CN102354611A - Graphene/ manganese oxide nano composite material and preparation method thereof - Google Patents
Graphene/ manganese oxide nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene/ manganese oxide nano composite material. A self-made thin graphene material is used as a reductant, and the composite material is obtained by reducing potassium permanganate at a low temperature by a reflux condensation process. The invention further provides a preparation method which mainly comprises the following steps of: carrying out oxidation stripping by using graphite paper as an anode, a carbon bar as a cathode and strong sulfuric acid (the concentration of 98%) as an electrolyte to prepare graphene oxide powder; then preparing the graphene oxide powder into graphene powder, adding the potassium permanganate to a graphene suspension, heating, separating, washing and drying in vacuum. The invention has the advantages of simple technology and low cost. The prepared composite material is of a porous network structure, has small crystal grain size, is uniformly distributed and has a manganese oxide content of 16-82%. Meanwhile, owning to the porous network structure of the surface, the dispersion co-efficiency of protons is bigger. The protons more easily enter active substances, so that the composite material has excellent electrochemical property and excellent electricity conducting property and can be used as electrode materials of super capacitors.
Description
Technical field
The present invention relates to a kind of electrode material.
Background technology
Graphene is because its unique electrical properties, makes itself and semi-conducting material compound become a hot research problem.Graphene is discrete fully monolayer carbon material, and its whole surface can form electric double layer, but in forming macroscopical aggregation process, congestion stack between the Graphene lamella can make the area that forms effective electric double layer reduce.Therefore; Through semiconductor nano material and Graphene is compound; Make its spacer as Graphene; With the interaction that reduces greatly between the Graphene lamella; Graphene is as the backing material of semi-conductor nano particles simultaneously; Can play the effect of electron transport passage, thereby improve the electric property of semi-conducting material effectively.At present; The method for preparing graphene-based nano composite material has following several: (1) graphene oxide reducing process: with nano particle attached on the graphene oxide sheet; Adopt chemical reducing agent or utilize the catalytic action of light that graphene oxide is reduced into Graphene, thereby obtain graphene-based nano composite material.This method cost is low, productive rate is high, but the recovery of Graphene intrinsic structure is undesirable during redox graphene, influences the conductivity of composite material.(2) electro-deposition method: Graphene is coated on the conductive current collector as electrode, adopts pulse current that metal oxide nanoparticles is deposited on the Graphene surface.The advantage of this method is that technological parameter is easy to control, and shortcoming is that high dielectric insulation property metal oxide is difficult on the Graphene of surface modification not and deposits, and can only deposit with fault location at the Graphene edge.(3) microwave method: the characteristics of utilizing microwave energy to concentrate make nano particle be deposited on the Graphene surface rapidly.The characteristics that adopt microwave method are that the time is short, and technology is simple, but reaction speed is too fast, and operating process is wayward, and composite material is reunited easily and grown up.
Summary of the invention
The object of the present invention is to provide a kind ofly be prone on Graphene deposition, reaction speed is easy to control, crystallite dimension is less, distribution uniform and Graphene/manganese dioxide nano-composite material that conducts electricity very well and preparation method
Graphene/manganese dioxide nano-composite material of the present invention is that a kind of average thickness is 1nm, and the lamella width is about 3 μ m, and manganese dioxide is equal ability nucleating growth on the two sides of graphene film, and is the composite material of porous network structure.
The preparation method of above-mentioned composite material is following:
One, the preparation of grapheme material
1, the preparation of graphene oxide:
With the graphite paper is anode, and carbon-point is a negative electrode, and the concentrated sulfuric acid (concentration 98%) is an electrolyte, under constant current 0.2A, graphite paper is carried out oxidation and peels off.After peeling off 20～30h, with 10 times of electrolyte dilution, treat to adopt the supercentrifuge of 12000 commentaries on classics/min to separate and filtration behind the solution cool to room temperature with distilled water.To neutral, 50～60oC oven dry promptly obtains the graphene oxide powder under 10～100Pa vacuum with the powder behind the abundant washing and filtering of distilled water.
