CN105321724A - Three-dimensional porous graphene, preparation method and application therefor - Google Patents
Three-dimensional porous graphene, preparation method and application therefor Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 108
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 229920002635 polyurethane Polymers 0.000 claims abstract description 36
- 239000004814 polyurethane Substances 0.000 claims abstract description 36
- 239000006185 dispersion Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 239000007772 electrode material Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 52
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- 239000003990 capacitor Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000005486 organic electrolyte Substances 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 238000010792 warming Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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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
- Y02E60/13—Energy storage using capacitors
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- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
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- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention provides a preparation method for three-dimensional porous graphene. The preparation method comprises the following steps: (A), mixing graphene oxide, an alkali substance and water to obtain a composite dispersion liquid; and (B), immersing a polyurethane sponge into the composite dispersion liquid, taking out the immersed polyurethane sponge and drying, then calcining the dried polyurethane sponge to obtain the three-dimensional porous graphene. The invention further provides an application of the prepared three-dimensional porous graphene as an electrode material. The prepared three-dimensional porous graphene has the advantages of high porosity and large specific surface area, so that the three-dimensional porous graphene is excellent in the electrochemical performance when the three-dimensional porous graphene is used as the electrode material; and the three-dimensional porous graphene is suitable for preparing high energy density supercapacitors having a relatively high demand on the electrode volume.
Description
Technical field
The present invention relates to electrode material technical field, particularly relate to a kind of three-dimensional porous Graphene, its preparation method and application thereof.
Background technology
Ultracapacitor is a kind of novel energy-storing original paper, due to its have that charge/discharge rates is fast, power density is high, the life-span is long, the feature such as non-maintaining and environmental friendliness, be subject to the extensive concern of domestic and international scientist.The character of electrode material is the key factor affecting ultracapacitor performance.The capacitance and the energy density that how to improve capacitor are the emphasis that people study, and therefore exploitation has the key problem that the electrode material of excellent properties is ultracapacitor research.
The excellent electrode material of ultracapacitor had both required high conductivity, also required high charge storage.Metal oxide and conducting polymer are that the Faraday pseudo-capacitance electrode material of representative has the outstanding capacitive property deriving from surface electrochemistry reaction, but its conductivity is relatively poor, and portion of material is with high costs, cyclical stability is not high yet, and above-mentioned factor seriously constrains metal oxide and conducting polymer applying in ultracapacitor.Current widely used super capacitor material is mainly concentrated on the carbon material.Material with carbon element has good conductivity, stability, with low cost and good charge adsorption energy.
Graphene has high-specific surface area and excellent conductivity in theory, is therefore considered to a kind of desirable material with carbon element that can be applicable to electrode of super capacitor.But make it again stacking due to the Van der Waals force after reduction between graphene sheet layer, or it is complete not to dissociate, and is unfavorable for its capacitive property; Meanwhile, ultracapacitor, except requiring electrode material and having huge specific area and good conductivity, also has requirement to its pore-size distribution.
The feature of polyurethane sponge has continuous poriferous structure, has acid-alkali-corrosive-resisting, and pore is even, and can cut into the advantage of arbitrary shape size.Thus, this application provides a kind of preparation method of three-dimensional porous Graphene.
Summary of the invention
The technical problem that the present invention solves is the preparation method providing a kind of three-dimensional porous Graphene, and three-dimensional porous Graphene prepared by the application has excellent chemical property as the electrode material of ultracapacitor.
In view of this, this application provides a kind of preparation method of three-dimensional porous Graphene, comprise the following steps:
A), graphene oxide, alkaline matter are mixed with water, obtains composite dispersion liquid;
B), polyurethane sponge is immersed in described composite dispersion liquid, dry after the polyurethane sponge obtained is taken out, then calcine, obtain three-dimensional porous Graphene.
Preferably, described alkaline matter is selected from one or both in potassium hydroxide and NaOH.
