CN108400023A - A kind of three-dimensional nitrogen-doped carbon foam combination electrode material and preparation method thereof - Google Patents
A kind of three-dimensional nitrogen-doped carbon foam combination electrode material and preparation method thereof Download PDFInfo
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- CN108400023A CN108400023A CN201810212762.6A CN201810212762A CN108400023A CN 108400023 A CN108400023 A CN 108400023A CN 201810212762 A CN201810212762 A CN 201810212762A CN 108400023 A CN108400023 A CN 108400023A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- 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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- 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
- H01G11/48—Conductive polymers
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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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- 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
Abstract
The invention belongs to storage material preparing technical field, specially a kind of three-dimensional nitrogen-doped carbon foam combination electrode material and preparation method thereof.Iron chloride and hydrochloric acid are added in deionized water first for preparation method of the present invention, and are sufficiently mixed；Then melamine foamed plastic (MS) is immersed, adds a certain amount of aniline monomer, from washing, be dried to obtain product after 10 are stirred at 20 90 DEG C for 24 hours；Obtained product is finally obtained into three-dimensional nitrogen-doped carbon foam combination electrode material in calcining.Preparation method of the present invention is simple and reliable, at low cost, environmental-friendly.Obtained nitrogen-doped carbon foamed composite has large specific surface area, cycle performance excellent and N doping makes surface charge store fast reaction, is ideal new energy materials, can be used as electrode material.
Description
Technical field
The present invention relates to a kind of three-dimensional nitrogen-doped carbon foam combination electrode materials and preparation method thereof, belong to energy storage material
Expect preparing technical field.
Background technology
Ultracapacitor is a kind of high-energy power storage element, the characteristic with traditional dielectric capacitance and battery, simultaneously
Also have that super large capacitor, the charge and discharge time is short, service life is long, maintenance cost is low, advantages of environment protection, be considered as this century
Most promising new green power.
Ultracapacitor device is called electrochemical capacitor, including double layer capacitor and pseudocapacitors, it is to pass through polarization
Electrolyte carrys out energy storage, is a kind of electrochemical element, and thermal energy storage process is reversible.Wherein electrode material is the core of capacitor
Part.Currently, the ultracapacitor of carbon material has obtained quick development because of its larger specific surface area and electric conductivity, but due to it
The features such as specific capacitance is small, energy density is low significantly limits its application.Nitrogen-doped porous carbon material can be provided for accommodating
The porous structure of the high surface area of charge, the carbon atom for adulterating nitrogen provide stronger electrolyte wettability and electron conduction,
There is high circulation simultaneously, can preferably make up deficiency of the carbon material in terms of capacitor application.
Therefore, it is intended that preparing one kind by a kind of method of high-efficiency environment friendly can be used for ultracapacitor, have compared with
The three-dimensional nitrogen-doped carbon foam combination electrode material of big specific surface area, super large capacitor, longer service life, and applied
On ultracapacitor.
Invention content
In view of the deficiencies of the prior art, the purpose of the invention is to provide a kind of simple and practicable preparation three-dimensional N dopings
Carbon foam electrode material and its method.The present invention is prepared using dipping-method for calcinating, obtained three-dimensional nitrogen-doped carbon foam electrode
Material morphology is controllable, and structure is uniform.
Technical scheme of the present invention is specific as follows.
A kind of preparation method of three-dimensional nitrogen-doped carbon foam combination electrode material, is as follows：
(1) ferric chloride hexahydrate of 5-15mmol is added in the hydrochloric acid of 15-25ml 0.5-1.5mol/l, ultrasonic 30-
60min；
(2) melamine foamed plastic is immersed in step (1) in mixed solution, and the aniline monomer of 0.1-2g is added, in 20-
10-24h is stirred at a temperature of 50 DEG C；
(3) by step (2) product deionized water and after absolute ethyl alcohol washs, then vacuum is dry at 20-90 DEG C
Dry 12-24h；
(4) by treated in step (3), product rises to 700-900 DEG C with 5-8 DEG C of heating rate, is protected in inert gas
Shield is lower to calcine 1-2h, and cooled to room temperature is to get to three-dimensional nitrogen-doped carbon foam combination electrode material later.
In above-mentioned steps (1), ultrasonic power 200-500W.
In above-mentioned steps (2), mixing speed should be being slowly stirred for 100-800r/min.
In above-mentioned steps (2), the size of melamine foamed plastic is 2 × 2 × 2-5 × 5 × 5cm3。
In above-mentioned steps (2), the quality of aniline monomer is 0.5-1.5g.
In above-mentioned steps (2), temperature is 20-35 DEG C.
In above-mentioned steps (4), inert gas is any in nitrogen or helium.
