CN103745836B - A method for preparing a g-C3N4/carbon quantum dot composite electrode for super capacitor - Google Patents
A method for preparing a g-C3N4/carbon quantum dot composite electrode for super capacitor Download PDFInfo
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- CN103745836B CN103745836B CN201310736114.8A CN201310736114A CN103745836B CN 103745836 B CN103745836 B CN 103745836B CN 201310736114 A CN201310736114 A CN 201310736114A CN 103745836 B CN103745836 B CN 103745836B
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Abstract
Provided is a method for preparing a g-C3N4/carbon quantum dot composite electrode for a super capacitor. 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 the capacitor.
Description
Technical field
The present invention relates to a kind of g-c3n4The 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 big, to environment
Close friend, with the features such as having extended cycle life, has important application at aspects such as electric automobile, communication, military affairs.Ultracapacitor is by electrode
Material, electrolyte solution, barrier film three part composition.Electrode material is the core content of ultracapacitor research.Wherein Graphene
The high-specific surface area of monatomic lamellar structure generation of material, high conductivity, the characteristic such as chemical stability, always super capacitor
The focus of device research.
g-c3n4There is the structure of class Graphene, be a kind of carboritride of two dimension.The lamellar structure of this graphite ene-type
Make g-c3n4There is high specific surface area, abundant pore structure, and the impact to compound structure due to n element, to material
The electrical conductivity of itself and electron density all increase.But due to g-c3n4Material electronicses transfer ability is weaker and non-conducting etc.
Shortcoming, limits its application on super-capacitor pole piece material.Carbon quantum dot (cqds) is that a kind of diameter is less than 10nm
Zero dimension material with carbon element, it has hypotoxicity, the features such as easy sense dough.
Content of the invention
The invention provides one kind can increase g-c3n4The electron transfer rate of material, has excellent conductive performance, and safety is no
The g-c of poison3n4The preparation method of/carbon quantum dot combination electrode.
The technical solution of the present invention is:
A kind of g-c3n4The preparation method of/carbon quantum dot combination electrode, it comprises the concrete steps that:
1.1st, prepare carbon quantum dot ethanol solution
Carbon quantum dot is added to the carbon quantum being configured in ethanol that carbon quantum dot mass percent concentration is 28%～32%
Point ethanol solution；
1.2nd, prepare g-c3n4/ carbon quantum dot composite
Carbamide is mixed according to mass ratio 1:1～1:2 with carbon quantum dot ethanol solution, 45w～55 w ultrasound wave disperses
It is transferred to after 5min～30min in crucible, be progressively warming up to after 350 DEG C～700 DEG C constant temperature 1h～3h with Muffle furnace and drop to room
Temperature, the material of gained is added after ethanol grinding is filtered and obtains final product g-c3n4/ carbon quantum dot composite.
The invention has the beneficial effects as follows:
1st, raw material is easy to get, cheap, and preparation method is simple, no coupling product；The composite property obtaining is stable, no
Easily decompose, nontoxic.
2nd, stable electrochemical property, high life, carbon quantum dot and graphite ene-type carbon-nitrogen material g-c3n4It is combined,
The small-size effect that carbon quantum dot has in itself as zero dimensional nanometer materials, skin effect makes carbon-nitrogen material activity increase, can be bright
The aobvious transfer rate accelerating electrolytic solution for super capacitor ion, increases constant current charge-discharge efficiency.
3rd, carbon quantum dot and g-c are adopted3n4Compound, the specific surface area of electrode can be strengthened, make electrode surface adsorb electronic capability
Strengthen, effectively improve the ratio electric capacity of capacitor.
4th, carbon quantum dot and g-c are passed through3n4It is combined, the electron transfer rate of material can be increased, thus increasing conduction
Property.
