CN105869903A - Preparation method of graphene - Google Patents
Preparation method of graphene Download PDFInfo
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- CN105869903A CN105869903A CN201610354181.7A CN201610354181A CN105869903A CN 105869903 A CN105869903 A CN 105869903A CN 201610354181 A CN201610354181 A CN 201610354181A CN 105869903 A CN105869903 A CN 105869903A
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- graphene
- preparation
- graphene oxide
- emulsion
- oil phase
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a preparation method of graphene. A graphene oxide emulsion is obtained by mixing graphene oxide and an oil phase, and self-assembly of graphene oxide sheet layers on an emulsion interface is realized; besides, a hollow and porous graphene ball structure is prepared with a hydrothermal method by means of the characteristic that citric acid can generate gas after being hydrolyzed at high temperature, the structure facilitates diffusion and transmission of electrolyte ions, a ball-shaped structure serves as a conductive network, and agglomeration and stacking of the graphene sheet layers are inhibited; an inner-crosslinking ball-shaped structure is established to serve as the conductive network, transmission of electrons is facilitated, interface resistance is effectively reduced, the specific capacity and the multiplying power of a supercapacitor are increased, and the cycle performance of the supercapacitor is improved. The graphene is simple in structure, has a high specific surface area and high conductivity and can be applied to the supercapacitor. The preparation method is simple in process, the reaction process is easy to control, a little equipment investment is required, the graphene does not need to be prepared under a vacuum high-pressure condition, and large-scale production can be realized.
Description
Technical field
The present invention relates to a kind of ultracapacitor Graphene, specifically, relate to a kind of ultracapacitor with having
Hollow, the preparation method of loose structure Graphene ball.
Background technology
Ultracapacitor have high power density, can fast charging and discharging, million rank long circulation lifes and safety
The characteristic such as reliable, has broad application prospects in fields such as track traffic, national defence and Aero-Space.But,
The relatively low shortcoming of super capacitor energy density governs that it is fast-developing, commercial activated carbon super capacitor energy
Density only 5～7Wh kg-1.Therefore, in order to meet ultracapacitor increasing need, develop light
And the ultracapacitor with high-energy-density, power density and good circulation stability is sending out of new energy field
One of exhibition trend.
Graphene is the two dimensional crystal being made up of one layer of carbon atom peeled off through graphite, and it has carbon hexatomic ring
The two-dimension periodic honeycomb lattice structure of composition, is to build other dimension carbonaceous material (fowler such as zero dimension
Alkene, one-dimensional CNT and three-dimensional graphite) elementary cell.Unique two-dimensional structure of Graphene and complete
Beautiful crystal structure makes it have high conductivity, high mechanical properties, high-termal conductivity and peculiar optical property,
The information apparatus such as transistor it are widely used in.At nano composite material, battery and super capacitor etc.
Field, the assembling form between two dimensional surface graphene layer is particularly important.At present, porous graphene not only has
There are the merit of Graphene, simultaneously its high-specific surface area having, excellent electrical conductivity and abundant hole knot
The features such as structure, also become the ideal electrode material of ultracapacitor.
At present, the Graphene using existing oxidation-reduction method to prepare due to π-π effect, Van der Waals force and is dredged
Aqueous, easily occur to reunite and stacking phenomenon, not only inhibit the infiltration of electrolyte and ion to spread, and significantly
Reduce the specific surface area of material.
Accordingly, it is desirable to provide a kind of improvement technical scheme not enough for above-mentioned prior art.
Summary of the invention
It is an object of the invention to for the problems referred to above, propose a kind of ultracapacitor with having hollow, loose structure
The preparation method of Graphene ball.The Graphene that the present invention obtains cross-links spherical knot in having hollow, porous graphene
The diffusion of structure, beneficially electrolyte ion and transmission, improve the transmission of electronics, significantly reduce interface resistance,
Improve the specific capacity of ultracapacitor, multiplying power and cycle performance.
For achieving the above object, the present invention is by the following technical solutions:
A kind of Graphene and CNT are combined macroscopic body, have loose structure.
