CN110364366A - A kind of high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material and preparation method and application - Google Patents
A kind of high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material and preparation method and application Download PDFInfo
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- CN110364366A CN110364366A CN201910582198.1A CN201910582198A CN110364366A CN 110364366 A CN110364366 A CN 110364366A CN 201910582198 A CN201910582198 A CN 201910582198A CN 110364366 A CN110364366 A CN 110364366A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01G11/24—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
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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
- H01G11/46—Metal oxides
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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 discloses a kind of high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material and preparation methods and application.This method comprises the following steps: (1) preparing molybdenum trioxide nano band；(2) polypyrrole is grown in molybdenum trioxide nano belt surface；(3) by under inert atmosphere protection in-situ reducing obtain the high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material.Preparation process of the invention is simple, it is reproducible, product purity is high, pattern is uniform, and the molybdenum dioxide and nitrogen-doped carbon combination electrode material prepared has high specific capacitance in organic electrolyte, and (when sweep speed is up to 2000 mV/s, capacity still is able to retain about 90 C/g, and after 20000 circulations for excellent high rate performance and cyclical stability, about 80%) capacity boost, has very high application value in the energy storage devices such as electrochemical capacitor.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of to prepare high-performance electric chemistry capacitor anode material two
Molybdenum oxide and nitrogen-doped carbon composite material and preparation method and application.
Background technique
As a large amount of consumption of fossil fuel have caused a series of environmental problem, brought to the environment of the earth huge
It influences, therefore finding new renewable energy is to maintain the important channel of human kind sustainable development.But these renewable energy
Such as solar energy, wind energy, vulnerable to the influence of the factors such as weather, geographical location, this intermittence can cause certain rush to power grid
It hits, then just needing to adjust the power swing of smart grid by energy storage device, being by these renewable energy conversions can be steady
Surely the energy exported.In these energy storage devices, electrochemical capacitor due to being capable of providing energy more higher than traditional capacitor,
Power more higher than secondary cell and cycle life, in smart grid, the various fields such as rail traffic and new-energy automobile are undertaken
Important role, however electrode material be the key that determine its performance parameter.MoO2Due to good electric conductivity, chemistry
The advantages that stability is good, and theoretical capacity is high has extensive research in terms of lithium ion battery negative material, but also faces all
More problems, kinetic reaction is slow in charge and discharge process, it is difficult to realize fast charging and discharging, and in process of intercalation, be easy
Volume expansion occurs, material is destroyed, so as to shorten cycle life.
Summary of the invention
The purpose of the present invention is to provide a kind of high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbons
Composite material and preparation method and application.The preparation process of this method is simple, reproducible, and product purity is high, and pattern is uniform,
It is easy to large-scale production, and the molybdenum dioxide and nitrogen-doped carbon combination electrode material that prepare have high ratio in organic lithium salt
Capacitor, excellent high rate performance and cyclical stability have very high using valence in the energy storage devices such as electrochemical capacitor
Value.
The purpose of the present invention is realized at least through one of following technical solution.
A kind of preparation method of high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material, tool
Body includes the following steps:
(1) molybdenum trioxide nano band is prepared；(2) polypyrrole is grown in molybdenum trioxide nano belt surface；(3) by inert atmosphere
Lower in-situ reducing is protected to obtain molybdenum dioxide and nitrogen-doped carbon composite material.
Further, in step (1), the process for preparing molybdenum trioxide nano band is into cold bath or ice bath environment
Hydrogenperoxide steam generator in be added molybdenum powder, molybdenum trioxide nano band is obtained by hydro-thermal reaction after oxidation reaction.
Further, in step (2), the detailed process in molybdenum trioxide nano belt surface growth polypyrrole are as follows: will
The molybdenum trioxide nano band obtained in step (1) is evenly dispersed in water, then sequentially adds pyrrole monomer and ammonium persulfate
Polymerization reaction is carried out, obtains the molybdenum trioxide nano band of surface growth polypyrrole by suction filtration, washing and drying.