The present invention also provides three-dimensional nitrogen-doped carbon foam combination electrode materials made from a kind of above-mentioned preparation method.
The three-dimensional nitrogen-doped carbon foam combination electrode material that the present invention obtains is in sponge foam shape, is a kind of classifying porous knot
Structure, have big specific surface area, excellent cycle performance, and it is carbon-nitrogen doped make surface charge store fast reaction, shorten fortune
Defeated path is one of ideal energy and material, can be used as electrode material.
Compared with existing preparation method, beneficial effects of the present invention are as described below：
1, the coupling of melamine sponge and aniline is taken full advantage of.
2, the synthetic method is simpler, morphology controllable, in the sponge foam shape that structure is uniform, has hierarchical structure.
3, the nitrogen-doped carbon foam combination electrode material that the present invention obtains has long service life, charge-discharge performance good,
With larger specific capacitance.
Description of the drawings
Fig. 1 is the surface sweeping electron microscope of melamine foamed plastic used in embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of gained nitrogen-doped carbon foam combination electrode material in embodiment 2.
Fig. 3 is the scanning electron microscope (SEM) photograph of gained nitrogen-doped carbon foam combination electrode material in embodiment 3.
Fig. 4 is the charge and discharge time graph of gained nitrogen-doped carbon foam combination electrode material in embodiment 3.
Fig. 5 is the scanning electron microscope (SEM) photograph of gained nitrogen-doped carbon foam combination electrode material in embodiment 4.
The cycle for the nitrogen-doped carbon foam combination electrode material that Fig. 6 is melamine foamed plastic through calcining and embodiment obtains
Volt-ampere curve figure.
The Raman for the nitrogen-doped carbon foam combination electrode material that Fig. 7 is melamine foamed plastic through calcining and embodiment obtains
Spectrogram.
Specific implementation mode
Below by specific embodiment and in conjunction with attached drawing, the present invention will be further described, it should be noted that this is specific
Embodiment does not constitute the limitation to the claimed scope of the invention.
Charge and discharge using blue electric battery test system to the three-dimensional nitrogen-doped carbon foam combination electrode material obtained by the present invention
Electrical property is tested, and steps are as follows：
It calculates in mass ratio, a kind of three-dimensional nitrogen-doped carbon foam combination electrode material of present invention gained：Conductive black：It is viscous
It is 8 to connect agent (PTFE):1:1 ratio is mixed, and the mixture of gained, which is added in absolute ethyl alcohol, is stirred by ultrasonic 30-60min,
The slurry of gained film in the nickel foam cut out and handled well in advance, film area are about 1cm2, the foam of film will be coated
Nickel is placed in 60-80 DEG C of baking oven and dries 10-12h, obtains applying the nickel foam of three-dimensional nitrogen-doped carbon foam, weighs and subtract
Nickel foam net weight obtains applying the quality of three-dimensional nitrogen-doped carbon foam combination electrode material；
Using the nickel foam for being coated with three-dimensional nitrogen-doped carbon foam combination electrode material of above-mentioned gained as working electrode, with blank
Nickel foam is used as to electrode, using saturated calomel electrode as reference electrode, is formed three-electrode system, is added in three electrode glass electrolytic cells
Enter 6M KOH aqueous solutions as electrolyte, respectively by working electrode, blank nickel foam is put into three electrodes to electrode and reference electrode
In glass electrolytic cell, corresponding test mouth is picked out, constant current charge-discharge loop test, charge and discharge instrument are carried out using blue electric charge and discharge instrument
It is picked out using alligator clip.
Required absolute ethyl alcohol is that analysis is pure in various embodiments of the present invention, other reagents are that chemistry is pure, are bought in traditional Chinese medicines
Solution on Chemical Reagents in Shanghai company of group.
Embodiment 1
A kind of three-dimensional nitrogen-doped carbon foam combination electrode material, method as follows are prepared：
(1) by the FeCl of 5mmol3.6H2In the hydrochloric acid solution of O and 20ml 1mol/l, and 200W ultrasounds are used at room temperature
30min；
(2) melamine foamed plastic that size is 3 × 3 × 3cm is immersed in step (1) in mixed solution, and 0.5g is added
Aniline monomer, stir 12h at 20 DEG C；
(3) by step (2) product deionized water and after absolute ethyl alcohol washs, be then dried in vacuo at 90 DEG C
12h；
(4) by treated in step (3), product rises to 900 DEG C with 5 DEG C of heating rate, calcines under nitrogen protection
2h, cooled to room temperature is to get to three-dimensional nitrogen-doped carbon foam combination electrode material later.