Preferably, in described composite dispersion liquid, the concentration of described graphene oxide is 0.1 ~ 10 mg/ml, and the concentration of described alkaline matter is 1 ~ 50 mg/ml.
Preferably, the mass ratio of described graphene oxide and described alkaline matter is 50:1 ~ 1:50.
Preferably, also comprise after described calcining:
By dry after the product cleaning after calcining.
Preferably, described calcining is carried out under protective atmosphere, and the temperature of described calcining is 600 ~ 1000 DEG C, and the time of described calcining is 30 ~ 600min.
Preferably, the programming rate of described calcining is 1 ~ 20 DEG C/min.
Present invention also provides the three-dimensional porous Graphene prepared by the preparation method described in a kind of such scheme.
The three-dimensional porous Graphene that present invention also provides described in prepared by the preparation method described in a kind of such scheme or such scheme can be used as electrode material for super capacitor and applies.
This application provides a kind of preparation method of three-dimensional porous Graphene, be specially: first graphene oxide, alkaline matter are mixed with water, obtain composite dispersion liquid; Again polyurethane sponge is immersed in composite dispersion liquid, make graphene oxide and alkaline matter load on polyurethane sponge, obtain compound system; Finally compound system is calcined, obtain three-dimensional porous Graphene.In the process of the three-dimensional porous Graphene of preparation, the application makes the surface of Graphene be filled with hole by the activation processing of alkaline matter, and itself and polyurethane sponge template act synergistically, and obtain the Graphene of high-specific surface area, high porosity; Polyurethane sponge is as masterplate simultaneously, for Graphene provides a kind of structure of three-dimensional intertexture, improves the stacking density of product.
Because the grapheme material itself please prepared has three-dimensional graded porous structure, its larger hole provides the passage that ion shuttles back and forth, a large amount of micropore and mesoporously provide abundant charge adsorption space, the Graphene that therefore prepared by the application has good chemical property as electrode material.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of three-dimensional grapheme prepared by the embodiment of the present invention 1;
Fig. 2 is the stereoscan photograph of three-dimensional porous Graphene prepared by the embodiment of the present invention 3;
Fig. 3 is the cycle performance curve chart of three-dimensional porous Graphene as electrode of super capacitor under organic electrolyte system of the embodiment of the present invention 3 preparation;
Fig. 4 is the cyclic voltammetric performance map of three-dimensional porous Graphene as electrode of super capacitor under organic electrolyte system of the embodiment of the present invention 4 preparation;
Fig. 5 is the high rate performance curve chart of three-dimensional porous Graphene as electrode of super capacitor under organic electrolyte system of the embodiment of the present invention 4 preparation.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of preparation method of three-dimensional porous Graphene, comprise the following steps:
A), graphene oxide, alkaline matter are mixed with water, obtains composite dispersion liquid;
B), polyurethane sponge is immersed in described composite dispersion liquid, dry after the polyurethane sponge obtained is taken out, then calcine, obtain three-dimensional porous Graphene.
This application provides a kind of preparation method of three-dimensional porous Graphene, it for raw material, by chemical reaction, obtains a kind of three-dimensional porous Graphene with graphene oxide, polyurethane sponge and alkaline matter.Structure due to Graphene makes its electrode material as ultracapacitor have excellent chemical property.
In the process of the three-dimensional porous Graphene of preparation, first graphene oxide, alkaline matter mix with water by the application, obtain composite dispersion liquid.In order to make above-mentioned raw materials mix, preferably, the preparation process of described composite dispersion liquid is specially:
Graphene oxide is mixed with water, ultrasonic disperse, obtain graphene oxide dispersion;
Alkaline matter is mixed with water, ultrasonic disperse, obtain the aqueous solution of alkaline matter;
Under ultrasonication, the described aqueous solution by alkaline matter is mixed with graphene oxide dispersion, obtains composite dispersion liquid.