2, the preparation of grapheme material:
The weight ratio of graphene oxide powder by 1:1 joined in the distilled water, and using ammoniacal liquor to regulate its pH is 9～10.At power is ultrasonic 1～3h under the 150W, to obtain stable graphene oxide suspension.In suspension, drip hydrazine hydrate, its addition adds 0.01～0.02 milliliter by every milligram of graphene oxide powder.With 75～85oC water bath with thermostatic control heating, 6～12h, to neutral, 50～60oC oven dry promptly obtains the thin layer grapheme material under 10～100Pa vacuum with the reactant washing.
Two, the preparation of Graphene/manganese dioxide nano-composite material:
Press potassium permanganate: thin layer Graphene=0.1～1.0:0.12～0.225 (weight ratio); With potassium permanganate join in the graphene suspension; This graphene suspension is above-mentioned thin layer grapheme material to be diluted by the concentration of 0.8～1.5mg/mL with distilled water to form (Graphene is excessive in the course of reaction); Behind the ultrasonic dispersion 30min, with the mixed liquor flask of packing into.Adopting the reflux condensation mode method is heating 4h～20h under 95oC～105oC in temperature, suspension-turbid liquid is centrifugalized under 4000 commentaries on classics/min, and sediment is washed with distilled water, in filtrating, detects the existence less than the K ion.At last with sediment 50～60oC oven dry under 10～100Pa vacuum, promptly obtain manganese dioxide content and be Graphene/manganese dioxide nano-composite material of 16～82%.
The present invention compared with prior art has following advantage:
1, the Graphene/manganese dioxide nano-composite material that adopts the present invention to obtain is the porous network shape, and crystallite dimension is less, distribution uniform, and the content of manganese dioxide is 16～82%.
2, Biao Mian porous network structure makes that the diffusion coefficient of proton is bigger, gets into active material inside more easily, thereby makes this composite material have good electrochemical, and electric conductivity is good, and the electrode material that is suitable as ultracapacitor uses.
3, technology is simple, and reaction speed is easy to control.
Description of drawings
Fig. 1 is the surface scan Electronic Speculum figure of Graphene/manganese dioxide nano-composite material of obtaining of the present invention;
Fig. 2 is the transmission electron microscope picture of Graphene/manganese dioxide nano-composite material of obtaining of the present invention.
Embodiment
Embodiment 1
With the graphite paper is anode, and carbon-point is a negative electrode, and the concentrated sulfuric acid of 200mL (concentration 98%) is an electrolyte, under constant current 0.2A, graphite paper is carried out oxidation and peels off.After peeling off 20h, the distilled water that adds 2L is treated electrolyte dilution to adopt the supercentrifuge of 12000 commentaries on classics/min to separate and filtration behind the solution cool to room temperature.To neutral, the 50oC oven dry obtains the graphene oxide powder under the 100Pa vacuum with the powder behind the abundant washing and filtering of distilled water.Above-mentioned 100mg graphene oxide powder is joined in the 100mL distilled water, and using ammoniacal liquor to regulate its pH is 9.At power is ultrasonic 1h under the 150W, obtains stable graphene oxide suspension.In suspension, drip the 1mL hydrazine hydrate, 75oC water bath with thermostatic control heating 12h, to neutral, the 50oC oven dry promptly obtains the thin layer grapheme material under the 100Pa vacuum with the reactant washing.
Taking by weighing 0.1g potassium permanganate joins among the graphene suspension 150mL that concentration is 1.5mg/mL; Behind the ultrasonic dispersion 30min; With the mixed liquor flask of packing into; In temperature is heating 20h under the 95oC; Suspension-turbid liquid is centrifugalized under 4000 commentaries on classics/min; And with sediment with distilled water washing 8 times, at last with sediment 50oC oven dry under the 100Pa vacuum, promptly obtain manganese dioxide content and be Graphene/manganese dioxide nano-composite material of 16%.
