CN103745836A - A method for preparing a g-C3N4/carbon quantum dot composite electrode - Google Patents
A method for preparing a g-C3N4/carbon quantum dot composite electrode Download PDFInfo
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- CN103745836A CN103745836A CN201310736114.8A CN201310736114A CN103745836A CN 103745836 A CN103745836 A CN 103745836A CN 201310736114 A CN201310736114 A CN 201310736114A CN 103745836 A CN103745836 A CN 103745836A
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Abstract
Provided is a method for preparing a g-C3N4/carbon quantum dot composite electrode. The method comprises: adding carbon quantum dots into ethanol in order to prepare carbon quantum dot ethanol solution; mixing urea with the carbon quantum dot ethanol solution, performing ultrasonic dispersion on the mixed solution and then transferring the mixed solution to a crucible; warming the mixed solution to 350 to 700 degree centigrade with a muffle furnace step by step, maintaining the temperature for one to three hours and then decreasing the temperature of the mixed solution to room temperature; and grinding the obtained substance with ethanol and filtering the same so as to obtain g-C3N4/carbon quantum dot composite material. The method has advantages of simpleness, no by-products, raw material easy to obtain, and low price. The obtained composite material is stable in performance, uneasy to decompose, and nontoxic. The method may increase the electron transfer rate of the g-C3N4 material, has good conductive performance, enhances electrode specific area, improves the electron adsorption capability of an electrode surface, and effectively increases the specific capacitance of a capacitor.
Description
Technical field
The present invention relates to a kind of g-C
3n
4the preparation method of/carbon quantum dot combination electrode.
Background technology
Ultracapacitor was risen 20 century 70s～eighties, because its power-performance is good, specific capacity is large, the environmentally friendly and feature such as have extended cycle life, at aspects such as electric automobile, communication, military affairs, had important application.Ultracapacitor is comprised of electrode material, electrolyte solution, barrier film three parts.Electrode material is the core content of ultracapacitor research.High-specific surface area, high conductivity that wherein the monatomic lamellar structure of grapheme material produces, the characteristics such as chemical stability are the focuses of ultracapacitor research always.
G-C
3n
4having the structure of class Graphene, is a kind of carboritride of two dimension.The lamellar structure of this Graphene type makes g-C
3n
4there is high specific area, abundant pore structure, and due to the impact of N element on compound structure, conductivity and electron density to material itself all increase.But due to g-C
3n
4the shortcomings such as material electronics transfer ability is weak and non-conducting, have limited its application in ultracapacitor pole piece material.The features such as carbon quantum dot (CQDs) is the zero dimension material with carbon element that a kind of diameter is less than 10nm, and it has hypotoxicity, easy functionalization.
Summary of the invention
The invention provides one and can increase g-C
3n
4the electron transfer rate of material, has excellent conductive performance, the g-C of safety non-toxic
3n
4the preparation method of/carbon quantum dot combination electrode.
Technical solution of the present invention is:
A kind of g-C
3n
4the preparation method of/carbon quantum dot combination electrode, its concrete steps are:
1.1, preparation carbon quantum dot ethanolic solution
Carbon quantum dot is joined and in ethanol, is mixed with the carbon quantum dot ethanolic solution that carbon quantum dot mass percent concentration is 28%～32%;
1.2, preparation g-C
3n
4/ carbon quantum dot composite material
Urea is mixed according to mass ratio 1:1～1:2 with carbon quantum dot ethanolic solution, 45W～55 W ultrasonic wave disperses to be transferred in crucible after 5min～30min, after being progressively warming up to 350 ℃～700 ℃ constant temperature 1h～3h with Muffle furnace, drop to room temperature, the material of gained is added after ethanol grinds filtration and obtains g-C
3n
4/ carbon quantum dot composite material.
The invention has the beneficial effects as follows:
1, raw material are easy to get, cheap, and preparation method is simple, no coupling product; Decomposition, nontoxic is stablized, is difficult for to the composite property obtaining.
2, stable electrochemical property, high life, carbon quantum dot and Graphene type carbon-nitrogen material g-C
3n
4carry out compound, the small-size effect that carbon quantum dot itself has as zero-dimension nano material, skin effect makes that carbon-nitrogen material is active to be increased, and can obviously accelerate the transmission rate of electrolytic solution for super capacitor ion, increases constant current charge-discharge efficiency.
3, adopt carbon quantum dot and g-C
3n
4compound, the specific area of energy intensifier electrode, strengthens electrode surface attract electrons ability, effectively improves the ratio electric capacity of capacitor.
4, by carbon quantum dot and g-C
3n
4carry out compoundly, can increase the electron transfer rate of material, thereby increase conductivity.
5, g-C in cyclic voltammetry
3n
4/ carbon quantum dot composite material still can keep approximate rectangular sweeping greatly of 400mV/s under speed, and through repeatedly decaying without obvious after circulation, this illustrates g-C
3n
4the active material utilization of/carbon quantum dot composite material is apparently higher than other material with carbon element.
