CN106653401A - Three-dimensional nitrogen-doped capsule-shaped carbon paper electrode material and preparation method thereof - Google Patents
Three-dimensional nitrogen-doped capsule-shaped carbon paper electrode material and preparation method thereof Download PDFInfo
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- CN106653401A CN106653401A CN201710019232.5A CN201710019232A CN106653401A CN 106653401 A CN106653401 A CN 106653401A CN 201710019232 A CN201710019232 A CN 201710019232A CN 106653401 A CN106653401 A CN 106653401A
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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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- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/32—Carbon-based
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a three-dimensional nitrogen-doped capsule-shaped carbon paper electrode material and a preparation method thereof. The method disclosed by the invention comprises the following steps: firstly with manganese nitrate and aluminum nitrate as raw materials, and urea as an alkali source, carrying out stirring and backflow at a certain temperature to obtain an Mg-Al layered metal hydroxide Mg-Al LDH; adding a certain amount of dopamine after carrying out cooling, carrying out stirring for a certain period of time at normal temperature to obtain a PL composite material coated with dopamine; then, carrying out a once etching-roasting-twice etching process to obtain a three-dimensional nitrogen-doped capsule-shaped carbon paper electrode material HCF2. According to the three-dimensional nitrogen-doped capsule-shaped carbon paper electrode material disclosed by the invention, the preparation process and the necessary equipment are simple, the raw material sources are rich, and the reaction temperature is relatively low; the obtained three-dimensional nitrogen-doped capsule-shaped carbon paper electrode material HCF2 not only has good thermal stability, high crystallinity and high energy density and power density, but also has high morphology controllability, thereby being one of the ideal energy materials.
Description
Technical field
The invention belongs to materialogy technical field, it particularly relates to a kind of three-dimensional N doping capsule shape carbon paper electrode material
Material and preparation method thereof.
Background technology
The progress of human social development, the increase of energy demand causes traditional fossil energy supply and demand crisis and ring occur
The environmental issues such as the deterioration in border, acid rain, the greenhouse gases of initiation become increasingly conspicuous, in the urgent need to people constantly seek new cleaning energy
Source.The appearance of ultracapacitor and lithium electricity, has complied with people to Novel clean regenerative resource (such as solar energy, wind energy, biomass
Can, geothermal energy and tide energy etc.) demand.Lithium electricity has extended cycle life, short discharge and recharge time, energy density, power density are high and
The excellent performance such as wider range, the good reliability of operating temperature and being widely applied property and be increasingly subject to pay attention to, gradually replace
Generation traditional Ni-MH battery, ickel-cadmium cell and lead-acid accumulator, are widely used in the various electronic equipments of information age today, such as
Mobile phone, digital camera, video camera and digital processor etc..In recent years, lithium ion battery is in hybrid vehicle of new generation
Application on (hybrid electrical vehicle, HEV) and pure electric automobile (electrical vehicle, HEV)
It is of increasing concern.
In ultracapacitor, double layer capacitor is in powerful device in occupation of important position.Wherein, with glue
The material with carbon element of capsule assembling structure is considered the double layer electrodes material of most application prospect.The material with carbon element of hollow structure has higher
Specific surface area, short electric transmission path and good electrolyte wetability, so as to excellent chemical property.Nitrogen is mixed
Miscellaneous material with carbon element can to a certain extent improve electronic conductivity, surface polarity and avtive spot, by improving certain counterfeit electricity
Hold to improve the chemical property of electrode material.And traditional material with carbon element is prepared more with poison such as polyaniline, polypyrrole and polythiophenes
Property larger polymer be carbon precursor, have certain negative effect to environment.
The content of the invention
For above-mentioned technical problem, it is an object of the invention to provide the three-dimensional carbon electrode material of capsule shape two dimension carbon paper composition
Material and preparation method thereof.The method can solve the bad control of nitrogen content of the prior art and the use of poisonous carbon precursor is asked
Topic, while will not work the mischief to environment.
First with manganese nitrate and aluminum nitrate as raw material, urea is to be stirred at reflux under alkali source, uniform temperature to the inventive method
To Mg-Al LDH；A certain amount of dopamine stirring at normal temperature certain hour is added after cooling, the PL composite woods of poly-dopamine cladding are obtained
Material.Then carry out the secondarily etched technique of suction filtration etching-calcining-and obtain final product HCF2.
Concrete technical scheme of the present invention is described below.
