CN107195465A - A kind of carbon quantum dot cobaltosic oxide combination electrode material and preparation method thereof - Google Patents
A kind of carbon quantum dot cobaltosic oxide combination electrode material and preparation method thereof Download PDFInfo
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- CN107195465A CN107195465A CN201710405473.3A CN201710405473A CN107195465A CN 107195465 A CN107195465 A CN 107195465A CN 201710405473 A CN201710405473 A CN 201710405473A CN 107195465 A CN107195465 A CN 107195465A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007772 electrode material Substances 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 64
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 64
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 32
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 24
- 239000010935 stainless steel Substances 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004202 carbamide Substances 0.000 claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 13
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960004543 anhydrous citric acid Drugs 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 57
- 229910052799 carbon Inorganic materials 0.000 claims description 47
- 239000002131 composite material Substances 0.000 claims description 44
- 229910017052 cobalt Inorganic materials 0.000 claims description 19
- 239000010941 cobalt Substances 0.000 claims description 19
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 239000011574 phosphorus Substances 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 4
- 244000025254 Cannabis sativa Species 0.000 claims description 3
- 235000007516 Chrysanthemum Nutrition 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 244000189548 Chrysanthemum x morifolium Species 0.000 claims 1
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 abstract description 10
- 150000001868 cobalt Chemical class 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 36
- 235000019441 ethanol Nutrition 0.000 description 26
- 239000006260 foam Substances 0.000 description 18
- 229910052759 nickel Inorganic materials 0.000 description 18
- 239000003643 water by type Substances 0.000 description 18
- 239000003990 capacitor Substances 0.000 description 17
- 239000000126 substance Substances 0.000 description 17
- 235000013495 cobalt Nutrition 0.000 description 15
- 239000003792 electrolyte Substances 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 230000008859 change Effects 0.000 description 10
- 235000015165 citric acid Nutrition 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 9
- 239000006230 acetylene black Substances 0.000 description 9
- 239000011149 active material Substances 0.000 description 9
- 150000002171 ethylene diamines Chemical class 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 230000014759 maintenance of location Effects 0.000 description 9
- 239000002086 nanomaterial Substances 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 9
- 230000004044 response Effects 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 241000723353 Chrysanthemum Species 0.000 description 2
- 229960004106 citric acid Drugs 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- MGPYDQFQAJEDIG-UHFFFAOYSA-N ethene;urea Chemical compound C=C.NC(N)=O MGPYDQFQAJEDIG-UHFFFAOYSA-N 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
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- Microelectronics & Electronic Packaging (AREA)
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Abstract
The invention discloses a kind of carbon quantum dot cobaltosic oxide combination electrode material and preparation method thereof.Comprise the following steps that：Anhydrous citric acid, ethylenediamine, phosphorus pentoxide and water are well mixed first, then carry out in polytetrafluoroethylene (PTFE) stainless steel cauldron hydro-thermal reaction；Water formation clear solution is added after reaction solution cooling, it is standby that centrifuge washing and vacuum drying obtain carbon quantum dot；Then the carbon quantum dot of synthesis, cobalt salt and urea are dissolved in ethanol；Hydro-thermal reaction is carried out in polytetrafluoroethylene (PTFE) stainless steel cauldron；Last centrifuge washing is simultaneously drying to obtain carbon quantum dot cobaltosic oxide combination electrode material.The pattern of carbon quantum dot cobaltosic oxide combination electrode material prepared by the present invention can be controlled by Auto-regulator proportioning and hydrothermal condition, and it has preferable cyclical stability, excellent electrochemical performance.
Description
Technical field
The present invention relates to electrode material for super capacitor technical field, and in particular to a kind of carbon quantum dot-cobaltosic oxide
Combination electrode material and preparation method thereof.