Accompanying drawing explanation
Fig. 1 is that the present invention does not carry out compound pure C
3n
4the transmission electron microscope picture of material;
Fig. 2 is g-C in the present invention (corresponding embodiment 1)
3n
4the transmission electron microscope picture of/carbon quantum dot composite material.
Embodiment
embodiment 1
1.1, preparation carbon quantum dot ethanolic solution
Carbon quantum dot is joined to the carbon quantum dot ethanolic solution that is mixed with carbon quantum dot mass percent concentration 30% in ethanol;
1.2, preparation g-C
3n
4/ carbon quantum dot composite material
The carbon quantum dot ethanolic solution that is 30% with 1g concentration by 1g urea mixes, 45W ultrasonic wave disperses to be transferred in crucible after 5min, after Muffle furnace is progressively warming up to 550 ℃ of constant temperature 2 h, drop to room temperature, obtain powdered substance, finally add after ethanol grinds filtration and obtain product.By product and the pure C of composite carbon quantum dot not
3n
4carry out transmission electron microscope sign (TEM).Fig. 1 is pure C
3n
4tEM, C as we can see from the figure
3n
4there is the fold lamellar structure of the nanometer grade thickness of nearly Graphene; Fig. 2 is the g-C after compound
3n
4the TEM of/carbon quantum dot, can be clear that from figure diameter is evenly distributed in C at the carbon quantum dot of 6nm left and right
3n
4in lamella and do not change C
3n
4the layer structure of material monolithic.
By g-C
3n
4/ carbon quantum dot composite material, Ketjen black conductive agent, polyfluortetraethylene of binding element emulsion mix successively according to mass ratio 85:10:5, dissolved in ethanol, in agate mortar, grinding obtains slurry after stirring, then be coated in equably in the thick nickel foam of 80 μ m, after dry, with slicing machine, be cut into diameter 16mm electrode slice, on infrared tablet press machine, 10Mpa pressure presses to 10 μ m thin skins, places in vacuum drying chamber, at 120 ℃, vacuumize 20 h, obtain g-C
3n
4/ carbon quantum dot composite pole piece.
In the glove box of argon gas atmosphere with g-C
3n
4/ carbon quantum dot composite pole piece is positive and negative electrode pole piece, take PP(Japan NKK ultracapacitor dedicated diaphragm) as barrier film, adopt 1 mol/LC
8h
20bF
4n/PC electrolyte is pressed into button-shaped ultracapacitor with sealing machine by the pole piece after drying in glove box.The capacitor assembling is carried out to the performance test of cyclic voltammetric, AC impedance, constant current charge-discharge, cyclic voltammetric is evaluated the operating voltage interval of capacitor, ac impedance spectroscopy obtains the internal resistance value of electrode, constant current charge-discharge curve is calculated to such an extent that the quality of capacitor compares capacitance, energy density, maximum power density, efficiency for charge-discharge.
embodiment 2
1.1, preparation carbon quantum dot ethanolic solution
Carbon quantum dot is joined to the carbon quantum dot ethanolic solution that is mixed with carbon quantum dot mass percent concentration 32% in ethanol;
1.2, preparation g-C
3n
4/ carbon quantum dot composite material
The carbon quantum dot ethanolic solution that is 32% with 1.2g concentration by 1g urea mixes, and 55W ultrasonic wave disperses to be transferred in crucible after 30min, after Muffle furnace is progressively warming up to 350 ℃ of constant temperature 1h, drops to room temperature, obtains powdered substance, adds after ethanol grinds filtration and obtains g-C
3n
4/ carbon quantum dot composite material.
With the g-C making
3n
4/ carbon quantum dot electrode material is assembled into button-shaped ultracapacitor according to the method identical with embodiment 1, utilizes electrochemical workstation to carry out cyclic voltammetric, AC impedance, constant current charge-discharge performance test to it.
embodiment 3
1.1, preparation carbon quantum dot ethanolic solution
Carbon quantum dot is joined to the carbon quantum dot ethanolic solution that is mixed with carbon quantum dot mass percent concentration 28% in ethanol;
1.2, preparation g-C
3n
4/ carbon quantum dot composite material
The carbon quantum dot ethanolic solution that is 28% with 1.5g concentration by 1g urea mixes, and 50W ultrasonic wave disperses to be transferred in crucible after 20min, after Muffle furnace is progressively warming up to 600 ℃ of constant temperature 1.5h, drops to room temperature, obtains powdered substance, adds after ethanol grinds filtration and obtains g-C
3n
4/ carbon quantum dot composite material.