5th, g-c in cyclic voltammetry3n4/ carbon quantum dot composite remains under speed keep approximate in sweeping greatly of 400mv/s
Rectangle, and no substantially decay after multiple circulation, this illustrates g-c3n4The active material utilization of/carbon quantum dot composite
Apparently higher than other material with carbon elements.
Brief description
Fig. 1 is that the present invention does not carry out compound pure c3n4The transmission electron microscope picture of material；
Fig. 2 is g-c in the present invention (corresponding embodiment 1)3n4The transmission electron microscope picture of/carbon quantum dot composite.
Specific embodiment
Embodiment 1
1.1st, prepare carbon quantum dot ethanol solution
Carbon quantum dot is added to be configured in ethanol carbon quantum dot mass percent concentration 30% carbon quantum dot ethanol molten
Liquid；
1.2nd, prepare g-c3n4/ carbon quantum dot composite
The carbon quantum dot ethanol solution that 1g carbamide is 30% with 1g concentration mixes, and is transferred to after 45w ultrasound wave dispersion 5min
In crucible, drop to room temperature after Muffle furnace is progressively warming up to 550 DEG C of constant temperature 2 h, obtain powdered substance, finally plus ethanol grind
Product is obtained after filtration.By product and the pure c not being combined carbon quantum dot3n4Carry out transmission electron microscope sign (tem).Fig. 1 is
Pure c3n4Tem, c as we can see from the figure3n4There is the fold lamellar structure of the nanometer grade thickness of nearly Graphene；Fig. 2 is compound
G-c afterwards3n4The tem of/carbon quantum dot, from figure it will be clear that diameter in 6nm about carbon quantum dot be evenly distributed
In c3n4Do not change c in lamella and3n4The overall layer structure of material.
By g-c3n4/ carbon quantum dot composite, Ketjen black conductive agent, polyfluortetraethylene of binding element emulsion are according to mass ratio
85:10:5 mix homogeneously successively, is dissolved in ethanol, grinds and obtain slurry, Ran Houjun after stirring in agate mortar
It is coated in 80 μ m-thick nickel foam evenly, after being dried, be cut into diameter 16mm electrode slice with microtome, on infrared tablet machine
10mpa pressure presses to 10 μm of thin skins, places in vacuum drying oven, is vacuum dried 20 h, obtains g-c at 120 DEG C3n4/ carbon quantum
Point composite pole piece.
With g-c in the glove box of argon gas atmosphere3n4/ carbon quantum dot composite pole piece is positive and negative electrode pole piece, with pp(Japan
Nkk ultracapacitor dedicated diaphragm) it is barrier film, using 1 mol/lc8h20bf4N/pc electrolyte, by the pole piece after drying in handss
It is pressed into button-shaped ultracapacitor with sealing machine in casing.Volt-ampere, AC impedance, perseverance are circulated to the capacitor assembling
The performance test of current charge-discharge electricity, the running voltage that cyclic voltammetric evaluates capacitor is interval, and ac impedance spectroscopy obtains the interior of electrode
Resistance, constant current charge-discharge curve calculate capacitor quality specific capacitance, energy density, maximum power density, discharge and recharge imitate
Rate.
Embodiment 2
1.1st, prepare carbon quantum dot ethanol solution
Carbon quantum dot is added to be configured in ethanol carbon quantum dot mass percent concentration 32% carbon quantum dot ethanol molten
Liquid；
1.2nd, prepare g-c3n4/ carbon quantum dot composite
The carbon quantum dot ethanol solution that 1g carbamide is 32% with 1.2g concentration mixes, and turns after 55w ultrasound wave dispersion 30min
Move in crucible, drop to room temperature after Muffle furnace is progressively warming up to 350 DEG C of constant temperature 1h, obtain powdered substance, plus ethanol is ground
G-c is obtained final product after filter3n4/ carbon quantum dot composite.
With the g-c being obtained3n4/ carbon quantum dot electrode material is assembled into button-shaped super according to method same as Example 1
Capacitor, is circulated volt-ampere, AC impedance, constant current charge-discharge performance test using electrochemical workstation to it.