Background technology
Relatively conventional capacitor and battery, ultracapacitor have higher energy density, longer cycle life, quickly
Charge-discharge velocity, wider potential windowses etc..These advantages make it in portable electric appts, hybrid-power electric vehicle, laser
Weapon, the field such as energy stores has latency development ability.Ultracapacitor can be divided into double according to the difference of its Ultrahigh
Electric layer ultracapacitor and Faradic pseudo-capacitor (fake capacitance capacitor).Electrical double layer capacitor electrodes mainly include carbon material,
Faradic pseudo-capacitor electrode is included such as metal material, and it is bimetallic oxide or hydroxide that current people, which study hotter,
The composite of metal and carbon material, and metal and polymer composite.
2006, scientist Chinese descendant in America professor Sun Yaping of Clemson University of the U.S. developed New Type of Carbon nanometer first
Material-carbon quantum dot, based on its superior function, countries in the world researcher is put among the exploration to carbon quantum dot.Make
For the rising star of carbon nanomaterial family, carbon quantum dot is a kind of almost spherical, scattered, size is less than 10nm, environment friend
The semiconductor nanocrystal particle of good type, these excellent properties make carbon quantum dot in life medical science, materials chemistry, analysis detection
It is widely used Deng field, and the research that carbon quantum dot is applied in terms of electrochemical energy storage is less, from 2013 years,
People begin attempt to prepare carbon quantum dot/RuO2, carbon quantum dot/polyaniline, carbon quantum dot/graphene composite material simultaneously probes into it
Chemical property, these reports find that carbon quantum dot can be that good contact interface is provided between electrolyte and electrode, so that
Improve the specific capacitance for improving electrode material, improve ratio performance and cyclical stability.It is used as one of transition metal oxide, four oxygen
Change three cobalts has potential application in fields such as catalysis, electrochemistry, sensor and solar cells, by wide concern,
Also possess good chemical property, Co in terms of ultracapacitor3O4With high theoretical capacity, aboundresources, it is environment-friendly,
Cheap the advantages of.
The content of the invention
It is an object of the invention to provide a kind of carbon quantum dot-cobaltosic oxide combination electrode material and preparation method thereof；This
Invention is combined the carbon quantum dot of nitrogen-containing group with cobaltosic oxide, can improve chemical property.Present invention process is simple, operation
It is convenient；The combination electrode material morphology controllable of preparation, is uniformly dispersed.
Technical scheme is specifically described as follows.
The present invention provides a kind of preparation method of carbon quantum dot-cobaltosic oxide combination electrode material, comprises the following steps that:
(1) carbon quantum dot of N doping is synthesized
Ethylenediamine, anhydrous citric acid, phosphorus pentoxide and water are added in polytetrafluoroethylene (PTFE) stainless steel cauldron and carried out
Hydro-thermal reaction；After reaction terminates, room temperature is cooled to, deionized water formation clear solution is added, adds absolute ethyl alcohol and centrifuged
Washing, obtains carbon quantum dot；
(2) carbon quantum dot-cobaltosic oxide composite material is synthesized
Mixed liquor after ultrasonic mixing is uniform in water, is transferred to polytetrafluoro by soluble cobalt, carbon quantum dot and urea
Ethene stainless steel cauldron carries out hydro-thermal reaction；After reaction terminates, centrifuge, wash, being drying to obtain carbon quantum dot-cobaltosic oxide
Composite.
It is preferred that, in step (1), anhydrous citric acid, ethylenediamine, phosphorus pentoxide and deionized water mass ratio for (1~
2):(2~5):(2~6):1.
It is preferred that, in step (1), hydrothermal temperature is 80~150 DEG C, and the hydro-thermal reaction time is 2~8h.
It is preferred that, in step (2), soluble cobalt is nitrate, sulfate, one kind in acetate and hydrochloride.
It is preferred that, in step (2), the molar concentration of soluble cobalt is 1~3mol/L.
It is preferred that, in step (2), the mol ratio of soluble cobalt and urea is 1:1~1:5；The quality of carbon quantum dot is
The 1.5%~4.5% of soluble cobalt quality.