In above process, the mass ratio of described graphene oxide and described alkaline matter is preferably 50:1 ~ 1:50, and in an embodiment, the mass ratio of described graphene oxide and described alkaline matter is preferably 1:1 ~ 1:20; The performance impact of mass ratio to three-dimensional porous Graphene of graphene oxide described in the application and alkaline matter is larger, if the mass ratio of graphene oxide and alkaline matter increases, then activation effect is stronger, pore-creating effect is more remarkable, but too high mass ratio is also unfavorable for the performance of product, make productive rate seriously diminish first, specific area also can not increase simultaneously.The mass concentration of described graphene oxide is preferably 0.1 ~ 10mg/ml, the mass concentration of described graphene oxide is more preferably 1mg/ml ~ 5mg/ml in an embodiment, if the concentration of graphene oxide is excessive, then composite dispersion liquid can be too sticky, is unfavorable for the absorption of polyurethane sponge.Graphene oxide described in the application preferably prepares according to the Hummers method improved.Alkaline matter described in the application be preferably in potassium hydroxide and NaOH one or more, be more preferably potassium hydroxide.
According to the present invention, after preparing composite dispersing agent, then polyurethane sponge is immersed in described composite dispersion liquid, make the abundant adsorption and oxidation Graphene of polyurethane sponge and alkaline matter, dry after again polyurethane sponge being taken out, make graphene oxide and alkaline matter load on polyurethane sponge.Described in the application, polyurethane sponge is as template, and graphene oxide can be assembled into three-dimensional by two dimension by graphene oxide-loaded by it.
Polyurethane sponge obtained above is finally calcined by the application, make graphene oxide and alkali substance reaction, at high temperature, alkaline matter carries out priming reaction, realize the pore-creating to graphene oxide, simultaneously due to the template action of polyurethane, make graphene oxide be assembled into three-dimensional structure by two-dimensional structure, thus improve density and the specific area of graphene oxide.Calcine described in the application and carry out under an inert atmosphere.Preferably, the application adopts the mode heated up gradually to be warming up to calcining heat, is beneficial to the fusing of alkaline matter, reaction.The described programming rate heated up gradually is preferably 1 ~ 20 DEG C/min.The temperature of described calcining is preferably 600 ~ 1000 DEG C, and the time of described calcining is preferably 30 ~ 600min.In calcination process, alkaline matter is for potassium hydroxide, and the reaction equation of described reaction is: 6KOH+2C=2K+3H
2+ 2K
2cO
3.
Preferably, after calcining, the product after calcining finally carries out cleaning by the application, dry, obtains three-dimensional porous Graphene.
The application has prepared a kind of three-dimensional porous Graphene according to above method, thus, this application provides a kind of three-dimensional porous Graphene prepared by preparation method described according to the method described above.
According to the structure of Graphene prepared by the application, the electrode material of ultracapacitor can be it can be used as.Thus, this application provides the application of three-dimensional porous Graphene on super capacitor material described in prepared by the preparation method described in such scheme or such scheme.
The application with polyurethane sponge, graphene oxide and alkaline matter for raw material, three-dimensional porous Graphene is obtained by chemical conversion means, the Graphene of this structure has remarkable advantage: have larger density having high specific area simultaneously, be beneficial to reduction of device volume; Three-dimensional porous Graphene is while providing abundant charge storage space, and the macroporous structure of itself is also beneficial to ion transport; Low raw-material cost, preparation technology is simple.Therefore, the three-dimensional porous Graphene that prepared by the application has excellent capacitive property as electrode material.
In order to understand the present invention further, below in conjunction with embodiment, the preparation method to three-dimensional porous Graphene provided by the invention is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
A) take the graphene oxide that 500mg prepared by the Hummers method improved and be placed in beaker, add 100ml deionized water wherein, abundant ultrasonic disperse, obtains graphene oxide dispersion;
B) polyurethane sponge of one piece of suitable size is immersed completely in a) the obtained graphene oxide dispersion of step, stir, extruding, it is made fully to absorb, take out sponge, be positioned on clean culture dish, dry at 60 DEG C, make graphene oxide and potassium hydroxide load on polyurethane sponge;
C) by step b) polyurethane structural of gained under an argon atmosphere, 5 DEG C/min is warming up to 1000 DEG C, and keeps 0.5h, and after calcining terminates, Temperature fall, obtains product;
D) cleaning also desciccate, obtains three-dimensional grapheme.
