CN108987119A - A kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material and preparation method and application - Google Patents
A kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material and preparation method and application Download PDFInfo
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- CN108987119A CN108987119A CN201810709900.1A CN201810709900A CN108987119A CN 108987119 A CN108987119 A CN 108987119A CN 201810709900 A CN201810709900 A CN 201810709900A CN 108987119 A CN108987119 A CN 108987119A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
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- 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
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- H01G11/46—Metal oxides
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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Abstract
The invention discloses a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite materials, it is mixed by Dopamine hydrochloride and carbon nanotube, first through carbonization treatment, obtain the carbon nanotube that there is poly-dopamine to modify, then it mixes with cobalt nitrate, nickel nitrate through sodium borohydride reduction, is finally again heat-treated mixture.Preparation method includes: 1) poly-dopamine-carbon nanotube preparation；2) poly-dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder preparation；3) poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material preparation.As electrode material for super capacitor, the charge and discharge in -0.1-0.45V range, when discharge current density is 1A/g, specific capacitance can achieve 900-1000F/g.The present invention uses carbonizatin method and hydro-thermal method, simple process；Using the carbon nanotube of poly-dopamine modification as skeleton, big specific surface area is provided, there are excellent electrochemical properties and chemical stability.
Description
Technical field
The present invention relates to supercapacitor technologies fields, and in particular to a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide
Composite material and preparation method and application.
Background technique
Supercapacitor is a kind of novel energy storage apparatus, it has, and power density is high, the charging time is short, long service life,
Good temp characteristic, it is energy saving and environmentally protective the features such as.Supercapacitor is between traditional physical capacitor and battery
A kind of preferable energy-storage travelling wave tube, huge superiority show themselves in that (1) power density height.The internal resistance very little of supercapacitor,
And fast storage and the release of charge are able to achieve in Cathode/Solution Interface and electrode material ontology.(2) charge and discharge cycles
Service life is long.There is no electrochemical reactions in charge and discharge process for supercapacitor, and cycle life is up to ten thousand times or more.(3)
Charging time is short.Fully charged several minutes of need.(4) high-specific-power and high-energy-density output are realized.(5) environment temperature is to normal
It is little using influencing.The normal working temperature range of supercapacitor is at -35-75 DEG C.
Carbon material is smaller separately as electrode material for super capacitor specific capacitance, and transition metal oxide is separately as super
Capacitor electrode material compact structure, electric conductivity is poor, with the biggish gold of the compound specific capacitance of the preferable carbon materials of electric conductivity
Belong to oxide, thus very good solution carbon electrode material smaller, mistake of comparing with metal oxide electrode material specific capacitance
Metal oxide is crossed separately as electrode material for super capacitor compact structure, is unfavorable for the infiltration of electrolyte, electric conductivity compared with
The problem of difference.
Dopamine not only has strong adhesion but also is rich in various functional groups as a kind of Biosilica-adhesive protein, can be in difference
Material surface, which further reacts, forms functional layer, to realize the functional modification to material surface.Contain in poly-dopamine structure
There are a large amount of-OH and-NH2, it is good second order reaction platform.On the one hand, these groups can be used for graft reaction；Another party
Face, these groups can effectively absorb metal ion, in addition poly-dopamine itself has weak reproducibility, can by noble metal from
For sub- solution reduction at noble metal nano particles (MNPs), the poly-dopamine sensor preparation of your MNPs modification is simple, sensitive efficient.
Simultaneously as poly-dopamine has oxidation reaction selectivity, the carbosphere made based on poly-dopamine is under alkaline environment
More porous, large specific surface area is suitble to do the electrode material of supercapacitor.
Summary of the invention
The object of the present invention is to provide a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material and its preparation sides
Method and application in supercapacitor field.
It is aggregated in the surface of carbon nanotube using the excellent adhesiveness and auto polymerization performance of dopamine, passes through pyrocarbon
Change processing, then restores to obtain Co and Ni using the effect of the week reduction of poly-dopamine and reducing agent；Co and Ni be again later
CoO and NiO are oxidized by the oxygen in the oxygen or air that contain in material.
The carbon nanometer micro ball obtained after poly-dopamine carbonization has preferably conductive capability, and the C atom of poly-dopamine is in ring
It is inside easier to be converted to Sp2C；The high doped of the reduction of Sp3 and electroactive N make carbon ball have lower impedance.