Using S-3400N electron microscopes (Hitachi) to the table of melamine foamed plastic (MS) used in above-described embodiment 1
Face structure is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in Figure 1, from figure 1 it appears that melamine foamed plastic used
(MS) it is foam sponge shape structure, and there is larger gap, the surface of material is relatively smooth.
Embodiment 2
A kind of three-dimensional nitrogen-doped carbon foam combination electrode material, method as follows are prepared：
(1) by the FeCl of 5mmol3.6H2In the hydrochloric acid solution of O and 20ml 1mol/l, and 200W ultrasounds are used at room temperature
30min；
(2) melamine foamed plastic that size is 3 × 3 × 3cm is immersed in step (1) in mixed solution, and is added 1g's
Aniline monomer stirs 12h at 30 DEG C；
(3) by step (2) product deionized water and after absolute ethyl alcohol washs, be then dried in vacuo at 60 DEG C
12h；
(4) by treated in step (3), product rises to 900 DEG C with 5 DEG C of heating rate, calcines under nitrogen protection
2h, later cooled to room temperature be named as MS-PANi-1 to get to three-dimensional nitrogen-doped carbon foam combination electrode material.
Using S-3400N electron microscopes (Hitachi) to the nitrogen-doped carbon foam combination electrode material of 2 gained of above-described embodiment
The surface texture of material is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in Fig. 2, from figure 2 it can be seen that nitrogenous conductive material
(polyaniline) is uniformly covered on the surface of carbon foam, while sample has larger hole, shows that we are successfully prepared out
Nitrogen-doped carbon foam combination electrode material.
Embodiment 3
A kind of three-dimensional nitrogen-doped carbon foam combination electrode material, method as follows are prepared：
(1) by the FeCl of 10mmol3.6H2In the hydrochloric acid solution of O and 20ml 1mol/l, and 200W ultrasounds are used at room temperature
30min；
(2) melamine foamed plastic that size is 3 × 3 × 3cm is immersed in step (1) in mixed solution, and 1.5g is added
Aniline monomer, stir 12h at 30 DEG C；
(3) by step (2) product deionized water and after absolute ethyl alcohol washs, be then dried in vacuo at 60 DEG C
12h；
(4) by treated in step (3), product rises to 900 DEG C with 5 DEG C of heating rate, calcines under nitrogen protection
2h, later cooled to room temperature be named as MS-PANi-2 to get to three-dimensional nitrogen-doped carbon foam combination electrode material.
Using S-3400N electron microscopes (Hitachi) to the nitrogen-doped carbon foam combination electrode material of 3 gained of above-described embodiment
The surface texture of material is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in figure 3, from figure 3, it can be seen that nitrogenous conductive material
(polyaniline) is uniformly covered on the surface of carbon foam, while sample has larger hole, shows that we are successfully prepared out
Nitrogen-doped carbon foam combination electrode material.
Three-electrode system is selected at ambient temperature using blue electric battery test system, is electrolysis with 6M KOH aqueous solutions
Liquid tests the capacitor chemical property of the three-dimensional nitrogen-doped carbon foam combination electrode material of 3 gained of above-described embodiment,
The charging and discharging curve figure of the electrode material is obtained, as shown in figure 4, obtaining the charging time and discharge time of the electrode material by figure
It is of substantially equal, and the charge and discharge time is longer, has preferable charge-discharge performance, may be used as electrode material for super capacitor.
Embodiment 4
A kind of three-dimensional nitrogen-doped carbon foam combination electrode material, method as follows are prepared：
(1) by the FeCl of 15mmol3.6H2In the hydrochloric acid solution of O and 20ml 1mol/l, and 200W ultrasounds are used at room temperature
30min；
(2) melamine foamed plastic that size is 3 × 3 × 3cm is immersed in step (1) in mixed solution, and 1.5g is added
Aniline monomer, stir 12h at 30 DEG C；
(3) by step (2) product deionized water and after absolute ethyl alcohol washs, be then dried in vacuo at 60 DEG C
12h；
(4) by treated in step (3), product rises to 900 DEG C with 5 DEG C of heating rate, calcines under nitrogen protection
2h, later cooled to room temperature be named as MS-PANi-3 to get to three-dimensional nitrogen-doped carbon foam combination electrode material.
Using S-3400N electron microscopes (Hitachi) to the nitrogen-doped carbon foam combination electrode material of 4 gained of above-described embodiment
The surface texture of material is scanned, and the scanning electron microscope (SEM) photograph of gained is as shown in figure 5, from figure 5 it can be seen that nitrogenous conductive material
(polyaniline) is uniformly covered on the surface of carbon foam, while sample has larger hole, shows that we are successfully prepared out
Nitrogen-doped carbon foam combination electrode material.