Embodiment 2
With the graphite paper is anode, and carbon-point is a negative electrode, and the concentrated sulfuric acid of 200mL (concentration 98%) is an electrolyte, under constant current 0.2A, graphite paper is carried out oxidation and peels off.After peeling off 24h, the distilled water that adds 2L is treated electrolyte dilution to adopt the supercentrifuge of 12000 commentaries on classics/min to separate and filtration behind the solution cool to room temperature.To neutral, the 55oC oven dry obtains the graphene oxide powder under the 50Pa vacuum with the powder behind the abundant washing and filtering of distilled water.Above-mentioned 100mg graphene oxide powder is joined in the 100mL distilled water, and using ammoniacal liquor to regulate its pH is 10.At power is ultrasonic 2h under the 150W, obtains stable graphene oxide suspension.In suspension, drip the 1.5mL hydrazine hydrate, 80oC water bath with thermostatic control heating 9h, to neutral, the 55oC oven dry promptly obtains the thin layer grapheme material under the 50Pa vacuum with the reactant washing.Taking by weighing 0.5g potassium permanganate joins among the graphene suspension 150mL that concentration is 0.8mg/mL; Behind the ultrasonic dispersion 30min; With the mixed liquor flask of packing into; In temperature is heating 12h under the 100oC; Suspension-turbid liquid is centrifugalized under 4000 commentaries on classics/min; And with sediment with distilled water washing 9 times, at last with sediment 55oC oven dry under the 50Pa vacuum, promptly obtain manganese dioxide content and be Graphene/manganese dioxide nano-composite material of 69%.
Embodiment 3
With the graphite paper is anode, and carbon-point is a negative electrode, and the concentrated sulfuric acid of 200mL (concentration 98%) is an electrolyte, under constant current 0.2A, graphite paper is carried out oxidation and peels off.After peeling off 30h, add 2L distilled water, treat to adopt the supercentrifuge of 12000 commentaries on classics/min to separate and filtration behind the solution cool to room temperature electrolyte dilution.To neutral, the 60oC oven dry obtains the graphene oxide powder under the 10Pa vacuum with the powder behind the abundant washing and filtering of distilled water.Above-mentioned 100mg graphene oxide powder is joined in the 100mL distilled water, and using ammoniacal liquor to regulate its pH is 9.At power is ultrasonic 3h under the 150W, obtains stable graphene oxide suspension.In suspension, drip the 2mL hydrazine hydrate, 85oC water bath with thermostatic control heating 6h, to neutral, the 60oC oven dry promptly obtains the thin layer grapheme material under the 10Pa vacuum with the reactant washing.Taking by weighing 1.0g potassium permanganate joins among the graphene suspension 150mL that concentration is 1.5mg/mL; Behind the ultrasonic dispersion 30min; With the mixed liquor flask of packing into; In temperature is heating 4h under the 105oC; Suspension-turbid liquid is centrifugalized under 4000 commentaries on classics/min; And with sediment with distilled water washing 8 times, at last with sediment 60oC oven dry under the 10Pa vacuum, promptly obtain manganese dioxide content and be Graphene/manganese dioxide nano-composite material of 82%.
Can find out through S4800 field emission scanning electron microscope (see figure 1) and JEOL2010 transmission electron microscope (see figure 2); Graphene/manganese dioxide nano-composite material of preparing is thinner; Its average thickness is about 1nm; The lamella width is about 3 μ m; Manganese dioxide is equal ability nucleating growth on the two sides of graphene film; And be porous network structure, distribution uniform; XRD analysis is indicated as
γ-manganese dioxide, average grain size is about 20nm.With its electrode material as ultracapacitor, when charging and discharging currents density was 3A/g, the specific capacity of this ultracapacitor was 575Fg
-1, and after 1000 circulations, capacity still remains on more than 95%.