It is preferred that, in step (2), hydrothermal temperature is 100~160 DEG C, and the hydro-thermal reaction time is 12~20h.
The present invention also provides carbon quantum dot-cobaltosic oxide composite material prepared by a kind of preparation method described above.It is excellent
Choosing, it is chrysanthemum shape space structure, circular flower-shaped, intensive flower-shaped or elongated blade of grass shape and globular combination.
Compared to the prior art, the beneficial effects of the present invention are：
The present invention chooses cheap citric acid as raw material, nontoxic using simple hydro-thermal method synthesizing environment-friendly first
The carbon quantum dot of nitrogen modification, then with resourceful cobalt salt, urea is mixed with the composite wood of carbon quantum dot-cobaltosic oxide
Material, wherein the zero-dimension nano structure carbon quantum dot modified through nitrogen not only has a higher specific surface area, and can for electrode and
Interfacial reaction between electrolyte provides fabulous avtive spot, promotes ion diffusion and improves charge-transfer dynamics, realizes
Efficiently utilize, so that electrode material shows more preferable chemical property；In addition, carbon quantum dot can strengthen cobaltosic oxide
Dispersing uniformity, reduce cobaltosic oxide reunion, strengthen cyclical stability；Relative to other carbon materials, carbon quantum dot
Zero-dimension nano structure allows it more neatly to build various structures, can be preferably by the addition for regulating and controlling carbon quantum dot
Control the pattern of cobaltosic oxide；It is easy to operate from simple hydro-thermal method；The composite excellent electrochemical performance of preparation.
Brief description of the drawings
Fig. 1:A is the ESEM of carbon quantum dot-cobaltosic oxide composite nano materials prepared by the embodiment of the present invention 1
Figure；B is that carbon quantum dot-cobaltosic oxide composite nano materials prepared by the embodiment of the present invention 1 are prepared into electrode of super capacitor,
It circulates the cycle performance figure after 2000 circles.
Fig. 2 is the scanning electron microscope (SEM) photograph of carbon quantum dot-cobaltosic oxide composite nano materials prepared by the embodiment of the present invention 2.
Fig. 3 is the scanning electron microscope (SEM) photograph of carbon quantum dot-cobaltosic oxide composite nano materials prepared by the embodiment of the present invention 3.
Fig. 4 is the scanning electron microscope (SEM) photograph of carbon quantum dot-cobaltosic oxide composite nano materials prepared by the embodiment of the present invention 4.
Fig. 5 is that carbon quantum dot-cobaltosic oxide composite nano materials prepared by the embodiment of the present invention 5 are prepared into super capacitor
Device electrode, determines its circulation volt in the case where sweep speed is 5mv/s, 10mv/s, 20mv/s, 40mv/s, 50mv/s, 100mv/s
Antu.
Embodiment
Technical scheme is described in detail with reference to the accompanying drawings and examples.
Embodiment 1
Synthesize the carbon quantum dot of N doping：500 μ L (0.45g) ethylenediamines are added under room temperature condition anhydrous containing 0.2g
In the mixed liquor of citric acid and 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters are added
And hydro-thermal reaction 3h at 120 DEG C is sealed in, then it is cooled to room temperature and adds 10mL deionized waters formation clear solution, is added
Absolute ethyl alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.01mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
The carbon quantum dot prepared in the present embodiment-cobaltosic oxide composite material sample, its scanning electron microscope (SEM) photograph is figure
1a, shows chrysanthemum shape space structure；When being prepared into electrode of super capacitor, obvious faraday's redox reaction is showed；
0.5A g-1When, specific capacitance is 1387.5F g-1；Its cycle performance for circulating after 2000 circles is shown in Fig. 1 b, and capacity retention is
97.6%.