With the g-C making
3n
4/ carbon quantum dot electrode material is assembled into button-shaped ultracapacitor according to the method identical with embodiment 1, utilizes electrochemical workstation to carry out cyclic voltammetric, AC impedance, constant current charge-discharge performance test to it.
embodiment 4
1.1, preparation carbon quantum dot ethanolic solution
Carbon quantum dot is joined to the carbon quantum dot ethanolic solution that is mixed with carbon quantum dot mass percent concentration 31% in ethanol;
1.2, preparation g-C
3n
4/ carbon quantum dot composite material
The carbon quantum dot ethanolic solution that is 31% with 2g concentration by 1g urea mixes, and 55W ultrasonic wave disperses to be transferred in crucible after 30min, after Muffle furnace is progressively warming up to 700 ℃ of constant temperature 3h, drops to room temperature, obtains powdered substance, adds after ethanol grinds filtration and obtains g-C
3n
4/ carbon quantum dot composite material.
With the g-C making
3n
4/ carbon quantum dot electrode material is assembled into button-shaped ultracapacitor according to the method identical with embodiment 1, utilizes electrochemical workstation to carry out cyclic voltammetric, AC impedance, constant current charge-discharge performance test to it.
The electric capacity of table 1 ultracapacitor constant current charge-discharge and other parameter
Table 2 ultracapacitor difference is swept the ratio electric capacity (F/g) of the lower cyclic voltammetric of speed
Claims (1)
1. a g-C
3n
4the preparation method of/carbon quantum dot combination electrode, is characterized in that: concrete steps are:
1.1, preparation carbon quantum dot ethanolic solution
Carbon quantum dot is joined and in ethanol, is mixed with the carbon quantum dot ethanolic solution that carbon quantum dot mass percent concentration is 28%～32%;
1.2, preparation g-C
3n
4/ carbon quantum dot composite material
Urea is mixed according to mass ratio 1:1～1:2 with carbon quantum dot ethanolic solution, 45W～55 W ultrasonic wave disperses to be transferred in crucible after 5min～30min, after being progressively warming up to 350 ℃～700 ℃ constant temperature 1h～3h with Muffle furnace, drop to room temperature, the material of gained is added after ethanol grinds filtration and obtains g-C
3n
4/ carbon quantum dot composite material.
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| CN104117375A (en) * | 2014-06-18 | 2014-10-29 | 南京大学 | Preparation method of synthesized carbon quantum dot-carbon nitrogen macromolecule composite infrared light catalyst |
| CN104841470A (en) * | 2015-04-17 | 2015-08-19 | 浙江工业大学 | Composite titanium dioxide nano-sheet photocatalyst, preparation method and applications thereof |
| CN104934232A (en) * | 2015-05-13 | 2015-09-23 | 东南大学 | Titanium dioxide or titanium nitride supported carbon quantum dot modification polypyrrole nanometer array material and preparation method and application thereof |
| CN105080577A (en) * | 2015-09-11 | 2015-11-25 | 中国科学技术大学 | Cobalt di-selenide nanobelt assembling sphere and preparation method and application thereof |
| CN105597807A (en) * | 2015-09-21 | 2016-05-25 | 江苏华天通纳米科技有限公司 | Preparation method of carbon nitride photocatalyst with sheet-shaped structure embedded with carbon nano particles |
| CN105810442A (en) * | 2016-03-16 | 2016-07-27 | 长春工业大学 | Fabrication method of g-C3N4 reinforced solar cell |
| CN106350830A (en) * | 2016-09-13 | 2017-01-25 | 北京科技大学 | TiO2/C3N4/CQDs (carbon quantum dots) composite photoanode and preparation method thereof |
| CN106971863A (en) * | 2017-04-21 | 2017-07-21 | 华中科技大学 | A kind of g C3N4/NiCo2S4Composite, preparation method and applications |
| CN107376967A (en) * | 2017-06-27 | 2017-11-24 | 常州大学 | A kind of preparation method of nitrogenous carbon quantum dot/graphite phase carbon nitride composite photo-catalyst |
| CN107519907A (en) * | 2017-07-19 | 2017-12-29 | 广东工业大学 | A kind of carbon point and graphite phase carbon nitride composite photo-catalyst and its preparation method and application |
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| CN110459754A (en) * | 2019-09-02 | 2019-11-15 | 载元派尔森新能源科技有限公司 | A kind of high performance lithium ion battery C3N4The preparation method of/carbon compound cathode materials |
| CN110871100A (en) * | 2019-12-10 | 2020-03-10 | 苏州大学 | Aniline carbon quantum dot doped carbon nitride material and preparation and application thereof |
| US11174165B2 (en) | 2020-01-17 | 2021-11-16 | Qatar University | Scalable nitrogen enriched carbon-based nanosystems for efficient and prompt capacitive seawater desalination under ambient conditions |
| CN114768844A (en) * | 2022-03-23 | 2022-07-22 | 桂林电子科技大学 | Ultrathin porous flaky g-C3N4Preparation method and application of photocatalyst |
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