A kind of graphene preparation method, said method comprising the steps of:
1) graphene oxide emulsion is prepared: after graphene oxide solution being mixed in proportion with citric acid, ultrasonic
Process 0.5～2h；Add oil phase, stirring, obtain graphene oxide emulsion；
2) prepare presoma: by step 1 at 180～200 DEG C) emulsion heating 0.5～5h, obtain presoma；
3) prepare Graphene: by step 2) in presoma freeze-drying after；In inert atmosphere, 650～1000 DEG C
Under, react 1～5h；Washing, dries, obtains goods.
Further, step 1) described in the concentration of graphene oxide be 0.1～5mg mL-1.
Further, step 1) described in oil phase be methyl methacrylate, EMA, methyl
One or more compositions in n-propyl, n-BMA and isopropyl methacrylate.
Further, step 1) described in graphene oxide and the mass ratio 1:(0.1～5 of citric acid).
Further, step 1) described in the volume ratio of graphene oxide and oil phase be 1:(0.05～5).
Further, the volume ratio of described graphene oxide and oil phase is 1:0.2.
Further, step 1) in mixing time be 5～20min.
Further, step 3) in nitrogen, at 800 DEG C, react 2h.
Further, step 3) in gained Graphene be hollow, porous spherical structure.
Further, the graphene oxide that the present invention uses is from crystalline flake graphite, uses Hummer
Method prepares.
Further, the Graphene that the present invention provides is mainly from graphene oxide；Due to graphene oxide
Surface is contained substantial amounts of oxygen-containing functional group and is had good hydrophilic interaction, and research simultaneously finds that Graphene bunch has one
Fixed hydrophobicity, the performance of such graphene oxide is close to an amphiphilic block copolymer.
Further, the present invention mixes to obtain graphene oxide emulsion by graphene oxide with oil phase, it is achieved oxygen
Functionalized graphene lamella, in the self assembly of emulsion interface, utilizes citric acid pyrohydrolysis to produce the characteristic of gas simultaneously,
Hydro-thermal method prepares hollow, porous graphene ball, and high annealing further, improves the electric conductivity of material.
Further, the Graphene application for ultracapacitor of gained is prepared.
Compared with immediate prior art, the technical scheme that the present invention provides has a following excellent effect:
1, the technical scheme that the present invention provides uses graphene oxide to mix to obtain graphene oxide emulsion with oil phase,
Achieve the self assembly at emulsion interface of the graphene oxide lamella, utilize citric acid pyrohydrolysis to produce gas simultaneously
Characteristic, hydro-thermal method prepares hollow, porous graphene ball, and high annealing further, improves leading of material
Electrically.
2, the technical scheme that the present invention provides builds hollow, loose structure are conducive to the diffusion of electrolyte ion
With transmission, Graphene chondritic is as conductive network, it is suppressed that the reunion of graphene sheet layer and stacking, simultaneously
In building, crosslinking chondritic is beneficial to the transmission of electronics as conductive network, effectively reduces interface resistance, simultaneously
Improve the specific capacity of ultracapacitor, multiplying power and cycle performance.
3, the graphene-structured that the present invention prepares is stable, has high-specific surface area, high conductivity, can apply
In ultracapacitor.
4, the preparation method technique of the present invention is simple, and course of reaction is easily controlled, and equipment investment is few, is not required to
To carry out under the conditions of vacuum high-pressure, large-scale production can be realized.
Accompanying drawing explanation
For the technical scheme being illustrated more clearly that in the present invention, below by embodiment required use attached
Figure is briefly described, it should be apparent that, the accompanying drawing in describing below is only some embodiments of the present invention,
For those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to according to these
Accompanying drawing obtains other accompanying drawing.
Fig. 1 is the Graphene scanning electron micrograph of embodiment 1 preparation；
Fig. 2 is the Graphene of embodiment 1 preparation cyclic voltammetry curve under 25mV s-1 sweeps speed；
Fig. 3 is the Graphene of embodiment 1 preparation constant current charge-discharge curve under 1A g-1 current density.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described
Embodiment be only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained, broadly fall into the model of present invention protection
Enclose.