A kind of preparation method of three-dimensional N doping capsule shape carbon paper electrode material, it is characterised in that comprise the following steps that：
(1) PDA/MgAl-LDH composites are prepared
Manganese nitrate, aluminum nitrate, urea and deionized water are well mixed first, are flowed back, naturally cool to room temperature, mixed
Close solution；Wherein：It is (1-4) by the mass ratio of manganese nitrate, aluminum nitrate and urea:19:100；
Then dopamine, stirring at normal temperature, afterwards washing, freeze-drying is added to obtain PDA/MgAl-LDH in mixed solution
Composite；Wherein dopamine and the mass ratio of manganese nitrate are 1：10-1：20；
(2) three-dimensional N doping capsule shape carbon paper electrode material is prepared
Take PDA/MgAl-LDH composites ultrasonic disperse in deionized water first, then with 0.8～1.2mol/L hydrochloric acid
Once etched, be dried after suction filtration；Then desciccate is calcined, product is carried out with 4.8～5.2mol/L hydrochloric acid after calcining
It is secondarily etched, after etching terminates, wash, be dried, obtain three-dimensional N doping capsule shape carbon paper electrode material.
In above-mentioned steps (1), the time is refluxed for 10～14h.The stirring at normal temperature time is 18-26h.Sublimation drying
For 40～50h.
In above-mentioned steps (2), calcining heat is 400-800 DEG C.
In above-mentioned steps (2), an etch period is 1.5-2h；The secondarily etched time is 5 days.
The present invention provides the three-dimensional N doping capsule shape carbon paper electrode material that a kind of above-mentioned preparation method is obtained.
The three-dimensional N doping capsule shape carbon paper electrode material of the present invention has high capacitance 346F g-1(0.1Ag-1Electricity
Under current density) and power density (5003.15W kg-1)。
The present invention, with dopamine as carbon nitrogen source, mixes with Mg-Al layered double hydroxide Mg-Al LDH as hard template
After miscellaneous nitrogen, etched by two steps, obtain the three-dimensional material with carbon element of hollow capsules structure paper-like formation.With prior art phase
Than, the beneficial effects of the present invention is：
1. the preparing raw material abundance of the present invention, reaction temperature are relatively low,
2. the three-dimensional capsule shape carbon paper electrode material for being obtained by the method for the present invention takes full advantage of nitrogen-doped carbon material
And the advantage of Mg-AlLDH templates, the simple individually low shortcoming of material with carbon element energy density is overcome, not only heat endurance is good, crystallization
Degree is high, and specific surface area is big, good cycling stability, and morphology controllable is strong, adds the dopamine of different quality ratio and can obtain
The different polymer of cladding poly-dopamine thickness.Additionally, the composite has higher specific capacitance, it is preferable energy and material
One of.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photographs of the Mg-Al LDH of the gained of embodiment 1 under 5000 multiplying power.
Fig. 2 is scanning electron microscope (SEM) photographs of the PL of the gained of embodiment 1 under 7000 multiplying power.
Fig. 3 is scanning electron microscope (SEM) photographs of the PL of the gained of embodiment 1 under 20000 multiplying power.
Fig. 4 is the scanning electron microscope (SEM) photograph before the HCF2 of the gained of embodiment 2 is calcined under 5000 multiplying power.
Fig. 5 is the scanning electron microscope (SEM) photograph before the HCF2 of the gained of embodiment 2 is calcined under 10000 multiplying power.
Fig. 6 is the scanning electron microscope (SEM) photograph after the HCF2 of the gained of embodiment 2 is calcined under 10000 multiplying power.
Fig. 7 is transmission electron microscope pictures of the Mg-Al LDH of the gained of embodiment 2 under high-resolution.
Fig. 8 is transmission electron microscope pictures of the PL of the gained of embodiment 2 under high-resolution.
Fig. 9 is the HCF2 electrochemical property tests CV figures of gained.
Figure 10 is the HCF2-600 electrochemical property tests CV figures of the gained of embodiment 2.
Figure 11 is the HCF2-600 loop test figures of the gained of embodiment 2.
Figure 12 is the XRD of the material obtained by embodiment.
Specific embodiment
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, but be not intended to limit the present invention.
Embodiment 1
A kind of preparation method of three-dimensional N doping capsule shape carbon paper electrode material, comprises the steps：
(1) PDA/MgAl-LDH (PL) is prepared
First, at room temperature, manganese nitrate, aluminum nitrate, urea and deionized water are pressed into 4:1:19:100 mass ratioes are in container
In be well mixed；Then, above-mentioned mixed solution is moved into round flask, is refluxed under the conditions of 100 DEG C；After reaction terminates, from
So it is cooled to room temperature.Then by the dopamine of 400mg, (dopamine is 1 with the mass ratio of manganese nitrate:10) add above-mentioned reaction molten
Liquid, stirring at normal temperature certain hour, deionized water and ethanol are washed 4 times, and freeze-drying obtains PL composites；
(2) preparation (HCF2-400) of three-dimensional N doping capsule shape carbon paper electrode material
First, take a certain amount of above-mentioned PL and be dissolved in deionized water ultrasonic disperse, with nature after the salt acid etch suction filtration of 1mol/L
It is cooled to room temperature；Then after is calcined at 400 DEG C above-mentioned desciccate, carried out with the hydrochloric acid of 5mol/L secondarily etched, spent
Ionized water cleaning product, is dried to obtain final product HCF2 under the conditions of 80 DEG C.
