CN105271204A - Graphene/graphene nanoribbon compound hydrogel and preparation method thereof - Google Patents
Graphene/graphene nanoribbon compound hydrogel and preparation method thereof Download PDFInfo
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- CN105271204A CN105271204A CN201510807596.0A CN201510807596A CN105271204A CN 105271204 A CN105271204 A CN 105271204A CN 201510807596 A CN201510807596 A CN 201510807596A CN 105271204 A CN105271204 A CN 105271204A
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- 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 belongs to the technical field of nanometer materials and particularly relates to graphene/graphene nanoribbon compound hydrogel and a preparation method thereof. The graphene nanoribbon is obtained by shearing off and stripping a multiwall carbon nanotube in the radial direction. The graphene/graphene nanoribbon compound hydrogel is of a three-dimensional network structure obtained by means of in-situ self-assembly of a graphene nanosheet and the graphene nanoribbon. Two-dimensional graphene sheet layers mainly serve as a physical crosslinking network to play a role in supporting skeleton, and the quasi-one-dimensional graphene nanoribbon serves as a penetration bridge to play in role in connecting the graphene sheet layers. The preparation method is a simple novel method for synthesizing and controlling the three-dimensional structure of a graphene-based composite material, operation is simple, control is easy, cost is low, pollution is avoided, and large-scale production is facilitated. The graphene/graphene nanoribbon compound hydrogel will become an ideal carrier material and an electrode material for a supercapacitor and other new energy devices.
Description
Technical field
The invention belongs to grapheme material technical field, be specifically related to a kind of Graphene/graphene nanobelt composite aquogel and preparation method thereof, the electrode materials of the new energy devices such as solid support material and ultracapacitor can be used as.
Technical background
Graphene is the graphite of monolithic layer, by sp
2carbon atom Hexagonal array forms.Graphene has higher inside carrier mobility (200000cm
2v
-1s
-1), good thermal conductivity (~ 5000Wm
-1k
-1), high transmission rate (~ 97.7%) and theoretical specific surface area (2630m
2g
-1), and the mechanical strength of excellence.Therefore, Graphene all has broad application prospects in many aspects.But in actual applications, because the π π of graphene film interlayer interacts, graphene sheet layer is easy to again stacking, forms the structure of class graphite, the excellent properties of Graphene itself cannot be fully used.Therefore, the stacking of graphene sheet layer how is effectively suppressed to be the key realizing grapheme material widespread use.
Graphene nanobelt is a kind of accurate one dimension c-based nanomaterial, and it has acted on the physical and chemical performance of carbon nanomaterial excellence, as higher electroconductibility, excellent mechanical property and good chemical stability etc.In addition, the fringing effect that graphene nanobelt is special makes it have the character more adjustable more flexibly than Graphene, carbon nanotube.These special propertys make it all have very wide application prospect in fields such as energy transformation and storage, field-effect transistor, electronic sensor, high molecule nano composite materials, become the study hotspot in carbon nanomaterial field.
Self-assembly is stacking by hydrogen bond, π π and electrostatic attraction etc. interacts and obtains a kind of effective ways of the multilevel hierarchy of physical crosslinking.Self assembling process is a kind of spontaneous process, by rational design, self assembling process can be carried out by polycomponent simultaneously and not affect being formed of product, and the structure of self-assembly can give material some be different from the special performance of bulk mass, thus widen its Application Areas.This self-assembling technique is applied in graphene-based matrix material, the three-dimensional porous network structure with high-specific surface area can be formed, thus it is mutually stacking effectively to suppress between graphene sheet layer and graphene nanobelt, is conducive to the transmission of electronics and the migration of ion.
Summary of the invention
The Graphene that the object of the present invention is to provide a kind of preparation process simple, with low cost/graphene nanobelt compound hydrogel material and preparation method thereof.
Graphene provided by the present invention/graphene nanobelt compound hydrogel material, its raw materials composition comprises: graphite oxide, single wall or multi-walled carbon nano-tubes, potassium permanganate, the vitriol oil, xitix, sodium ascorbate, hydroiodic acid HI etc.
Graphene provided by the present invention/graphene nanobelt compound hydrogel material, its preparation process be with reductive agent by stannic oxide/graphene nano sheet, stannic oxide/graphene nano band carries out in-situ reducing and self-assembly prepares.Concrete steps are as follows:
(1) graphite oxide is scattered in deionized water, through ultrasonic disperse, obtains the graphene oxide dispersion of certain density stable dispersion;
(2) in proportion reductive agent is joined in graphene oxide water solution, ultrasonicly make it be uniformly dispersed, obtain mixed solution;
(3) by the mixed solution of the aqueous dispersions of a certain amount of stannic oxide/graphene nano band instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) mixed dispersion liquid of step (3) gained is kept standing at a certain temperature, for some time is reacted in oil bath, can obtain Graphene/graphene nanobelt composite aquogel.