Embodiment 2
Synthesize the carbon quantum dot of N doping：500 μ L ethylenediamines are added to containing 0.1g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 3h at 120 DEG C, is then cooled to room temperature and adds 10mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.01mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Fig. 2 is that carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained obtains scanning electron microscope (SEM) photograph, it is seen that its pattern
For elongated blade of grass shape and globular combination；When being prepared into electrode of super capacitor, in 0.5A g-1When, specific capacitance is 1037.6F
g-1；Its capacity retention for circulating after 2000 circles is 90.5%.
Embodiment 3
Synthesize the carbon quantum dot of N doping：500 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 6h at 100 DEG C, is then cooled to room temperature and adds 10mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.01mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Fig. 3 is that carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained obtains scanning electron microscope (SEM) photograph, it is seen that its pattern
To be intensive flower-shaped；When being prepared into electrode of super capacitor, in 0.5A g-1When, specific capacitance is 1158.9F g-1；It circulates 2000
Capacity retention is 88.3% after circle.
Embodiment 4
Synthesize the carbon quantum dot of N doping：500 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 3h at 120 DEG C, is then cooled to room temperature and adds 10mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 20mg carbon quantum dot,
0.01mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Fig. 4 is that carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained obtains scanning electron microscope (SEM) photograph, it is seen that its pattern
It is flower-shaped for circle；When being prepared into electrode of super capacitor, in 0.5A g-1When, specific capacitance is 859.4F g-1；It circulates 2000 and enclosed
Capacity retention afterwards is 96.8%.
Embodiment 5
Synthesize the carbon quantum dot of N doping：500 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 3h at 110 DEG C, is then cooled to room temperature and adds 5mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.01mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Fig. 5 works as carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained is prepared into electrode of super capacitor,
Its cyclic voltammogram in the case where sweep speed is 5mv/s, 10mv/s, 20mv/s, 40mv/s, 50mv/s, 100mv/s is determined,
Under 100mv/s, obvious redox peaks are still showed, show preferable high rate performance.In 0.5A g-1When, specific capacitance is
1096.0F g-1；Its capacity retention for circulating after 2000 circles is 91.6%.
Embodiment 6
Synthesize the carbon quantum dot of N doping：500 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 5h at 120 DEG C, is then cooled to room temperature and adds 10mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.006mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained is surveyed when being prepared into electrode of super capacitor
Its fixed chemical property：In 0.5A g-1When, specific capacitance is 853.7F g-1；Its circulate 2000 circle after capacity retention be
87.2%.
Embodiment 7
Synthesize the carbon quantum dot of N doping：300 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 3h at 120 DEG C, is then cooled to room temperature and adds 10mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.01mol urea is mixed and added into 30mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
140 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained is surveyed when being prepared into electrode of super capacitor
Its fixed chemical property：In 0.5A g-1When, specific capacitance is 906.8F g-1；Its circulate 2000 circle after capacity retention be
77.8%.
Embodiment 8
Synthesize the carbon quantum dot of N doping：500 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.4g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 1mL deionized waters is added and seals
The hydro-thermal reaction 6h at 100 DEG C, is then cooled to room temperature and adds 10mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 40mg carbon quantum dot,
0.015mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
140 DEG C of heating response 14h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained is surveyed when being prepared into electrode of super capacitor
Its fixed chemical property：In 0.5A g-1When, specific capacitance is 1219.5F g-1；Its circulate 2000 circle after capacity retention be
94.7%.
Embodiment 9
Synthesize the carbon quantum dot of N doping：600 μ L ethylenediamines are added to containing 0.2g anhydrous citric acids under room temperature condition
In the mixed liquor of 0.6g phosphorus pentoxides, polytetrafluoroethylene (PTFE) stainless steel cauldron is transferred to, 2mL deionized waters is added and seals
The hydro-thermal reaction 5h at 120 DEG C, is then cooled to room temperature and adds 5mL deionized waters formation clear solution, add anhydrous second
Alcohol carries out centrifuge washing, carbon quantum dot precipitation is obtained, in vacuum drying chamber drying for standby.