Therefore, obtained composite material not only shows the electric double layer capacitance performance of porous carbon, but also shows metal
Faraday's capacitive property of oxide, thus there is the superperformance of the electrode material as supercapacitor.One side carbon is received
The carbon of mitron, N doping has good electric conductivity, can provide high electric double layer capacitance；The presence of another aspect CoO, NiO
The electric conductivity of composite material is improved, volume of the oxide in the corrosion and charge and discharge process of electrolyte has effectively been restrained and has received
Contracting, effectively increases composite material specific capacitance, and the carbosphere made based on poly-dopamine is more porous under alkaline environment,
Large specific surface area is the electrode material for the supercapacitor that production is had excellent performance.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention are as follows:
A kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material is mixed by Dopamine hydrochloride and carbon nanotube, is first passed through
Carbonization treatment, obtains the carbon nanotube that there is poly-dopamine to modify, and the polymer with nitrogen is poly-dopamine, the poly- DOPA
In amine/carbon nanotube@cobalt-nickel oxide composite material, carbon shell is N doping.
A kind of preparation method of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material the following steps are included:
The preparation of step 1) poly-dopamine-carbon nanotube meets mass ratio with Dopamine hydrochloride and carbon nanotube for 5 ~ 10:1, incites somebody to action
Dopamine hydrochloride and carbon nanotube addition are dissolved in 0.01mol/L trimethylamino methane buffer solution, under the conditions of 25-30 DEG C
20-30min is stirred, then assisting ultrasonic reacts 30min again, 10h is reacted under dark condition, by drying, crushing, grinding,
Finally under a nitrogen atmosphere, with 5-10 DEG C/min of heating rate, 600 ~ 900 DEG C is warming up to and is calcined, 2-3h is then kept the temperature, obtains
To poly-dopamine-carbon nanotube；
Step 2 poly-dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder preparation will be walked with certain mass ratio for 5 ~ 10:1
Rapid 1) gained poly-dopamine-first ultrasound the 30min of carbon nanotube powder, is then mixed with cobalt nitrate, nickel nitrate, second alcohol and water
It closes, stirs 1-2h；Then the sodium borohydride solution that concentration is 2.6 ~ 5.2mol/L is added dropwise, stirs 30-60min, finally drying, powder
Broken, grinding, obtains poly-dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder；
The preparation of step 3) poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, the poly-dopamine-that step 2 is obtained
Carbon nanotube-cobalt nitrate-nickel nitrate powder with 5-10 DEG C/min of heating rate, is warming up to 250- under a nitrogen atmosphere
300 DEG C are calcined, and then keep the temperature 2-3h calcining, poly-dopamine/carbon nanotube@cobalt nickel oxygen of poly-dopamine modification can be obtained
Compound composite material.
A kind of poly-dopamine/application of the carbon nanotube@cobalt-nickel oxide composite material as electrode material for super capacitor,
The charge and discharge in -0.1-0.45V range, when discharge current density is 1A/g, specific capacitance can achieve 900 1000F/g.
A kind of poly-dopamine of the invention/carbon nanotube@cobalt-nickel oxide composite material through experimental tests is as a result as follows:
A kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material is through transmissioning electric mirror test, and CoO, NiO nanoparticle are very
Good is supported on Nano carbon balls.
A kind of electrochemical property test of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material is detected in -0.1-
Charge and discharge within the scope of 0.45V, when discharge current density is 1A/g, a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide is compound
Material electrode of super capacitor specific capacitance range is in 900 ~ 1000F/g.
And the specific capacitance of the carbon material without CoO and NiO of poly-dopamine preparation is used merely for 100-200F/g, in phase
With under current density, a kind of discharge time of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material material is apparently higher than single
Poly-dopamine carbon porous carbon electrode material, discharge time improves shows the more single porous carbon of its specific capacitance more 8 times
Performance is obviously improved, and shows that a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material has good super electricity
Capacitive energy.
Therefore, a kind of poly-dopamine of the invention/carbon nanotube@cobalt-nickel oxide composite material is for the prior art, tool
It has the advantage that
1. preparation method is simple, a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite wood is achieved with using hydro-thermal method
Material, and Dopamine hydrochloride is widely used, it is cheap, it is a kind of environmentally friendly reagent；
2. the present invention uses the mixing of poly-dopamine-carbon nanotube, the excellent adhesiveness and auto polymerization performance of poly-dopamine
It can be very good to load to carbon nano tube surface；
3. resulting poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, the carbon nanometer obtained after poly-dopamine carbonization is micro-
Ball has preferably conductive capability, effectively increases the electric conductivity of material；
4. resulting poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, CoO and NiO are carried on Nano carbon balls, and one
Aspect improves the electric conductivity of material, on the other hand prevents the volume contraction in the corrosion and charge and discharge process of CoO and NiO.
