CN102760582A - Graphene/carbon nano tube/nickel electrode and preparation method and application of grapheme/carbon nano tube/nickel electrode - Google Patents
Graphene/carbon nano tube/nickel electrode and preparation method and application of grapheme/carbon nano tube/nickel electrode Download PDFInfo
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- Y02E60/10—Energy storage using batteries
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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 field of electrochemical materials, and discloses a grapheme/carbon nano tube/nickel electrode and a preparation method thereof. The preparation method of the composite material comprises the following steps: a graphene oxide and carbon nano tube mixed solution is prepared; a graphite oxide/carbon nano tube/nickel electrode is prepared through electrophoresis; and the grapheme/carbon nano tube/nickel electrode is prepared. The invention provides the preparation method of the grapheme/carbon nano tube/nickel electrode; as the graphite oxide/carbon nano tube material is directly deposited on an electrode plate, a complicated coating process can be omitted, the process is simple, and the time is short; in addition, equivalent series resistance (ESR) of the graphite oxide/carbon nano tube/nickel electrode is reduced, so that the power density of a super capacitor is increased more efficiently.
Description
Technical field
The present invention relates to the electrochemical material field, relate in particular to a kind of Graphene/CNT/nickel electrode, its preparation method and application.
Background technology
The strong K sea nurses of the peace moral of Univ Manchester UK (Andre K.Geim) etc. were prepared grapheme material in 2004, pay attention to widely because its particular structure and photoelectric property have received people.Mono-layer graphite is because its big specific area, good conduction, heat conductivility and low thermal coefficient of expansion and be considered to desirable material.As: 1, high strength, the Young mole, (1,100GPa), fracture strength: (125GPa); 2, high heat conductance, (5,000W/mK); 3, high conductivity, carrier transport rate, (200,000cm
2/ V*s); 4, high specific area, (calculated value: 2,630m
2/ g).Especially its high conductivity matter, the structural property of the big specific surface character and the nanoscale of its monolayer two dimension can be used as electrode material in ultracapacitor and lithium ion battery.
In addition since the two-dimensional structure of the monolayer of Graphene in drying loses the water process of interlayer, be easy to take place to reunite and be range upon range of; Curl or height fold; Finally cause the utilance of its specific area to reduce greatly,, therefore can be inserted between graphene layer through CNT because CNT and Graphene have a lot of similarities on structure and performance; Perhaps functional group on the CNT and the functional group on the Graphene react each other; Make CNT be grafted on the Graphene surface, make to be separated from each other out between graphene layer and the layer, improve the dried specific area of Graphene to reach; Avoid Graphene to reunite and lamination, and then increase the purpose of the ratio electric capacity of ultracapacitor.
The technology of traditional preparation process electrode slice is comparatively complicated, and adds certain binding agent, has increased the equivalent series resistance of electrode, influences the power density of ultracapacitor.
Summary of the invention
The object of the present invention is to provide Graphene/CNT that a kind of equivalent series resistance is low, electric conductivity is high/nickel electrode.
Graphene/CNT of the present invention/nickel electrode is to be made by following processing step:
Step S1, with mass ratio 1～2: 1 graphite oxide and CNT add alcoholic solvent (as; Ethanol, isopropyl alcohol, propyl alcohol) in; Ultrasonic dispersion 0.5～2h, stirring at room 0.5～1h subsequently obtains the mixed solution of homodisperse graphene oxide and CNT;
It is 0.2～0.5mg/ml magnesium nitrate (Mg (NO that step S2, the mixed solution in step S1 add concentration
3)
26H
2O); Ultrasonic agitation 15～60min, parallel insertion spacing is two nickel foil electrodes of 0.5-1cm in the mixed solution subsequently, and between two electrodes, adds 40～80V direct current; Electrophoresis 5～20min can obtain graphene oxide/CNT/nickel electrode at negative pole;
After step S3, graphene oxide/CNT/nickel electrode that step S2 is obtained were dried naturally, then in inert atmosphere, in 400～800 ℃ of following calcination processing 3～8h, cooling obtained said Graphene/CNT/nickel electrode.
