CN102760582B - A kind of graphene/carbon nano-tube/nickel electrode, its preparation method and application - Google Patents
A kind of graphene/carbon nano-tube/nickel electrode, its preparation method and application Download PDFInfo
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- CN102760582B CN102760582B CN201110105430.6A CN201110105430A CN102760582B CN 102760582 B CN102760582 B CN 102760582B CN 201110105430 A CN201110105430 A CN 201110105430A CN 102760582 B CN102760582 B CN 102760582B
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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
- Y02E60/10—Energy storage using batteries
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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
Abstract
The invention belongs to electrochemical material field, it discloses a kind of graphene/carbon nano-tube/nickel electrode and preparation method thereof; The preparation method of this composite material comprises step: prepare graphene oxide and carbon nano-tube mixed solution; Electrophoretic preparation graphite oxide/carbon nano-tube/nickel electrode; Preparation graphene/carbon nano-tube/nickel electrode.The invention provides obtained graphene/carbon nano-tube/nickel electrode preparation method, graphite oxide/carbon nano-tube material is deposited directly on electrode slice, can save complicated coating process, and technique is simple and the time is short; The equivalent series resistance (ESR) of graphite oxide/carbon nano-tube/nickel electrode can be reduced simultaneously, thus the power density of more effective raising ultracapacitor.
Description
Technical field
The present invention relates to electrochemical material field, particularly relate to a kind of graphene/carbon nano-tube/nickel electrode, its preparation method and application.
Background technology
Strong K sea nurse (AndreK.Geim) of the peace moral of Univ Manchester UK etc. prepared grapheme material in 2004, paid attention to widely because the structure of its uniqueness and photoelectric property receive people.Mono-layer graphite due to its large specific area, excellent conduction, heat conductivility and low thermal coefficient of expansion and be considered to desirable material.As: 1, high strength, 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 connductivity character, the structural property of the nanoscale of large specific surface character and its monolayer two dimension, can be used as electrode material in ultracapacitor and lithium ion battery.
Be easy to occur to reunite and stacked because the two-dimensional structure of the monolayer of Graphene to lose in drying in the water process of interlayer in addition, curling or height fold, the utilance of its specific area is finally caused greatly to reduce, because carbon nano-tube and Graphene have a lot of similarity on stuctures and properties, therefore be inserted between graphene layer by carbon nano-tube, or the functional group in carbon nano-tube and the functional group on Graphene react mutually, carbon nano-tube is made to be grafted on graphenic surface, Graphene is separated from each other out between layers, the dried specific area of Graphene is improved to reach, Graphene is avoided to reunite and lamination, and then the object of the ratio capacitance of increase ultracapacitor.
The technique that tradition prepares electrode slice is comparatively complicated, and adds certain binding agent, increases the equivalent series resistance of electrode, affects the power density of ultracapacitor.
Summary of the invention
The object of the present invention is to provide graphene/carbon nano-tube/nickel electrode that a kind of equivalent series resistance is low, electric conductivity is high.
Graphene/carbon nano-tube/nickel electrode of the present invention is obtained by following processing step:
Step S1, the graphite oxide of mass ratio 1 ~ 2: 1 and carbon nano-tube added alcoholic solvent (as, ethanol, isopropyl alcohol, propyl alcohol) in, ultrasonic disperse 0.5 ~ 2h, subsequently stirring at room temperature 0.5 ~ 1h, obtain the mixed solution of homodisperse graphene oxide and carbon nano-tube;
Step S2, to add concentration to the mixed solution in step S1 be 0.2 ~ 0.5mg/ml magnesium nitrate (Mg (NO
3)
26H
2o), ultrasonic agitation 15 ~ 60min, in mixed solution, parallel insertion spacing is two nickel foil electrodes of 0.5-1cm subsequently, and adds 40 ~ 80V direct current between two electrodes, electrophoresis 5 ~ 20min, can obtain graphene oxide/carbon nano-tube/nickel electrode at negative pole;
After step S3, the graphene oxide/carbon nano-tube/nickel electrode obtained by step S2 are dried naturally, then in an inert atmosphere, at 400 ~ 800 DEG C calcination processing 3 ~ 8h, cooling, obtain described graphene/carbon nano-tube/nickel electrode.