Embodiment 1
Taking 100ml concentration is 3mg mL-1 graphene oxide water solution, adds 100mg citric acid, ultrasonic
Process 1h；According to graphene solution with oil phase volume than 1:0.2, methylate methyl acrylate, mixing time
For 20min, prepare graphene oxide emulsion；At 180 DEG C, emulsion is heated 3h, obtain presoma；Will
Presoma is freeze-dried, the most in a nitrogen environment, at 800 DEG C, reacts 2h；Take product spend from
Sub-water cleans repeatedly, dries, obtains grapheme material.
Graphene prepared by the present embodiment is scanned Electronic Speculum detection (SEM), as shown in Figure 1, it is known that graphite
Alkene is porous, interior crosslinking chondritic, beneficially electrolyte diffusion and transmission, simultaneously crosslinking layer structure in this
The transmission of electronics is conducive to as conductive network.
Weigh Graphene, 10mg conductive agent Super P and 10mg bonding prepared by 80mg the present embodiment respectively
Agent PVDF, puts in agate mortar and grinds, and drips 1-METHYLPYRROLIDONE NMP, is ground to muddy,
It is coated uniformly in nickel foam, in 120 DEG C of dry 4h, is pressed into pole piece, each pole piece with the pressure of 10MPa
Active material load capacity be 3～5mg；Take out the equal pole piece of two tablet qualities as ultracapacitor both positive and negative polarity,
With ionic liquid as electrolyte, glass fibre membrane is barrier film, is assembled into CR2032 button cell, tests electrode
The chemical property of material；Graphene electrodes material prepared by the present embodiment circulation volt under 25mV/s sweeps speed
Peace curve, as in figure 2 it is shown, this material shows preferable electric double layer capacitance characteristic as can be known from Fig. 2.Carry out again
Constant current charge-discharge is tested, as shown in Figure 3, it is known that the specific volume that this Graphene has under the current density of 1A/g
Amount reaches 150F/g.
Embodiment 2
Taking 100ml concentration is 0.5mg mL-1 graphene oxide water solution, adds 50mg citric acid, ultrasonic
Process 1.5h；According to graphene solution with oil phase volume than 1:0.5, methylate ethyl acrylate, mixing time
For 15min, prepare graphene oxide emulsion；At 190 DEG C, emulsion is heated 1h, obtain presoma；Will
Presoma is freeze-dried, the most in a nitrogen environment, at 900 DEG C, reacts 3h；Take product spend from
Sub-water cleans repeatedly, dries, obtains grapheme material.
Embodiment 3
Taking 100ml concentration is 4mg mL-1 graphene oxide water solution, adds 200mg citric acid, ultrasonic
Process 0.5h；According to graphene solution with oil phase volume than 1:2, methylate methyl acrylate, mixing time
For 5min, prepare graphene oxide emulsion；At 200 DEG C, emulsion is heated 0.5h, obtain presoma；Will
Presoma is freeze-dried, the most in a nitrogen environment, at 1000 DEG C, reacts 1h；Take product to use
Deionized water is cleaned repeatedly, dries, obtains grapheme material.
Embodiment 4
Taking 100ml concentration is 2mg mL-1 graphene oxide water solution, adds 200mg citric acid, ultrasonic
Process 1.5h；According to graphene solution with oil phase volume than 1:3, methylate n-butyl acrylate, during stirring
Between be 10min, prepare graphene oxide emulsion；At 185 DEG C, emulsion is heated 2h, obtain presoma；
Presoma is freeze-dried, the most in a nitrogen environment, at 700 DEG C, react 3h；Take product to spend
Ionized water cleans repeatedly, dries, obtains grapheme material.
Embodiment 5
Taking 100ml concentration is 1mg mL-1 graphene oxide water solution, adds 300mg citric acid, ultrasonic place
Reason 2h；According to graphene solution with oil phase volume than 1:3.5, methylate n-propyl, mixing time
For 15min, prepare graphene oxide emulsion；At 195 DEG C, emulsion is heated 4h, obtain presoma；Will
Presoma is freeze-dried, the most in a nitrogen environment, at 850 DEG C, reacts 3h；Take product spend from
Sub-water cleans repeatedly, dries, obtains grapheme material.