In the present invention, described stannic oxide/graphene nano band cuts off carbon nanotube by solution oxide method radial direction to prepare, and this method can referenced patent US2010/0105834Al.
In the present invention, reductive agent used is selected from: xitix (vitamins C), sodium ascorbate, hydroiodic acid HI, Resorcinol.
In the present invention, the graphite oxide described in step (1) is prepared by Hummers method, and graphene oxide dispersion concentration is 2-5mg/mL.
In the present invention, the concentration of the reductive agent described in step (2) is 40-80mmol/L.
In the present invention, the concentration of the stannic oxide/graphene nano band aqueous dispersions described in step (3) is 0.5-1.5mg/mL.
In the present invention, in the mixed dispersion liquid described in step (4), the mass ratio of graphene oxide and stannic oxide/graphene nano band is 4:1 ~ 1:1.
In the present invention, the temperature described in step (4) is 80-100 DEG C, and the reaction times is 0.5-3.5h.
Use scanning electronic microscope (SEM), transmission electron microscope (TEM), X-ray diffractometer (XRD), electrochemical workstation characterizes structure and morphology and its performance as electrode material for super capacitor of Graphene-graphene nanobelt composite aquogel that the present invention obtains, and its result is as follows:
(1) SEM test result shows: Graphene/graphene nanobelt composite aquogel prepared in the present invention has multistage pore space structure, graphene sheet layer and graphene nanobelt are built into the skeleton structure of three-dimensional network jointly, graphene sheet layer is wrapped in banded graphene nanobelt, and simultaneously graphene nanobelt through between graphene sheet layer.This three-dimensional composite network not only defines hierarchical porous structure, and improves the specific surface area of material;
(2) TEM test result shows further: Graphene/graphene nanobelt composite aquogel prepared in the present invention is formed by graphene sheet layer and the collaborative dispersion of graphene nanobelt and self-assembly.Graphene nanobelt has high length-to-diameter ratio and special band edge, and banded graphene nanobelt is connected with each other by the laminated structure of Graphene, conductive network structure formed thus impels the special performance of graphene nanobelt to be fully used further.And graphene nanobelt interts in graphene sheet layer simultaneously, serve again the effect suppressing graphene sheet layer stacking simultaneously;
(3) XRD test result shows: prepared stannic oxide/graphene nano band (GONR) has a stronger diffraction peak in 2 θ=10.0 °, illustrate that carbon nanotube is successfully peeled off into nano belt structure.Graphene nanobelt (GNR) after reduction has a wider diffraction peak in 2 θ=26.0 °, correspond to (002) crystal face.Similarly, prepared graphene oxide (GO) has a stronger diffraction peak in 2 θ=10.0 °, illustrate that Graphene (G) is successfully oxidized.After reduction, there is the diffraction peak that is wider in 2 θ=26.0 °, same corresponding to (002) crystal face.And the similar XRD figure spectrum of Graphene/graphene nanobelt (G/GNR) matrix material again demonstrates mixture under the effect of reductive agent and is successfully reduced;
(4) electrochemical workstation test result shows, when prepared Graphene/graphene nano belt composite is used as electrode material for super capacitor, there is excellent ratio capacitance performance, can draw from constant current charge-discharge curve, when current density is 1A/g, its specific capacity value can reach 187.5F/g.
The invention has the advantages that:
1, preparation process is simple, environmental protection, easy handling, is a kind of preparation method effectively efficiently;
2, experimental design is ingenious:
First, the Graphene of two dimension and quasi-one-dimensional graphene nanobelt are carried out compound, the Graphene of high conductivity, high-specific surface area is interconnected with the graphene nanobelt with unique length-to-diameter ratio and marginal texture run through, increase the specific surface area of matrix material, effectively construct multilevel hierarchy;
The second, prepare matrix material by the method for simple self-assembly, reaction conditions is gentle, and can be realized by multiple reductive agent in the short period of time;
Graphene prepared by the present invention/graphene nanobelt composite aquogel, can be used as the electrode materials of the new energy devices such as a kind of desirable solid support material and ultracapacitor.
Accompanying drawing explanation
Fig. 1 is the photo of Graphene/graphene nanobelt composite aquogel prepared by embodiment 1.
Fig. 2 is the SEM figure after the Graphene/graphene nanobelt composite aquogel lyophilize of embodiment 1 preparation.
Fig. 3 is the TEM figure of Graphene/graphene nano belt composite prepared by embodiment 1.
Fig. 4 is the XRD figure of Graphene/graphene nano belt composite prepared by embodiment 1.
Fig. 5 is (A) cyclic voltammetry curve of Graphene/graphene nano belt composite prepared by embodiment 1, (B) constant current charge-discharge curve.