In above-mentioned preparation method, in step 1, described graphite oxide adopts following steps to obtain:
Be that 50 order graphite powders of the purity 99.5% of 2: 1: 1, potassium peroxydisulfate and phosphorus pentoxide add in the concentrated sulfuric acid of 80 DEG C by mass ratio, stir, cooling more than 6h, washing is to neutral, dry; Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 230mL, add potassium permanganate (its quality consumption is 3 times of graphite powder) again, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water; After 15min, add 2.8L deionized water again, then add the hydrogen peroxide solution that 50mL concentration is 30wt%, mixture color becomes glassy yellow afterwards, suction filtration while hot, then carry out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 60 DEG C of vacuumize 48h.
Graphene/carbon nano-tube/nickel electrode that said method obtains can be applied in ultracapacitor, plays electrode effect.
The present invention obtains graphene/carbon nano-tube/nickel electrode, and tool has the following advantages:
(1) by graphite oxide and carbon nano-tube are dissolved in ultrasonic agitation in ethanol, then obtain Graphene by thermal reduction, can better carbon nano-tube be inserted between graphene sheet layer, play the effect of performance complement better;
(2) by the method for electro-deposition, graphite oxide/carbon nano-tube material is deposited directly on electrode slice, can save complicated coating process, and technique is simple and the time is short; The equivalent series resistance (ESR) of electrode can be reduced simultaneously, thus the power density of more effective raising ultracapacitor.
Accompanying drawing explanation
Fig. 1 is graphene/carbon nano-tube of the present invention/nickel electrode preparation technology flow chart;
Fig. 2 is the SEM figure of Graphene;
Fig. 3 is graphene/carbon nano-tube in embodiment 1/nickel electrode SEM figure.
Embodiment
Graphene/carbon nano-tube/nickel electrode of the present invention.First prepare the composite material of graphite oxide and carbon nano-tube, then this composite material is joined ultrasonic process in ethanol, then add Mg (NO in above-mentioned suspension
3)
26H
2o; ultrasonic to obtain uniform solution as electrolyte, using nickel foil as electrode, its Parallel Symmetric is placed in electrolyte; the direct current of 40-80V is added at the two ends of electrode; two die openings are 0.5cm, electrophoresis a period of time, just can obtain graphite oxide/carbon nano-tube/nickel electrode; naturally after drying; under argon shield, be slowly warming up to 400-800 DEG C of calcination 3-8h, take out after naturally cooling to room temperature, just can obtain graphene/carbon nano-tube/nickel electrode.
A preparation method for graphene/carbon nano-tube/nickel electrode, as shown in Figure 1, comprises the steps:
Step S1, the graphite oxide of mass ratio 1 ~ 2: 1 and carbon nano-tube added alcoholic solvent (as, ethanol, isopropyl alcohol, propyl alcohol) in, ultrasonic disperse 0.5 ~ 2h, subsequently stirring at room temperature 0.5 ~ 1h, obtain the mixed solution of homodisperse graphene oxide and carbon nano-tube;
Step S2, add to the mixed solution in step S1 the magnesium nitrate (Mg (NO that concentration is 0.2 ~ 0.5mg/ml
3)
26H
2o), ultrasonic agitation 15 ~ 60min, in mixed solution, parallel insertion spacing is two nickel foil electrodes of 0.5cm subsequently, and adds 40 ~ 80V direct current between two electrodes, electrophoresis 5 ~ 20min, obtains graphene oxide/carbon nano-tube/nickel electrode at negative pole;
After step S3, the graphene oxide/carbon nano-tube/nickel electrode obtained by step S2 are dried naturally, then in an inert atmosphere, at 400 ~ 800 DEG C calcination processing 3 ~ 8h, cooling, obtain described graphene/carbon nano-tube/nickel electrode.
In above-mentioned preparation method, in step S1, described graphite oxide adopts following steps to obtain:
Be that 50 order graphite powders of the purity 99.5% of 2: 1: 1, potassium peroxydisulfate and phosphorus pentoxide add in the concentrated sulfuric acid of 80 DEG C by mass ratio, stir, cooling more than 6h, washing is to neutral, dry; Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 230mL, add potassium permanganate (its quality consumption is 3 times of graphite powder) again, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water; After 15min, add 2.8L deionized water again, then add the hydrogen peroxide solution that 50mL concentration is 30wt%, mixture color becomes glassy yellow afterwards, suction filtration while hot, then carry out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 60 DEG C of vacuumize 48h.