Three-electrode system is selected at ambient temperature using blue electric battery test system, is electrolysis with 6M KOH aqueous solutions
Liquid, to the capacitor electrochemistry of the poly cyanamid foam after calcining and the nitrogen-doped carbon foam combination electrode material prepared by embodiment
Performance is tested, and the cyclic voltammetry curve of the capacitor is obtained, as shown in fig. 6, as ultracapacitor in use, not having substantially
There is fake capacitance effect；While the result shows that, under identical potential, its current density higher of the carbon material of nitrogen doped, table
Bright its possesses the specific capacitance of bigger, and chemical property is obviously improved.
Using laser Raman spectrometer to the melamine foamed plastic after calcining and the nitrogen-doped carbon foam prepared by embodiment
Combination electrode material is measured, and the Raman spectrogram of gained is as shown in fig. 7, it can be seen from figure 7 that MS, MS- in figure
The I of PANi-1, MS-PANi-2, MS-PANi-3D/IGRatio is followed successively by：1.28,1.31,1.35,1.30, wherein MS-PANi-2
Corresponding ID/IGRatio highest is graphitized Chengdu highest.
In conclusion the present invention provides a kind of three-dimensional nitrogen-doped carbon foam combination electrode material, with controllable three-dimensional
Pattern, and crystallinity is good, there are hierarchical structures, while it has many advantages, such as that good cycling stability, charge-discharge performance are excellent, can
To be used as the electrode material of ultracapacitor.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the technical principles of the invention, several improvement can also be made, these improvement also should be regarded as this
The protection domain of invention.
Claims (8)
1. a kind of preparation method of three-dimensional nitrogen-doped carbon foam combination electrode material, which is characterized in that be as follows：
(1) ferric chloride hexahydrate of 5-15mmol is added in the hydrochloric acid of 15-25ml 0.5-1.5mol/l, ultrasonic 30-
60min；
(2) melamine foamed plastic is immersed in step (1) in mixed solution, and the aniline monomer of 0.1-2g is added, at 20-50 DEG C
At a temperature of stir 10-24h；
(3) by step (2) product deionized water and after absolute ethyl alcohol washs, be then dried in vacuo 12- at 20-90 DEG C
24h；
(4) by treated in step (3), product rises to 700-900 DEG C with 5-8 DEG C of heating rate, under inert gas protection
1-2h is calcined, cooled to room temperature is to get to three-dimensional nitrogen-doped carbon foam combination electrode material later.
2. preparation method as described in claim 1, which is characterized in that in step (1), ultrasonic power 200-500W.
3. preparation method as described in claim 1, which is characterized in that in step (2), mixing speed should be 100-800r/min
Be slowly stirred.
4. preparation method as described in claim 1, which is characterized in that in step (2), the size of melamine foamed plastic is 2 × 2
×2-5×5×5cm3。
5. preparation method as described in claim 1, which is characterized in that in step (2), the quality of aniline monomer is 0.5-
1.5g。
6. preparation method as described in claim 1, which is characterized in that in step (2), temperature is 20-35 DEG C.
7. preparation method as described in claim 1, which is characterized in that in step (4), inert gas is to appoint in nitrogen or helium
It is a kind of.
8. three-dimensional nitrogen-doped carbon foam combination electrode material made from a kind of preparation method as described in one of claim 1-7.
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| CN109360992A (en) * | 2018-10-23 | 2019-02-19 | 青岛科技大学 | A kind of metal-nitrogen-carbon nanosheet preparation method and application of three-dimensional continuous carbon skeleton adulteration |
| CN109671921A (en) * | 2018-11-05 | 2019-04-23 | 欣旺达电子股份有限公司 | Stannic oxide/carbon flexible self-supporting composite material preparation method and application |
| CN109698341A (en) * | 2018-12-27 | 2019-04-30 | 银隆新能源股份有限公司 | A kind of electrode preparation method, electrode and battery |
| CN110033953A (en) * | 2019-04-22 | 2019-07-19 | 山东建筑大学 | A kind of functionalization carbon cloth conductive substrates and the preparation method and application thereof |
| CN112002563A (en) * | 2020-07-07 | 2020-11-27 | 浙江工业大学 | Method for preparing foam carbon-based flexible electrode material based on supercritical fluid technology |
| CN115818790A (en) * | 2022-11-08 | 2023-03-21 | 中国石油大学(华东) | Three-dimensional porous metal-free electrode, and preparation method and application thereof |
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| CN115818790A (en) * | 2022-11-08 | 2023-03-21 | 中国石油大学(华东) | Three-dimensional porous metal-free electrode, and preparation method and application thereof |
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Application publication date: 20180814 |