Embodiment
Below in conjunction with specific examples, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition, after the content of having read the present invention's instruction, those skilled in the art can make various change or amendment to the present invention, and these equivalent form of values fall within the application's appended claims limited range equally.
embodiment 1,the present embodiment comprises the following steps:
(1) graphite oxide is scattered in deionized water, the ultrasonic graphene oxide dispersion obtaining the stable dispersion of 2mg/mL;
(2) 170mg xitix is joined in 12mL graphene oxide water solution, ultrasonicly make it be uniformly dispersed;
(3) by the mixed solution of 8mL1.5mg/mL stannic oxide/graphene nano band aqueous dispersions instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) kept by the mixed solution of step (3) gained leaving standstill at 90 DEG C, oil bath reaction 1h, can obtain Graphene/graphene nanobelt composite aquogel.
SEM figure after the photo of this composite aquogel, lyophilize, TEM figure are shown in shown in Fig. 1-Fig. 3.
embodiment 2,the present embodiment comprises the following steps:
(1) graphite oxide is scattered in deionized water, the ultrasonic graphene oxide dispersion obtaining the stable dispersion of 2mg/mL;
(2) 170mg xitix is joined in 9mL graphene oxide water solution, ultrasonicly make it be uniformly dispersed;
(3) by the mixed solution of 13.3mL1.4mg/mL stannic oxide/graphene nano band aqueous dispersions instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) kept by the mixed solution of step (3) gained leaving standstill at 90 DEG C, oil bath reaction 2h, can obtain Graphene/graphene nanobelt composite aquogel.
embodiment 3,the present embodiment comprises the following steps:
(1) graphite oxide is scattered in deionized water, the ultrasonic graphene oxide dispersion obtaining the stable dispersion of 2mg/mL;
(2) 170mg xitix is joined in 14.4mL graphene oxide water solution, ultrasonicly make it be uniformly dispersed;
(3) by the mixed solution of 5.3mL1.4mg/mL stannic oxide/graphene nano band aqueous dispersions instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) kept by the mixed solution of step (3) gained leaving standstill at 90 DEG C, oil bath reaction 0.5h, can obtain Graphene/graphene nanobelt composite aquogel.
embodiment 4,the present embodiment comprises the following steps:
(1) graphite oxide is scattered in deionized water, the ultrasonic graphene oxide dispersion obtaining the stable dispersion of 2mg/mL;
(2) hydroiodic acid HI of 273mg45% is joined in 12mL graphene oxide water solution, ultrasonicly make it be uniformly dispersed;
(3) by the mixed solution of 8mL1.5mg/mL stannic oxide/graphene nano band aqueous dispersions instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) kept by the mixed solution of step (3) gained leaving standstill at 90 DEG C, oil bath reaction 2.5h, can obtain Graphene/graphene nanobelt composite aquogel.
embodiment 5,the present embodiment comprises the following steps:
(1) graphite oxide is scattered in deionized water, the ultrasonic graphene oxide dispersion obtaining the stable dispersion of 2mg/mL;
(2) 72mg sodium ascorbate is joined in 12mL graphene oxide water solution, ultrasonicly make it be uniformly dispersed;
(3) by the mixed solution of 12mL1mg/mL stannic oxide/graphene nano band aqueous dispersions instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) kept by the mixed solution of step (3) gained leaving standstill at 95 DEG C, oil bath reaction 5h, can obtain Graphene/graphene nanobelt composite aquogel.
Claims (9)
1. a preparation method for Graphene/graphene nanobelt compound hydrogel material, is characterized in that concrete steps are as follows:
(1) graphite oxide is scattered in deionized water, through ultrasonic disperse, obtains the graphene oxide dispersion of stable dispersion;
(2) reductive agent is joined in graphene oxide water solution, ultrasonicly make it be uniformly dispersed, obtain mixed solution;
(3) by the mixed solution of the aqueous dispersions of stannic oxide/graphene nano band instillation step (2) gained, stir for some time, form homogeneous dispersion liquid;
(4) mixed dispersion liquid of step (3) gained is kept standing at a certain temperature, through oil bath reaction, namely obtain Graphene/graphene nanobelt composite aquogel.
2. the preparation method of Graphene-graphene nanobelt composite aquogel according to claim 1, is characterized in that the graphene oxide dispersion concentration described in step (1) is 2-5mg/mL.
3. the preparation method of Graphene/graphene nanobelt composite aquogel according to claim 2, is characterized in that the reductive agent described in step (2) is selected from xitix, sodium ascorbate, hydroiodic acid HI, Resorcinol.
4., according to the preparation method of one of claim 1-3 described Graphene/graphene nanobelt composite aquogel, it is characterized in that the concentration of the reductive agent described in step (2) is 40-80mmol/L.