Using field emission scanning electron microscope (German Zeiss ultra 55) instrument, the above-mentioned institute under 5000 multiplying power
PL powder be scanned, the scanning electron microscope (SEM) photograph of gained is as shown in figure 1, as can be seen from Figure 1 complete regular hexagon Mg-
AlLDH composite structures, have been indicated above successfully preparing Mg-Al LDH；Under 7000 and 20000 multiplying power, to above-mentioned
Gained compound PL sheet two-dimensional materials are scanned, and the scanning electron microscope (SEM) photograph of gained from Fig. 2 and 3 as shown in Fig. 2 can be seen that
Poly-dopamine is evenly distributed in regular hexagon Mg-Al LDH surfaces, and remains without unnecessary poly-dopamine, poly-dopamine
Thickness is very uniform, has been indicated above poly-dopamine and regular hexagon Mg-Al LDH are combined with each other well, successfully prepares PL
Sheet two-dimensional material.
Embodiment 2
A kind of preparation method of three-dimensional N doping capsule shape carbon paper electrode material, comprises the steps：
(1) PDA/MgAl-LDH (PL) is prepared
First, at room temperature, manganese nitrate, aluminum nitrate, urea and deionized water are pressed into 3:1:19:100 mass ratioes are in container
In be well mixed；Then, above-mentioned mixed solution is moved into round flask, is refluxed under the conditions of 100 DEG C；After reaction terminates, from
So it is cooled to room temperature.Then by the dopamine of 400mg, (dopamine is 1 with the mass ratio of manganese nitrate:15) add above-mentioned reaction molten
Liquid, stirring at normal temperature certain hour, deionized water and ethanol are washed 4 times, and freeze-drying obtains PL composites；
(2) preparation (HCF2-600) of three-dimensional N doping capsule shape carbon paper electrode material
First, take a certain amount of above-mentioned PL and be dissolved in deionized water ultrasonic disperse, with nature after the salt acid etch suction filtration of 1mol/L
It is cooled to room temperature；Then after is calcined at 600 DEG C above-mentioned desciccate, carried out with the hydrochloric acid of 5mol/L secondarily etched, spent
Ionized water cleaning product, is dried to obtain final product HCF2 under the conditions of 80 DEG C.
Using field emission scanning electron microscope (German Zeiss ultra 55) instrument, in 5000 and 10000 multiplying power
Under above-mentioned gained HCF2 calcined materials before be scanned, the scanning electron microscope (SEM) photograph of gained as shown in Figures 4 and 5, from figure can be with
Find out after first step acid etch, successfully prepared and three-dimensional cavernous structure is piled into by sheet hollow capsules shape structure
Composite.Pile up neat between the composite material sheet and piece, show successfully to have prepared three-dimensional composite material.Fig. 6 is gained
600 DEG C of HCF2 calcined materials gained afterwards scanning electron microscope (SEM) photograph, it can be seen that well three-dimensional knot is remained in that after calcining
Structure；Fig. 7 is transmission electron microscope pictures of the Mg-Al LDH of gained under high-resolution, and Fig. 8 is transmission electricity of the PL of gained under high-resolution
Mirror figure, can significantly find out from Fig. 7 and Fig. 8, and the success of poly-dopamine is coated on Mg-Al LDH.
Embodiment 3
A kind of preparation method of three-dimensional N doping capsule shape carbon paper electrode material, comprises the steps：
(1) PDA/MgAl-LDH (PL) is prepared
First, at room temperature, manganese nitrate, aluminum nitrate, urea and deionized water are pressed into 2:1:19:100 mass ratioes are in container
In be well mixed；Then, above-mentioned mixed solution is moved into round flask, is refluxed under the conditions of 100 DEG C；After reaction terminates, from
So it is cooled to room temperature.Then by the dopamine of 400mg, (dopamine is 1 with the mass ratio of manganese nitrate:20) add above-mentioned reaction molten
Liquid, stirring at normal temperature certain hour, deionized water and ethanol are washed 4 times, and freeze-drying obtains PL composites；
(2) preparation (HCF2-800) of three-dimensional N doping capsule shape carbon paper electrode material
First, take a certain amount of above-mentioned PL and be dissolved in deionized water ultrasonic disperse, with nature after the salt acid etch suction filtration of 1mol/L
It is cooled to room temperature；Then after is calcined at 800 DEG C above-mentioned desciccate, carried out with the hydrochloric acid of 5mol/L secondarily etched, spent
Ionized water cleaning product, is dried to obtain final product HCF2 under the conditions of 80 DEG C.