The preparation method of a kind of graphene/carbon nano-tube/nickel electrode provided by the invention, tool has the following advantages:
(1) by graphite oxide and carbon nano-tube are dissolved in ultrasonic agitation in ethanol, then obtain Graphene by thermal reduction, can better carbon nano-tube be inserted between graphene sheet layer, play the effect of performance complement better;
(2) by the method for electro-deposition, graphite oxide/carbon nano-tube material is deposited directly on electrode slice, can save complicated coating process, and technique is simple and the time is short; The equivalent series resistance (ESR) of electrode can be reduced simultaneously, thus the power density of more effective raising ultracapacitor.
Below preferred embodiment of the present invention is described in further detail.
Embodiment 1
(1) 50 order graphite powders of 20g purity 99.5%, 10g potassium peroxydisulfate and 10g phosphorus pentoxide are added in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, washing is to neutral, dry; Dried sample is added 0 DEG C, in the concentrated sulfuric acid of 230mL, then add 60g potassium permanganate, the temperature of mixture remains on less than 20 DEG C, after then keeping 2h in the oil bath of 35 DEG C, slowly adds 920mL deionized water; After 15min, add 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, then carry out washing with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely obtain graphite oxide at 60 DEG C of vacuumize 48h
(2) graphite oxide and acid-treated carbon nano-tube are added in alcohol solvent with the ratio of mass ratio 1: 1, ultrasonic 0.5h, stirring at room temperature 0.5h, obtain homodisperse graphene oxide and carbon nano-tube mixed solution
(3) in (2) mixed solution, the Mg (NO that concentration is 0.5mg/ml is added
3)
26H
2o, ultrasonic 15min, to obtain uniform solution as electrolyte, using the nickel foil of 5cm diameter as electrode, its Parallel Symmetric is placed in electrolyte, adds the direct current of 40V at the two ends of electrode, two die openings are 0.5cm, electrophoresis 5min, just can obtain graphene oxide/carbon nano-tube/nickel electrode;
(4), after the graphene oxide/carbon nano-tube/nickel electrode of (3) gained being dried naturally, under argon shield, be slowly warming up to 400 DEG C of calcination 8h, take out after naturally cooling to room temperature, just can obtain graphene/carbon nano-tube/nickel electrode.
As shown in Figures 2 and 3, comparison chart 2 and Fig. 3, can observe from the electrode surface Fig. 3, and Graphene is kept apart by carbon nano-tube is well-proportioned, and the phenomenon of lamination or reunion does not occur, and substrate have also been obtained good covering.
Embodiment 2
(1) identical with (1) in embodiment 1;
(2) graphene oxide and acid-treated carbon nano-tube are added in isopropanol solvent with the ratio of mass ratio 1: 1, ultrasonic 2h, stirring at room temperature 1h, obtain homodisperse graphene oxide and carbon nano-tube mixed solution;
(3) in (2) mixed solution, the Mg (NO that concentration is 0.2mg/ml is added
3)
26H
2o, ultrasonic 15min, to obtain uniform solution as electrolyte, using the nickel foil of 5cm diameter as electrode, be placed in electrolyte by its Parallel Symmetric, add the direct current of 80V at the two ends of electrode, two die openings are 0.5cm, electrophoresis 20min, just can obtain graphene oxide/carbon nano-tube/nickel electrode;
(4), after the graphene oxide/carbon nano-tube/nickel electrode of (3) gained being dried naturally, under argon shield, be slowly warming up to 800 DEG C of calcination 3h, take out after naturally cooling to room temperature, just can obtain graphene/carbon nano-tube/nickel electrode.