5. the preparation method of Graphene/graphene nanobelt composite aquogel according to claim 4, is characterized in that the concentration of the stannic oxide/graphene nano band aqueous dispersions described in step (3) is 0.5-1.5mg/mL.
6., according to the preparation method of one of claim 1,2,3,5 described Graphene/graphene nanobelt composite aquogel, it is characterized in that the mass ratio of graphene oxide and stannic oxide/graphene nano band in the mixed dispersion liquid described in step (4) is 4:1 ~ 1:1.
7. the preparation method of Graphene/graphene nanobelt composite aquogel according to claim 6, it is characterized in that the temperature of the oil bath reaction described in step (4) is 80-100 ° of C, the reaction times is 0.5-6.5h.
8. the Graphene prepared by the described preparation method of one of claim 1-7/graphene nanobelt composite aquogel.
9. if Graphene according to claim 8/graphene nanobelt composite aquogel is as the application of the electrode materials of solid support material and ultracapacitor new energy devices.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082341A (en) * | 2016-06-07 | 2016-11-09 | 东华大学 | A kind of preparation method of molybdenum sulfide/Graphene graphene nanobelt aerogel composite |
| CN106207125A (en) * | 2016-08-23 | 2016-12-07 | 东华大学 | Sulfur doping selenizing molybdenum/Graphene graphene nanobelt aeroge and preparation thereof |
| CN106970116A (en) * | 2017-03-20 | 2017-07-21 | 中国石油大学(华东) | A kind of polyhedral cobaltosic oxide three-dimensional porous Graphene gel composite material film sensitive to acetone |
| CN107731570A (en) * | 2017-11-24 | 2018-02-23 | 南京正森环保科技有限公司 | A kind of method that Supercapacitor carbon surface chemistry group eliminates |
| CN108101029A (en) * | 2017-12-25 | 2018-06-01 | 信利光电股份有限公司 | A kind of preparation method of graphene-Nano-Zinc water-setting gel electrode |
| CN108132289A (en) * | 2017-12-25 | 2018-06-08 | 信利光电股份有限公司 | A kind of preparation method of graphene-nano-silver water gel electrode |
| CN112265982A (en) * | 2020-10-23 | 2021-01-26 | 哈尔滨工业大学 | Preparation method of N-doped graphene/graphene nanoribbon composite aerogel |
| CN115376836A (en) * | 2022-09-14 | 2022-11-22 | 南通海星电子股份有限公司 | Preparation method and application of caffeic acid modified chemically-cut carbon nanotube self-assembled composite material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106082341A (en) * | 2016-06-07 | 2016-11-09 | 东华大学 | A kind of preparation method of molybdenum sulfide/Graphene graphene nanobelt aerogel composite |
| CN106207125A (en) * | 2016-08-23 | 2016-12-07 | 东华大学 | Sulfur doping selenizing molybdenum/Graphene graphene nanobelt aeroge and preparation thereof |
| CN106207125B (en) * | 2016-08-23 | 2018-10-26 | 东华大学 | Sulfur doping selenizing molybdenum/graphene-graphene nanobelt aeroge and its preparation |
| CN106970116A (en) * | 2017-03-20 | 2017-07-21 | 中国石油大学(华东) | A kind of polyhedral cobaltosic oxide three-dimensional porous Graphene gel composite material film sensitive to acetone |
| CN106970116B (en) * | 2017-03-20 | 2019-09-10 | 中国石油大学(华东) | The sensitive polyhedral cobaltosic oxide of a kind of pair of acetone-three-dimensional porous Graphene gel composite material film |
| CN107731570A (en) * | 2017-11-24 | 2018-02-23 | 南京正森环保科技有限公司 | A kind of method that Supercapacitor carbon surface chemistry group eliminates |
| CN107731570B (en) * | 2017-11-24 | 2019-10-18 | 南京正森环保科技有限公司 | A kind of method that Supercapacitor carbon surface chemistry group is eliminated |
| CN108101029A (en) * | 2017-12-25 | 2018-06-01 | 信利光电股份有限公司 | A kind of preparation method of graphene-Nano-Zinc water-setting gel electrode |
| CN108132289A (en) * | 2017-12-25 | 2018-06-08 | 信利光电股份有限公司 | A kind of preparation method of graphene-nano-silver water gel electrode |
| CN112265982A (en) * | 2020-10-23 | 2021-01-26 | 哈尔滨工业大学 | Preparation method of N-doped graphene/graphene nanoribbon composite aerogel |
| CN115376836A (en) * | 2022-09-14 | 2022-11-22 | 南通海星电子股份有限公司 | Preparation method and application of caffeic acid modified chemically-cut carbon nanotube self-assembled composite material |
| CN115376836B (en) * | 2022-09-14 | 2023-08-01 | 南通海星电子股份有限公司 | Preparation method and application of caffeic acid modified chemically-cut carbon nano tube self-assembled composite material |
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