Among the above-mentioned preparation method, in the step 1, said graphite oxide is to adopt following steps to make:
Be that 50 order graphite powders, potassium peroxydisulfate and the phosphorus pentoxide of 2: 1: 1 purity 99.5% adds in 80 ℃ the concentrated sulfuric acid with mass ratio, stir that more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add potassium permanganate (its quality consumption is 3 times of graphite powder) again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add the 2.8L deionized water again, then add the hydrogen peroxide solution that 50mL concentration is 30wt%, the mixture color becomes glassy yellow afterwards; Suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h.
Graphene/CNT that said method makes/nickel electrode can be applied to play the electrode effect in the ultracapacitor.
The present invention makes Graphene/CNT/nickel electrode, has following advantage:
(1) through graphite oxide and CNT are dissolved in ultrasonic agitation in the ethanol, obtains Graphene through thermal reduction again, can better CNT be inserted between the Graphene lamella, bring into play the effect of performance complement better;
(2) through the method for electro-deposition, graphite oxide/carbon nano-tube material directly is deposited on the electrode slice, can save complicated coating process, and technology is simple and the time short; Can reduce simultaneously the equivalent series resistance (ESR) of electrode, thus the power density of more effective raising ultracapacitor.
Description of drawings
Fig. 1 is Graphene/CNT of the present invention/nickel electrode preparation technology's flow chart;
Fig. 2 is the SEM figure of Graphene;
Fig. 3 is Graphene/CNT among the embodiment 1/nickel electrode SEM figure.
Embodiment
Graphene/CNT of the present invention/nickel electrode.Prepare the composite material of graphite oxide and CNT earlier, then this composite material is joined sonicated in the ethanol, in above-mentioned suspension, add Mg (NO again
3)
26H
2O, ultrasonic to obtain uniform solution as electrolyte, with nickel foil as electrode; Its parallel symmetry is placed in the electrolyte, adds the direct current of 40-80V at the two ends of electrode, two die openings are 0.5cm; Electrophoresis a period of time just can obtain graphite oxide/CNT/nickel electrode, after drying naturally; Under argon shield, slowly be warming up to 400-800 ℃ of calcination 3-8h, take out after naturally cooling to room temperature, just can obtain Graphene/CNT/nickel electrode.
The preparation method of a kind of Graphene/CNT/nickel electrode, as shown in Figure 1, comprise the steps:
Step S1, with mass ratio 1～2: 1 graphite oxide and CNT add alcoholic solvent (as; Ethanol, isopropyl alcohol, propyl alcohol) in; Ultrasonic dispersion 0.5～2h, stirring at room 0.5～1h subsequently obtains the mixed solution of homodisperse graphene oxide and CNT;
It is the magnesium nitrate (Mg (NO of 0.2～0.5mg/ml that step S2, the mixed solution in step S1 add concentration
3)
26H
2O), ultrasonic agitation 15～60min, parallel insertion spacing is two nickel foil electrodes of 0.5cm in the mixed solution subsequently, and between two electrodes, adds 40～80V direct current, electrophoresis 5～20min obtains graphene oxide/CNT/nickel electrode at negative pole;
After step S3, graphene oxide/CNT/nickel electrode that step S2 is obtained are dried naturally, then in inert atmosphere, in 400～800 ℃ of following calcination processing 3～8h, cooling,, obtain said Graphene/CNT/nickel electrode.
Among the above-mentioned preparation method, among the step S1, said graphite oxide is to adopt following steps to make:
Be that 50 order graphite powders, potassium peroxydisulfate and the phosphorus pentoxide of 2: 1: 1 purity 99.5% adds in 80 ℃ the concentrated sulfuric acid with mass ratio, stir that more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add potassium permanganate (its quality consumption is 3 times of graphite powder) again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add the 2.8L deionized water again, then add the hydrogen peroxide solution that 50mL concentration is 30wt%, the mixture color becomes glassy yellow afterwards; Suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h.