Embodiment 3
(1) identical with (1) in embodiment 1;
(2) graphite oxide and acid-treated carbon nano-tube are added in propanol solvent with the ratio of mass ratio 2: 1, ultrasonic 1h, stirring at room temperature 1h, obtain homodisperse graphene oxide and carbon nano-tube solution;
(3) in (2) mixed solution, the Mg (NO that concentration is 0.3mg/ml is added
3)
26H
2o, ultrasonic 15min, to obtain uniform solution as electrolyte, using the nickel foil of 5cm diameter as electrode, be placed in electrolyte by its Parallel Symmetric, add the direct current of 60V at the two ends of electrode, two die openings are 0.5cm, electrophoresis 20min, just can obtain graphene oxide/carbon nano-tube/nickel electrode;
(4), after the graphene oxide/carbon nano-tube/nickel electrode of (3) gained being dried naturally, under argon shield, be slowly warming up to 600 DEG C of calcination 5h, take out after naturally cooling to room temperature, just can obtain graphene/carbon nano-tube/nickel electrode.
Should be understood that, the above-mentioned statement for present pre-ferred embodiments is comparatively detailed, and therefore can not 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 claims.
Claims (7)
1. comprise a combination electrode for Graphene, carbon nano-tube and nickel, it is characterized in that, this combination electrode is adopted and is obtained with the following method:
S11, add in alcoholic solvent by the graphite oxide of mass ratio 1 ~ 2:1 and carbon nano-tube, ultrasonic disperse, obtains the mixed solution of graphene oxide and carbon nano-tube;
S12, add magnesium nitrate solution to the mixed solution in step S11, stir, parallel insertion two nickel foil electrodes in mixed solution subsequently, and add the direct current of 40 ~ 80V between two electrodes, carry out electrophoresis reaction, can obtain graphene oxide/carbon nano-tube/nickel electrode at negative pole, the concentration of magnesium nitrate is 0.2 ~ 0.5mg/ml, and the spacing between two electrodes is 0.5cm;
After S13, the graphene oxide/carbon nano-tube/nickel electrode obtained by step S12 are dried, then in an inert atmosphere, at 400 ~ 800 DEG C calcination processing 3 ~ 8h, cooling, obtain described graphene/carbon nano-tube/nickel electrode.
2. comprise a preparation method for the combination electrode of Graphene, carbon nano-tube and nickel, it is characterized in that, this preparation method comprises the steps:
S21, add in alcoholic solvent by the graphite oxide of mass ratio 1 ~ 2:1 and carbon nano-tube, ultrasonic disperse, obtains the mixed solution of graphene oxide and carbon nano-tube;
S22, add magnesium nitrate solution to the mixed solution in step S21, stir, parallel insertion two nickel foil electrodes in mixed solution subsequently, and add direct current between two electrodes, carry out electrophoresis reaction, can obtain at negative pole the combination electrode comprising graphene oxide, carbon nano-tube and nickel, the concentration of magnesium nitrate is 0.2 ~ 0.5mg/ml, and the spacing between two electrodes is 0.5cm;
After S23, the combination electrode comprising graphene oxide, carbon nano-tube and nickel obtained by step S22 dry, then in an inert atmosphere, calcination processing 3 ~ 8h at 400 ~ 800 DEG C, cooling, comprises the combination electrode of Graphene, carbon nano-tube and nickel described in obtaining.
3. preparation method according to claim 2, is characterized in that, in step S21, described graphite oxide adopts following steps to obtain:
S211, be the graphite powder of 2:1:1 by mass ratio, potassium peroxydisulfate and phosphorus pentoxide add in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, washing is to neutral, dry, obtains mixture;
S212, the mixture obtained by step S211 join in the concentrated sulfuric acid of 0 DEG C, add potassium permanganate again, and in the oil bath of 35 DEG C after insulation reaction 2h, slowly add deionized water, add the hydrogen peroxide solution that concentration is 30wt% subsequently, then carry out suction filtration, washing, again suction filtration and dry process, namely obtain graphite oxide.
4. preparation method according to claim 3, is characterized in that, the mass ratio of described graphite powder and potassium permanganate is 1:3.
5. preparation method according to claim 2, is characterized in that, described alcoholic solvent is at least one in ethanol, isopropyl alcohol or propyl alcohol.
6. preparation method according to claim 2, is characterized in that, in described step S22, described galvanic voltage is 40 ~ 80V.
7. the combination electrode material comprising Graphene, carbon nano-tube and nickel as claimed in claim 1 in ultracapacitor or lithium ion battery as the application of electrode material.
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