The classifying porous graphene-structured of three-dimensional embodiment 1 prepared carries out sem test, and as shown in Figure 1, as shown in Figure 1, three-dimensional grapheme prepared by the present embodiment has three-dimensional cross-linked frame structure.
Embodiment 2
A) take 100mg NaOH and be placed in beaker, add 50ml deionized water wherein, abundant ultrasonic disperse, obtains sodium hydrate aqueous solution;
B) polyurethane sponge of one piece of suitable size is immersed completely in a) the obtained NaOH dispersion liquid of step, stir, extruding, make it fully absorb, take out sponge, be positioned on clean culture dish, dry at 40 DEG C, make NaOH load on polyurethane sponge;
C) by step b) polyurethane structural of gained under an argon atmosphere, 10 DEG C/min is warming up to 600 DEG C, and keeps h, and after calcining terminates, Temperature fall, cannot obtain product.
Embodiment 3
A) take the graphene oxide that 5mg prepared by the Hummers method improved and be placed in beaker, add 5ml deionized water wherein, abundant ultrasonic disperse, obtains graphene oxide dispersion;
B) take 100mg potassium hydroxide and be placed in beaker, add 5ml deionized water wherein, abundant ultrasonic disperse, obtains potassium hydroxide aqueous solution;
C) under continual ultrasonic, by step b) potassium hydroxide aqueous solution that obtains joins in the graphene oxide dispersion that step a) obtains, wherein: in every milliliter of dispersion liquid, the mass ratio of graphene oxide and potassium hydroxide is 1:20, and the mass concentration of graphene oxide is 0.5mg/ml; Continual ultrasonic 2h, namely obtains graphene oxide-potassium hydroxide composite dispersion liquid;
D) polyurethane sponge of one piece of suitable size is immersed step c completely) in obtained composite dispersion liquid, stir, extruding, it is made fully to absorb, take out sponge, be positioned on clean culture dish, at room temperature naturally dry, make graphene oxide and potassium hydroxide load on polyurethane sponge;
E) by steps d) polyurethane structural of gained in a nitrogen atmosphere, 1 DEG C/min is warming up to 900 DEG C and calcines, and keeps 0.5h, and after calcining terminates, Temperature fall, obtains product;
F) cleaning also desciccate, obtains three-dimensional classifying porous Graphene.
The classifying porous Graphene of three-dimensional embodiment 3 prepared carries out sem test, and as shown in Figure 2, as shown in Figure 2, Graphene prepared by the present embodiment has outside for three-dimensional cross-linked, and inside is full of the frame structure of hole.
Fig. 3 is the cycle performance curve chart of the classifying porous graphene-structured of three-dimensional as electrode of super capacitor under organic electrolyte system of embodiment 3 preparation, after 1000 circle cycle charge-discharges, its ratio capacitance is circulate first 94%, indicates Graphene prepared by the present embodiment and has excellent electrochemical stability as electrode material.
Embodiment 4
A) take the graphene oxide that 500mg prepared by the Hummers method improved and be placed in beaker, add 50ml deionized water wherein, abundant ultrasonic disperse, obtains graphene oxide dispersion;
B) take 500mg potassium hydroxide, be placed in beaker, add 50ml deionized water wherein, abundant ultrasonic disperse, obtains potassium hydroxide aqueous solution;
C) under continual ultrasonic, by step b) potassium hydroxide aqueous solution that obtains joins in the graphene oxide dispersion that step a) obtains, wherein: in every milliliter of dispersion liquid, the mass ratio of graphene oxide and potassium hydroxide is 1:1, and the mass concentration of graphene oxide is 5mg/ml; Continual ultrasonic 1h, namely obtains graphene oxide-potassium hydroxide composite dispersion liquid;
D) polyurethane sponge of one piece of suitable size is immersed step c completely) in obtained composite dispersion liquid, stir, extruding, make it fully absorb, take out sponge, be positioned on clean culture dish, dry at 90 DEG C, make graphene oxide and potassium hydroxide load on polyurethane sponge;
E) by steps d) polyurethane structural of gained in a nitrogen atmosphere, 20 DEG C/min is warming up to 900 DEG C and calcines, and keeps 4h, and after calcining terminates, Temperature fall, obtains product;
F) cleaning also desciccate, obtains three-dimensional classifying porous Graphene.