Claims (2)
1. Graphene/manganese dioxide nano-composite material, it is characterized in that: this composite material is that a kind of average thickness is 1nm, and the lamella width is about 3 μ m, manganese dioxide all can nucleating growth on the two sides of graphene film, and is the composite material of porous network structure.
2. the preparation method of above-mentioned Graphene/manganese dioxide nano-composite material is characterized in that:
One, the preparation of grapheme material
(1) preparation of graphene oxide: with the graphite paper is anode; Carbon-point is a negative electrode; Concentration is that 98% concentrated sulfuric acid is an electrolyte; Under constant current 0.2A, graphite paper being carried out oxidation peels off; After peeling off 20h～30h, with 10 times of electrolyte dilution, treat to adopt the supercentrifuge of 12000 commentaries on classics/min to separate and filtration behind the solution cool to room temperature with distilled water; To neutral, 50～60oC is dried under 10～100Pa vacuum with the powder behind the abundant washing and filtering of distilled water;
(2) preparation of grapheme material:
The weight ratio of above-mentioned graphene oxide powder by 1:1 joined in the distilled water; Using ammoniacal liquor to regulate its pH is 9～10; At power is ultrasonic 1～3h under the 150W; In suspension, drip hydrazine hydrate; Its addition adds 0.01～0.02 milliliter by every milligram of graphene oxide powder; With 75～85oC water bath with thermostatic control heating, 6～12h, to neutral, 50～60oC is dried under 10～100Pa vacuum with the reactant washing;
Two, the preparation of Graphene/manganese dioxide nano-composite material:
Press potassium permanganate: thin layer Graphene=0.1～1.0:0.12～0.225(weight ratio); With potassium permanganate join in the graphene suspension; This graphene suspension is with the concentration of distilled water by 0.8～1.5mg/mL above-mentioned thin layer grapheme material dilution to be formed; Behind the ultrasonic dispersion 30min; With the mixed liquor flask of packing into; Adopting the reflux condensation mode method is heating 4～20h under 95～105oC in temperature; Suspension is centrifugalized under 4000 commentaries on classics/min; And sediment washed with distilled water; In filtrating, detect existence, at last with sediment 50～60oC oven dry under 10～100Pa vacuum less than the K ion.
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Cited By (15)
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| CN102568855A (en) * | 2012-03-12 | 2012-07-11 | 重庆大学 | Carbon material-loading manganese dioxide nanowire array composite and method for producing same |
| CN102751105A (en) * | 2012-06-26 | 2012-10-24 | 北京交通大学 | Preparation method of dye-sensitized solar cell photoanode |
| CN102751097A (en) * | 2012-06-26 | 2012-10-24 | 北京交通大学 | Supercapacitor |
| CN103013056A (en) * | 2012-12-01 | 2013-04-03 | 福州大学 | Graphene/MnO2/conjugated polymer composite material, as well as preparation method and application thereof |
| CN103077835A (en) * | 2013-01-15 | 2013-05-01 | 上海大学 | Graphene load flower manganese dioxide (MnO2) composite material and ultrasonic synthetic method thereof |
| CN103107024A (en) * | 2013-02-26 | 2013-05-15 | 苏州大学 | Nitrogenous mesoporous carbon/MnO2 composite material and preparation method thereof |
| CN103489660A (en) * | 2013-09-05 | 2014-01-01 | 北京工业大学 | Manganese dioxide nanorod/graphene composite electrode material and preparation method thereof |
| CN103730257A (en) * | 2012-10-16 | 2014-04-16 | 海洋王照明科技股份有限公司 | Manganese dioxide/graphene composite electrode material, preparing method thereof, and electrochemical capacitor |
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| CN107754786A (en) * | 2017-10-16 | 2018-03-06 | 广西大学 | One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper |
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