Fig. 9 and Figure 12 are the CV circulations figures and the XRD of all composites of gained HCF2 composites.Can be with from Fig. 9
The composite for finding out the gained of embodiment 2 has highest specific capacitance 346F g-1(0.1Ag-1Current density under)；From Figure 12
As can be seen that the successful preparation of Mg-Al LDH, PL and HCF2 composites.Figure 10 and 11 is gained HCF2-600 composites
CV circulation figure and cycle performance figure, even if under big sweep speed 200mV/s, what CV cyclic curves shape do not have substantially
Change, and after charge and discharge cycles 10000 are enclosed, specific capacity still can reach 99.73% conservation rate.It can be seen that gained is compound
The good chemical property of material.
In sum, the preparation method of the three-dimensional structure electrode material of a kind of N doping capsule shape carbon paper of the invention composition
Composite under the different calcining heats of gained, their chemical property is different under different calcining heats, in 1M KOH
It is prepared with three-electrode system in electrochemical workstation and the chemical property of blue electric system test material under electrolyte conditions
The best HCF2-600 electrodes of chemical property in 0.2Ag-1There is specific capacity 298F during constant current charge-discharge, but due in charge and discharge
In electric process, its volume can be changed significantly, and after circulation 10000 times, specific capacity is not changed in substantially, and close in high current
Under degree, high rate performance declines unobvious；With good cyclical stability and forthright again.
The above is only specifically enumerating for embodiments of the present invention, and according to appointing that technical scheme is made
What equivalent transformation, all should belong to protection scope of the present invention.
Claims (7)
1. a kind of preparation method of three-dimensional N doping capsule shape carbon paper electrode material, it is characterised in that comprise the following steps that：
(1) PDA/MgAl-LDH composites are prepared
Manganese nitrate, aluminum nitrate, urea and deionized water are well mixed first, are flowed back, naturally cool to room temperature, obtain mixing molten
Liquid；Wherein：It is (1-4) by the mass ratio of manganese nitrate, aluminum nitrate and urea:19:100；
Then dopamine, stirring at normal temperature, washing afterwards, freeze-drying is added to obtain PDA/MgAl-LDH and be combined in mixed solution
Material；Wherein dopamine and the mass ratio of manganese nitrate are 1：10-1：20；
(2) three-dimensional N doping capsule shape carbon paper electrode material is prepared
PDA/MgAl-LDH composites ultrasonic disperse in deionized water is taken first, then is carried out with 0.8～1.2mol/L hydrochloric acid
Once etch, be dried after suction filtration；Then desciccate is calcined, product 4.8～5.2mol/L hydrochloric acid carries out secondary after calcining
Etching, after etching terminates, washs, is dried, and obtains three-dimensional N doping capsule shape carbon paper electrode material.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), is refluxed the time for 10～14h.
3. preparation method as claimed in claim 1, it is characterised in that in step (1), the stirring at normal temperature time is 18-26h.
4. preparation method as claimed in claim 1, it is characterised in that in step (1), sublimation drying is 40～50h.
5. preparation method as claimed in claim 1, it is characterised in that in step (2), calcining heat is 400-800 DEG C.
6. preparation method as claimed in claim 1, it is characterised in that in step (2) a, etch period is 1.5-2h；Two
Secondary etch period is 5 days.
7. the three-dimensional N doping capsule shape carbon paper electrode material that the preparation method as described in one of claim 1-6 is obtained.
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| CN108270017A (en) * | 2018-01-19 | 2018-07-10 | 东华大学 | A kind of nickel-nitrogen-doped carbon composite material and its preparation method and application |
| CN108565469A (en) * | 2017-12-28 | 2018-09-21 | 东华大学 | A kind of cobalt-nitrogen-doped carbon composite material and preparation method |
| CN108706568A (en) * | 2018-05-04 | 2018-10-26 | 青海泰丰先行锂能科技有限公司 | A kind of preparation method of N doping Porous hollow carbon Nano capsule material and the material of preparation |
| CN110424039A (en) * | 2019-09-16 | 2019-11-08 | 东北大学 | The preparation method of the anti-corrosion selfreparing differential arc oxidation coating of magnesium alloy based on hydrotalcite nano inhibition microcapsules |
| CN111167495A (en) * | 2020-01-07 | 2020-05-19 | 郑州大学 | Catalyst Ni for ammonia borane hydrogen production2-xFex@ CN-G and preparation method thereof |
| CN114933294A (en) * | 2022-05-13 | 2022-08-23 | 西安交通大学 | High-volume-density multilayer compact porous carbon nanosheet and preparation method and application thereof |
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| CN114933294A (en) * | 2022-05-13 | 2022-08-23 | 西安交通大学 | High-volume-density multilayer compact porous carbon nanosheet and preparation method and application thereof |
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