holding 20-30min, 780 DEG C keep 5-6h, obtain nano-silicon/spherical graphite alkene microsphere compound；Compound and organic carbon source are disperseed in a solvent again, By ultrasound, stir, uniformly rear removing solvent to be mixed, under an inert gas 80 DEG C of holding 10-20min, 260 DEG C keep 20- 30min, 780 DEG C of holding 5-6h, 880 DEG C of holding 8-10h, obtain graphene-based Si-C composite material.
- A kind of 3. graphene-based Si-C composite material, it is characterised in that：Prepared using method as claimed in claim 1 or 2.
- A kind of 4. lithium ion battery negative material, it is characterised in that：Using graphene-based silicon-carbon composite wood as claimed in claim 3 Material.
- A kind of 5. lithium ion battery, it is characterised in that：Using negative material as claimed in claim 4.
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| CN201711064440.3A CN107946556B (en) | 2017-11-02 | 2017-11-02 | Preparation method of graphene-based silicon-carbon composite material |
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| CN201711064440.3A CN107946556B (en) | 2017-11-02 | 2017-11-02 | Preparation method of graphene-based silicon-carbon composite material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102306757A (en) * | 2011-08-26 | 2012-01-04 | 上海交通大学 | Silicon graphene composite anode material of lithium ion battery and preparation method of silicon graphene composite anode material |
| CN104591177A (en) * | 2015-02-03 | 2015-05-06 | 辽宁工程技术大学 | Method for preparing self-supporting three-dimensional porous graphene composite microsphere |
| CN105304884A (en) * | 2015-05-18 | 2016-02-03 | 深圳市国创新能源研究院 | Graphene-based silicon-carbon composite anode material and preparation method thereof |
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2017
- 2017-11-02 CN CN201711064440.3A patent/CN107946556B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102306757A (en) * | 2011-08-26 | 2012-01-04 | 上海交通大学 | Silicon graphene composite anode material of lithium ion battery and preparation method of silicon graphene composite anode material |
| CN104591177A (en) * | 2015-02-03 | 2015-05-06 | 辽宁工程技术大学 | Method for preparing self-supporting three-dimensional porous graphene composite microsphere |
| CN105304884A (en) * | 2015-05-18 | 2016-02-03 | 深圳市国创新能源研究院 | Graphene-based silicon-carbon composite anode material and preparation method thereof |
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