Embodiment 3
1.1st, prepare carbon quantum dot ethanol solution
Carbon quantum dot is added to be configured in ethanol carbon quantum dot mass percent concentration 28% carbon quantum dot ethanol molten
Liquid；
1.2nd, prepare g-c3n4/ carbon quantum dot composite
The carbon quantum dot ethanol solution that 1g carbamide is 28% with 1.5g concentration mixes, and turns after 50w ultrasound wave dispersion 20min
Move in crucible, drop to room temperature after Muffle furnace is progressively warming up to 600 DEG C of constant temperature 1.5h, obtain powdered substance, plus ethanol grinds
G-c is obtained final product after filtration3n4/ carbon quantum dot composite.
With the g-c being obtained3n4/ carbon quantum dot electrode material is assembled into button-shaped super according to method same as Example 1
Capacitor, is circulated volt-ampere, AC impedance, constant current charge-discharge performance test using electrochemical workstation to it.
Embodiment 4
1.1st, prepare carbon quantum dot ethanol solution
Carbon quantum dot is added to be configured in ethanol carbon quantum dot mass percent concentration 31% carbon quantum dot ethanol molten
Liquid；
1.2nd, prepare g-c3n4/ carbon quantum dot composite
The carbon quantum dot ethanol solution that 1g carbamide is 31% with 2g concentration mixes, and shifts after 55w ultrasound wave dispersion 30min
To crucible, drop to room temperature after Muffle furnace is progressively warming up to 700 DEG C of constant temperature 3h, obtain powdered substance, plus ethanol grinds and filters
After obtain final product g-c3n4/ carbon quantum dot composite.
With the g-c being obtained3n4/ carbon quantum dot electrode material is assembled into button-shaped super according to method same as Example 1
Capacitor, is circulated volt-ampere, AC impedance, constant current charge-discharge performance test using electrochemical workstation to it.
The electric capacity of table 1 ultracapacitor constant current charge-discharge and other parameters
Table 2 ultracapacitor difference sweeps ratio electric capacity (f/g) of cyclic voltammetric under speed
Claims (1)
1. a kind of g-c for ultracapacitor3n4The preparation method of/carbon quantum dot combination electrode material, is characterized in that: concrete
Step is:
1.1st, prepare carbon quantum dot ethanol solution
Carbon quantum dot is added to the carbon quantum dot second being configured in ethanol that carbon quantum dot mass percent concentration is 28%～32%
Alcoholic solution；
1.2nd, prepare g-c3n4/ carbon quantum dot composite
Carbamide is mixed according to mass ratio 1:1～1:2 with carbon quantum dot ethanol solution, 45w～55 w ultrasound wave dispersion 5min～
It is transferred to after 30min in crucible, be progressively warming up to after 350 DEG C～700 DEG C constant temperature 1h～3h with Muffle furnace and drop to room temperature, by institute
After the material obtaining adds ethanol grinding filtration, obtain the g-c for ultracapacitor3n4/ carbon quantum dot combination electrode material.
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| CN108630442B (en) * | 2018-04-28 | 2019-09-24 | 长春工业大学 | A kind of preparation method of the enhanced supercapacitor of C3N4 |
| CN109999882A (en) * | 2019-04-25 | 2019-07-12 | 湖南大学 | A kind of carbon quantum dot-graphite phase carbon nitride composite material, preparation method and application |
| CN110459754B (en) * | 2019-09-02 | 2022-06-24 | 晶瑞新能源科技有限公司 | High-performance lithium ion battery C3N4Preparation method of/carbon composite negative electrode material |
| CN110871100B (en) * | 2019-12-10 | 2022-07-12 | 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 |
| CN114515588A (en) * | 2021-12-29 | 2022-05-20 | 苏州科技大学 | g-C synthesized based on hollyhock stems3N4Method for preparing/C composite material |
| 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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