The preparation method of a kind of Graphene/CNT provided by the invention/nickel electrode has following advantage:
(1) through graphite oxide and CNT are dissolved in ultrasonic agitation in the ethanol, obtains Graphene through thermal reduction again, can better CNT be inserted between the Graphene lamella, bring into play the effect of performance complement better;
(2) through the method for electro-deposition, graphite oxide/carbon nano-tube material directly is deposited on the electrode slice, can save complicated coating process, and technology is simple and the time short; Can reduce simultaneously the equivalent series resistance (ESR) of electrode, thus the power density of more effective raising ultracapacitor.
Do further explain in the face of preferred embodiment of the present invention down.
Embodiment 1
(1) 50 order graphite powders of 20g purity 99.5%, 10g potassium peroxydisulfate and 10g phosphorus pentoxide are added in 80 ℃ the concentrated sulfuric acid, stir, more than the cooling 6h, washing is to neutral, drying; In the concentrated sulfuric acid with 0 ℃ of dried sample adding, 230mL, add 60g potassium permanganate again, the temperature of mixture remains on below 20 ℃, in 35 ℃ oil bath, behind the maintenance 2h, slowly adds the 920mL deionized water then; Behind the 15min; Add the 2.8L deionized water again, then add the hydrogen peroxide solution that 50mL concentration is 30wt%, thing color to be mixed becomes glassy yellow; Suction filtration while hot uses that 5L concentration is that 10% hydrochloric acid washs again, suction filtration, promptly obtains graphite oxide at 60 ℃ of vacuumize 48h
(2) CNT with graphite oxide and acid treatment adds in the alcohol solvent with 1: 1 ratio of mass ratio, ultrasonic 0.5h, and stirring at room 0.5h obtains homodisperse graphene oxide and CNT mixed solution
(3) in (2) mixed solution, adding concentration is the Mg (NO of 0.5mg/ml
3)
26H
2O, ultrasonic 15min is to obtain uniform solution as electrolyte;, as electrode its parallel symmetry is placed in the electrolyte with the nickel foil of 5cm diameter, adds the direct current of 40V at the two ends of electrode; Two die openings are 0.5cm, and electrophoresis 5min just can obtain graphene oxide/CNT/nickel electrode;
(4) graphene oxide/CNT/nickel electrode of (3) gained is dried naturally after, under argon shield, slowly be warming up to 400 ℃ of calcination 8h, take out after naturally cooling to room temperature, just can obtain Graphene/CNT/nickel electrode.
Shown in Fig. 2 and 3, comparison Fig. 2 and Fig. 3, the electrode surface from Fig. 3 can be observed, and Graphene is kept apart by CNT is well-proportioned, and lamination or aggregation phenomenon do not take place, and substrate has also obtained good covering.
Embodiment 2
(1) with embodiment 1 in (1) identical;
(2) CNT with graphene oxide and acid treatment adds in the isopropanol solvent with 1: 1 ratio of mass ratio, ultrasonic 2h, and stirring at room 1h obtains homodisperse graphene oxide and CNT mixed solution;
(3) in (2) mixed solution, adding concentration is the Mg (NO of 0.2mg/ml
3)
26H
2O, ultrasonic 15min is to obtain uniform solution as electrolyte; With the nickel foil of 5cm diameter as electrode; Its parallel symmetry is placed in the electrolyte, adds the direct current of 80V at the two ends of electrode, two die openings are 0.5cm; Electrophoresis 20min just can obtain graphene oxide/CNT/nickel electrode;
(4) graphene oxide/CNT/nickel electrode of (3) gained is dried naturally after, under argon shield, slowly be warming up to 800 ℃ of calcination 3h, take out after naturally cooling to room temperature, just can obtain Graphene/CNT/nickel electrode.
Embodiment 3
(1) with embodiment 1 in (1) identical;
(2) CNT with graphite oxide and acid treatment adds in the propyl alcohol solvent with 2: 1 ratio of mass ratio, ultrasonic 1h, and stirring at room 1h obtains homodisperse graphene oxide and carbon nano-tube solution;
(3) in (2) mixed solution, adding concentration is the Mg (NO of 0.3mg/ml
3)
26H
2O, ultrasonic 15min is to obtain uniform solution as electrolyte; With the nickel foil of 5cm diameter as electrode; Its parallel symmetry is placed in the electrolyte, adds the direct current of 60V at the two ends of electrode, two die openings are 0.5cm; Electrophoresis 20min just can obtain graphene oxide/CNT/nickel electrode;
(4) graphene oxide/CNT/nickel electrode of (3) gained is dried naturally after, under argon shield, slowly be warming up to 600 ℃ of calcination 5h, take out after naturally cooling to room temperature, just can obtain Graphene/CNT/nickel electrode.