Synthesize carbon quantum dot-cobaltosic oxide composite material：By 0.005mol CoCl2﹒ 6H2O, 50mg carbon quantum dot,
0.015mol urea is mixed and added into 40mL deionized water ultrasonic mixings and is formed uniformly red, transparent solution, and mixed liquor is transferred to
120 DEG C of heating response 20h of polytetrafluoroethylene (PTFE) stainless steel cauldron, with ethanol centrifuge washing and are drying to obtain the oxygen of carbon quantum dot-four
Change three cobalt composite materials.
Electrode is prepared and electrochemical property test：It is 8 according to mass ratio:1:1 weighs active material 8mg, acetylene black respectively
1mg, the μ L of polytetrafluoroethylene (PTFE) 100, add 1mL ethanol as solvent, are uniformly mixed, are dried in grume, are applied to 1cm*
In 3cm*1mm nickel foams, 12h is dried in vacuo, using 2M KOH solutions as electrolyte, Ag electrodes are used as reference electrode, nickel foam
As reference electrode, the chemical property of material is determined under three-electrode system.
Carbon quantum dot-cobaltosic oxide composite material that the present embodiment is obtained is surveyed when being prepared into electrode of super capacitor
Its fixed chemical property：In 0.5A g-1When, specific capacitance is 880.5F g-1；Its circulate 2000 circle after capacity retention be
90.2%.
Claims (9)
1. the preparation method of a kind of carbon quantum dot-cobaltosic oxide combination electrode material, it is characterised in that comprise the following steps that：
(1) carbon quantum dot of N doping is synthesized
Ethylenediamine, anhydrous citric acid, phosphorus pentoxide and water are added in polytetrafluoroethylene (PTFE) stainless steel cauldron and carry out hydro-thermal
Reaction；After reaction terminates, room temperature is cooled to, deionized water formation clear solution is added, adds absolute ethyl alcohol and carry out centrifuge washing,
Obtain carbon quantum dot；
(2) carbon quantum dot-cobaltosic oxide composite material is synthesized
Mixed liquor after ultrasonic mixing is uniform in water, is transferred to polytetrafluoroethylene (PTFE) by soluble cobalt, carbon quantum dot and urea
Hydro-thermal reaction is carried out in stainless steel cauldron；After reaction terminates, centrifuge, wash, to be drying to obtain carbon quantum dot-cobaltosic oxide multiple
Condensation material.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), anhydrous citric acid, ethylenediamine, five oxidations
Two phosphorus and the mass ratio of deionized water are (1~2):(2~5):(2~6):1.
3. preparation method as claimed in claim 1, it is characterised in that in step (1), hydrothermal temperature is 80~150 DEG C,
The hydro-thermal reaction time is 2~8h.
4. preparation method as claimed in claim 1, it is characterised in that in step (2), soluble cobalt is nitrate, sulfuric acid
One kind in salt, acetate and hydrochloride.
5. preparation method as claimed in claim 1, it is characterised in that in step (2), the molar concentration of soluble cobalt is 1
~3mol/L.
6. preparation method as claimed in claim 1, it is characterised in that in step (2), the mol ratio of soluble cobalt and urea
For 1:1~1:5；The quality of carbon quantum dot is the 1.5%~4.5% of soluble cobalt quality.
7. preparation method as claimed in claim 1, it is characterised in that in step (2), hydrothermal temperature is 100~160
DEG C, the hydro-thermal reaction time is 12~20h.
8. carbon quantum dot-cobaltosic oxide composite material prepared by a kind of preparation method as described in one of claim 1~7.
9. carbon quantum dot-cobaltosic oxide composite material as claimed in claim 8, it is characterised in that it is chrysanthemum shape space
Structure, circle are flower-shaped, intensive flower-shaped, or elongated blade of grass shape and globular combination.
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