Fig. 4 is the cyclic voltammetric performance map of the classifying porous graphene-structured of three-dimensional as electrode of super capacitor under organic electrolyte system of embodiment 4 preparation, curve a is the cyclic voltammetric performance curve of ultracapacitor 200mV/s, curve b is the cyclic voltammetry curve of ultracapacitor 150mV/s, curve c is the cyclic voltammetry curve of 100mV/s, and curve d is the cyclic voltammetry curve of 50mV/s; As shown in Figure 4, the Graphene that prepared by the present embodiment has excellent fast charging and discharging performance as electrode material.Fig. 5 is the high rate performance curve chart of the Graphene prepared of the present embodiment as electrode of super capacitor under organic electrolyte system, and as shown in Figure 5, this electrode material still has good performance under high rate charge-discharge, is conducive to practical application.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection range of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (9)
1. a preparation method for three-dimensional porous Graphene, comprises the following steps:
A), graphene oxide, alkaline matter are mixed with water, obtains composite dispersion liquid;
B), polyurethane sponge is immersed in described composite dispersion liquid, dry after the polyurethane sponge obtained is taken out, then calcine, obtain three-dimensional porous Graphene.
2. preparation method according to claim 1, is characterized in that, described alkaline matter be selected from potassium hydroxide and NaOH one or both.
3. preparation method according to claim 1, is characterized in that, in described composite dispersion liquid, the concentration of described graphene oxide is 0.1 ~ 10 mg/ml, and the concentration of described alkaline matter is 1 ~ 50 mg/ml.
4. preparation method according to claim 1, is characterized in that, the mass ratio of described graphene oxide and described alkaline matter is 50:1 ~ 1:50.
5. preparation method according to claim 1, is characterized in that, also comprises after described calcining:
By dry after the product cleaning after calcining.
6. preparation method according to claim 1, is characterized in that, described calcining is carried out under protective atmosphere, and the temperature of described calcining is 600 ~ 1000 DEG C, and the time of described calcining is 30 ~ 600min.
7. preparation method according to claim 1, is characterized in that, the programming rate of described calcining is 1 ~ 20 DEG C/min.
8. the three-dimensional porous Graphene prepared by the preparation method described in any one of claim 1 ~ 7.
9. three-dimensional porous Graphene prepared by the preparation method according to any one of claim 1 ~ 7 or according to claim 8 can be used as electrode material for super capacitor and applies.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240731A (en) * | 2019-05-23 | 2019-09-17 | 东南大学 | A kind of preparation method of graphene with high specific surface-metal oxide composite sponge |
| CN117603659A (en) * | 2024-01-18 | 2024-02-27 | 常熟理工学院 | Preparation method of liquid metal/graphene three-dimensional heat conduction material and heat conduction polymer composite material |
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| CN110240731B (en) * | 2019-05-23 | 2021-06-25 | 东南大学 | Preparation method of graphene-metal oxide composite sponge with high specific surface area |
| CN117603659A (en) * | 2024-01-18 | 2024-02-27 | 常熟理工学院 | Preparation method of liquid metal/graphene three-dimensional heat conduction material and heat conduction polymer composite material |
| CN117603659B (en) * | 2024-01-18 | 2024-04-19 | 常熟理工学院 | Preparation method of liquid metal/graphene three-dimensional heat conduction material and heat conduction polymer composite material |
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