Therefore, the present invention has broad application prospects in supercapacitor field.
Detailed description of the invention:
Fig. 1 is poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material scanning electron microscope (SEM) photograph of preparation of the embodiment of the present invention；
Fig. 2 is poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material transmission electron microscope picture of preparation of the embodiment of the present invention；
Fig. 3 is that poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material high-resolution of preparation of the embodiment of the present invention transmits electricity
Mirror figure；
Fig. 4 is pair of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material discharge curve of preparation of the embodiment of the present invention
Than figure.
Specific embodiment
The present invention is described in further detail the content of present invention in conjunction with Figure of description, but be not pair by embodiment
Restriction of the invention.
Embodiment
A kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material:
Step 1) poly-dopamine-carbon nanotube preparation, under the conditions of magnetic agitation, by 2.4g Dopamine hydrochloride and 0.24g carbon
Nanotube addition is dissolved in 0.01mol/L trimethylamino methane buffer solution, and NH is added dropwise3▪H2PH value is adjusted to by O
8.5,30min is stirred, then assisting ultrasonic reacts 30min again, 10h is reacted under dark condition, by drying, crushing, grinding,
Finally under a nitrogen atmosphere, with 5 DEG C/min of heating rate, 600 DEG C is warming up to and is calcined, 2h is then kept the temperature, obtains poly- DOPA
Amine-carbon nanotube；
Step 2 poly-dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder preparation, by 0.5g by poly- DOPA obtained by step 1)
The first ultrasound 30min of amine-carbon nanotube powder, is then dissolved in 20ml ethyl alcohol for 3g cobalt nitrate, 1.5g nickel nitrate and 100ml water carries out
1h is stirred in mixing；Then the sodium borohydride solution that dropwise addition concentration is 5.2mol/L stirs 30min, finally then dry, crush,
Grinding, obtains poly-dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder；
The preparation of step 3) poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, the poly-dopamine-that step 2 is obtained
Carbon nanotube-cobalt nitrate-nitric acid nickel by powder is put into tube furnace, under a nitrogen atmosphere, with 5 DEG C/min of heating rate, is warming up to 300
It DEG C is calcined, then keeps the temperature 2h calcining, poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material can be obtained.
Poly-dopamine/carbon nanotube cobalt-nickel oxide composite material is through microscopic appearance Fig. 1 obtained by sem test and thoroughly
Shown in radio mirror Fig. 2.As can be seen from the figure spherical nanoparticles generate.High-resolution-ration transmission electric-lens Fig. 3 can be seen that carbon nanometer
The dispersion of pipe@cobalt nickel bimetal oxide is more uniform.
In order to verify the remarkable effect that CoO and NiO promote material property, according to above-mentioned poly-dopamine/carbon nanotube@cobalt
The identical preparation method of nickel oxide composite material is prepared for the carbon material without CoO and NiO, not specified step with it is upper
It is identical to state preparation method, the difference is that: the step 2 does not add cobalt nitrate, nickel nitrate, cannot get poly-dopamine/carbon and receives
Mitron@cobalt-nickel oxide composite material.
Poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material electrochemical property test, method particularly includes: it weighs
0.008g poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, 0.001g acetylene black and 0.001g polytetrafluoroethylene (PTFE) are micro-
Powder is placed in small agate and grinds in alms bowl, and 0.5mL ethyl alcohol is added and is ground；With the pressure of 10kPa by after grinding sample and 1mm it is thick
Foamed nickel current collector compacting, dry in air, at room temperature, cut into 2cm × 2cm, be made electrode of super capacitor, test
Its specific capacitance.
Testing result is as shown in Figure 4, it is known that: the charge and discharge in -0.1-0.45V range are 1A/g in discharge current density
When, poly-dopamine/carbon nanotube@cobalt-nickel oxide composite supercapacitor electrode specific capacitance can achieve 944F/g, and
The specific capacitance for the porous carbon materials without CoO and NiO for using poly-dopamine to prepare merely is 134F/g.In same current density
Under, poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material discharge time is apparently higher than single carbon electrode material,
Discharge time improves shows that the performance of the more single porous carbon of its specific capacitance is obviously improved more 7 times, show poly- DOPA
Amine/carbon nanotube cobalt-nickel oxide composite material has good super capacitor performance.