Should be understood that above-mentioned statement to preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with accompanying claims.
Claims (9)
1. Graphene/CNT/nickel electrode is characterized in that, the following method of this composite material by adopting makes:
S11, with mass ratio 1～2: 1 graphite oxide and CNT add in the alcoholic solvent, and ultrasonic dispersion obtains the mixed solution of graphene oxide and CNT;
S12, the mixed solution in step S11 add magnesium nitrate solution; Stir, two nickel foil electrodes of parallel insertion in the mixed solution subsequently, and between two electrodes, add the direct current of 40～80V; Carry out the electrophoresis reaction, can obtain graphene oxide/CNT/nickel electrode at negative pole;
After S13, graphene oxide/CNT/nickel electrode that step S12 is obtained were dried, then in inert atmosphere, in 400～800 ℃ of following calcination processing 3～8h, cooling obtained said Graphene/CNT/nickel electrode.
2. the preparation method of Graphene/CNT/nickel electrode is characterized in that, this preparation method comprises the steps:
S21, with mass ratio 1～2: 1 graphite oxide and CNT add in the alcoholic solvent, and ultrasonic dispersion obtains the mixed solution of graphene oxide and CNT;
S22, the mixed solution in step S21 add magnesium nitrate solution; Stir, two nickel foil electrodes of parallel insertion in the mixed solution subsequently, and between two electrodes, add direct current; Carry out the electrophoresis reaction, can obtain graphene oxide/CNT/nickel electrode at negative pole;
After S23, graphene oxide/CNT/nickel electrode that step S22 is obtained are dried, then in inert atmosphere, in 400～800 ℃ of following calcination processing 3～8h, cooling,, obtain said Graphene/CNT/nickel electrode.
3. preparation method according to claim 2 is characterized in that, among the step S21, said graphite oxide is to adopt following steps to make:
S211, with mass ratio be 2: 1: 1 graphite powder, potassium peroxydisulfate and phosphorus pentoxide add 80 ℃ the concentrated sulfuric acid in, stir, more than the cooling 6h, washing is to neutral, drying obtains mixture;
S212, the mixture that step S211 is obtained join in 0 ℃ the concentrated sulfuric acid; Add potassium permanganate again; And in 35 ℃ oil bath, behind the insulation reaction 2h, slowly add deionized water, add the hydrogen peroxide solution that concentration is 30wt% subsequently; Then carry out suction filtration, washing, suction filtration and dried again, promptly obtain graphite oxide.
4. preparation method according to claim 3 is characterized in that, the mass ratio of said graphite powder and potassium permanganate is 1: 3.
5. preparation method according to claim 2 is characterized in that, said alcoholic solvent is at least a in ethanol, isopropyl alcohol or the propyl alcohol.
6. preparation method according to claim 2 is characterized in that, among the said step S22, the concentration of said magnesium nitrate is 0.2～0.5mg/ml.
7. according to claim 2 or 6 described preparation methods, it is characterized in that among the said step S22, the spacing between said two electrodes is 0.5～1cm.
8. preparation method according to claim 8 is characterized in that, among the said step S22, said galvanic voltage is 40～80V.
A Graphene/polythiophene derivant composite materials as claimed in claim 1 in ultracapacitor or lithium ion battery as the application of electrode material.
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| CN103258656A (en) * | 2013-04-25 | 2013-08-21 | 华中科技大学 | Method for preparing electrodes of super capacitor based on nickel foam and products thereof |
| CN103346051A (en) * | 2013-06-09 | 2013-10-09 | 中国科学院深圳先进技术研究院 | Carbon nanometer tube negative electrode and method for preparing carbon nanometer tube negative electrode |
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| CN110548447A (en) * | 2019-09-11 | 2019-12-10 | 北京航空航天大学 | Preparation equipment and preparation method of conductive paste |
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