Embodiment 6
Taking 100ml concentration is 0.1mg mL-1 graphene oxide water solution, adds 50mg citric acid, ultrasonic
Process 1h；According to graphene solution with oil phase volume than 1:0.1, methylate isopropyl acrylate, during stirring
Between be 8min, prepare graphene oxide emulsion；At 195 DEG C, emulsion is heated 1h, obtain presoma；
Presoma is freeze-dried, the most in a nitrogen environment, at 900 DEG C, react 3.5h；Take product to use
Deionized water is cleaned repeatedly, dries, obtains grapheme material.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, all await the reply right in the present invention
Within the scope of Yao Qiubaohu.
Claims (10)
1. a graphene preparation method, it is characterised in that said method comprising the steps of:
1) graphene oxide emulsion is prepared: the ultrasonically treated mixture prepared in proportion by graphene oxide solution and citric acid
After 0.5～2h；Add oil phase mix and blend, prepare to obtain emulsion；
2) prepare presoma: heating steps 1 at 180～200 DEG C) emulsion 0.5～5h, obtain presoma；
3) prepare Graphene: by step 2) presoma freeze-drying after；React in inert atmosphere, at 650～1000 DEG C
1～5h；Washing, dries, obtains goods.
2. preparation method as claimed in claim 1, it is characterised in that step 1) described in the concentration of graphene oxide be 0.1～5
mg mL-1。
3. preparation method as claimed in claim 1, it is characterised in that step 1) described in oil phase be methyl methacrylate,
One or many in EMA, n propyl methacrylate, n-BMA and isopropyl methacrylate
Plant composition.
4. preparation method as claimed in claim 1, it is characterised in that step 1) described in graphene oxide and citric acid
Mass ratio 1:(0.1～5).
5. preparation method as claimed in claim 1, it is characterised in that step 1) described in graphene oxide and the body of oil phase
Long-pending ratio is 1:(0.05～5).
6. preparation method as claimed in claim 5, it is characterised in that the volume ratio of described graphene oxide and oil phase is 1:
0.2。
7. preparation method as claimed in claim 1, it is characterised in that step 1) in mixing time be 5～20min.
8. preparation method as claimed in claim 1, it is characterised in that step 3) in nitrogen, at 800 DEG C, react 2h.
9. preparation method as claimed in claim 1, it is characterised in that step 3) in gained Graphene be hollow, porous ball
Shape structure.
10. the Graphene described in a claim 1 is for preparing the application of ultracapacitor.
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Cited By (4)
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| CN106449129A (en) * | 2016-09-29 | 2017-02-22 | 成都新柯力化工科技有限公司 | Graphene self-assembled electrode material for super-capacitor and preparation method |
| CN107082420A (en) * | 2017-04-27 | 2017-08-22 | 中国科学院宁波材料技术与工程研究所 | The preparation method and ultracapacitor of a kind of graphene powder |
| CN107942572A (en) * | 2017-11-17 | 2018-04-20 | 深圳市华星光电技术有限公司 | A kind of preparation method of color membrane substrates and black-matrix material |
| CN115180616A (en) * | 2022-08-11 | 2022-10-14 | 深圳一个烯材科技有限公司 | Nano-porous graphene material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106449129A (en) * | 2016-09-29 | 2017-02-22 | 成都新柯力化工科技有限公司 | Graphene self-assembled electrode material for super-capacitor and preparation method |
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| CN107942572A (en) * | 2017-11-17 | 2018-04-20 | 深圳市华星光电技术有限公司 | A kind of preparation method of color membrane substrates and black-matrix material |
| CN107942572B (en) * | 2017-11-17 | 2020-12-04 | 深圳市华星光电技术有限公司 | Color film substrate and preparation method of black matrix material |
| CN115180616A (en) * | 2022-08-11 | 2022-10-14 | 深圳一个烯材科技有限公司 | Nano-porous graphene material |
| CN115180616B (en) * | 2022-08-11 | 2023-04-11 | 深圳一个烯材科技有限公司 | Nano-porous graphene material |
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