Claims (9)
1. a kind of poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, it is characterised in that: received by Dopamine hydrochloride and carbon
Mitron mixing obtains the carbon nanotube that there is poly-dopamine to modify, then by itself and cobalt nitrate, nickel nitrate first through carbonization treatment
Mixture is finally heat-treated to obtain N doping porous carbon Supported Co nickel bimetal oxide by mixing again through sodium borohydride reduction.
2. poly-dopamine according to claim 1/carbon nanotube@cobalt-nickel oxide composite material, it is characterised in that: described
Polymer with nitrogen be micron spherical shape grain structure.
3. poly-dopamine according to claim 1/carbon nanotube@cobalt-nickel oxide composite material, it is characterised in that: described
Cobalt nickel bimetal oxide be nano-lamellar structure.
4. poly-dopamine according to claim 1/carbon nanotube@cobalt-nickel oxide composite material, it is characterised in that: carbon is received
The carbon-coated tubulose carbon of mitron and N doping is to be carbonized to synthesize by a step.
5. poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material preparation method according to claim 1, feature
Be the following steps are included:
The preparation of step 1) poly-dopamine-carbon nanotube meets certain mass ratio with Dopamine hydrochloride and carbon nanotube, by hydrochloric acid
Dopamine and carbon nanotube addition is dissolved in trimethylamino methane buffer solution, under certain condition react and by drying,
The processing such as crushing, grinding, finally calcining obtains poly-dopamine-carbon nanotube under certain condition；
Step 2 poly-dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder preparation will be obtained by step 1) with certain mass ratio
The first ultrasound 30min of poly-dopamine-carbon nanotube powder, is then sufficiently mixed with cobalt nitrate, nickel nitrate, second alcohol and water, is stirred
Mix 1-2h；Then certain density sodium borohydride solution is added dropwise, stirs 30-60min, finally dries, crush, grinding, being gathered
Dopamine-carbon nanotube-cobalt nitrate-nitric acid nickel by powder；
The preparation of step 3) poly-dopamine/carbon nanotube@cobalt-nickel oxide composite material, the poly-dopamine-that step 2 is obtained
Carbon nanotube-cobalt nitrate-nitric acid nickel by powder, is calcined under certain condition, and poly-dopamine/carbon of poly-dopamine modification can be obtained
Nanotube@cobalt-nickel oxide composite material.
6. preparation method according to claim 6, it is characterised in that: the matter of the step 1) poly-dopamine and carbon nanotube
For amount than being 5 ~ 10:1, the reaction condition of the step 1) is under agitation, the trimethylamino first of 0.01mol/L to be added
Alkane buffer solution, is added dropwise NH3▪H2PH value is adjusted to 8.5-9.0 by O, and temperature is maintained at 25-30 DEG C, reacts 30-60min, so
Assisting ultrasonic reacts 20-30min again afterwards, and 10h is reacted under dark condition, and calcination condition is under a nitrogen atmosphere, with the speed that heats up
5-10 DEG C of rate/min is warming up to 600-900 DEG C and is calcined, then keeps the temperature 2-3h.
7. preparation method according to claim 6, it is characterised in that: the poly-dopamine of the step 2, carbon nanotube, nitre
Sour cobalt, nickel nitrate, sodium borohydride, second alcohol and water mass ratio: 5 ~ 10:1:3:1.5:0.5 ~ 1:0.01 ~ 0.02:0.1.
8. preparation method according to claim 6, it is characterised in that: the calcination condition of the step 3) is in condition of nitrogen gas
Under, with 5-10 DEG C/min of heating rate, it is warming up to 250-300 DEG C and is calcined, then keep the temperature 2-3h.
9. poly-dopamine according to claim 1/carbon nanotube@cobalt-nickel oxide composite material is as super capacitor electrode
The application of pole material, it is characterised in that: the charge and discharge in -0.1-0.45V range, when discharge current density is 1A/g, than electricity
Appearance can achieve 900-1000F/g.
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| CN109734136A (en) * | 2019-02-08 | 2019-05-10 | 桂林理工大学 | Variety classes precipitating reagent prepares the method and application of cobalt nickel bimetal oxide |
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