Further, in the step (2) molar ratio of pyrrole monomer used in growth polypyrrole and ammonium persulfate be 1:1~
4:1, polymerization time are 1 ~ 24 h, and the mass ratio of molybdenum trioxide and pyrrole monomer is 2:1~1:2, and the concentration of pyrroles is 10 ~ 20
mmol/L。
Further, the temperature of in-situ reducing described in the step (3) is 400~600 DEG C, time of heat preservation is 1~
10 h, the speed of heating are 1 ~ 10 DEG C/min.
Further, inert atmosphere described in the step (3) is nitrogen or argon gas.
The high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon obtained by above-mentioned preparation method
Composite material.
The high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material are in manufacture capacitor
In application, the electrolyte of the capacitor is lithium salts.
The present invention utilizes in-situ reducing technology, has obtained that pattern is uniform, and the molybdenum dioxide and nitrogen-doped carbon of high-purity are compound
Nano material, the negative electrode material for being used for electrochemical capacitor has the ability of fast charging and discharging, and specific capacitance is high, circulation
Service life is long.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) method that the present invention prepares high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material,
Process is simple, reproducible, and product purity is high, and pattern is uniform, environmental-friendly, is easy to large-scale production, and practical value is high.
(2) molybdenum dioxide prepared by the present invention and nitrogen-doped carbon combination electrode material are carbon-coated nanometer band structure, are led
Electrically good, steady chemical structure has high specific capacitance, excellent high rate performance and cyclical stability in organic electrolyte
(when sweep speed is up to 2000 mV/s, capacity still is able to retain 90 C/g, and after 20000 circulations, capacity boost
About 80%), there is very high application value in the energy storage devices such as electrochemical capacitor.
Detailed description of the invention
Fig. 1 is X-ray powder diffraction (XRD) figure of N doping molybdenum carbide and carbon composite nano-material that embodiment 1 obtains；
Fig. 2 is high magnification scanning electron microscope (SEM) photo of the molybdenum dioxide that embodiment 1 obtains and nitrogen-doped carbon composite material；
Fig. 3 is transmission electron microscope (TEM) photo of the molybdenum dioxide that embodiment 1 obtains and nitrogen-doped carbon composite material；
Fig. 4 is that the circulation of the molybdenum dioxide that embodiment 1 obtains and nitrogen-doped carbon combination electrode material under different scanning rates lies prostrate
Pacify curve；
Fig. 5 be the obtained molybdenum dioxide of embodiment 1 with nitrogen-doped carbon combination electrode material the corresponding appearance under different scanning rates
Amount；
Fig. 6 is the molybdenum dioxide that embodiment 1 obtains and nitrogen-doped carbon combination electrode material under the high sweep speed of 50 mV/s
Long-term cycle stability test.
Specific embodiment
The present invention will be further described below by way of examples, but the present invention is not restricted to following embodiment.
Embodiment 1
It takes 10 mL hydrogenperoxide steam generators (30%) to be placed in ice bath in 200 mL beakers, 1g molybdenum is slowly added into beaker
Powder completely after reaction, then adds 20 mL H into beaker2O is diluted, and stirs 30 min.It is then transferred into reaction kettle in drum
The white precipitate of acquisition is washed with deionized drying, obtained by 200 DEG C of 24 h of heat preservation, cooled to room temperature in wind baking oven
Molybdenum trioxide nano band presoma.
Molybdenum trioxide nano band presoma is distributed to 30 min of magnetic agitation in deionized water, is placed in ice bath, three oxygen
The mass ratio control for changing molybdenum and pyrrole monomer is 1:1, and pyrrole monomer is added and continues to stir 30 min, the concentration of pyrroles is controlled 15
Ammonium persulfate is added in mmol/L, and the molar ratio control of pyrroles and ammonium persulfate are 2:1,12 h of magnetic agitation, are filtered by vacuum, use
It is dried after deionized water and ethanol washing.Then it is raised in tube furnace under nitrogen atmosphere protection with the heating rate of 1 DEG C/min
600 DEG C, 4 hours are kept the temperature, room temperature is down to naturally, obtains molybdenum dioxide and nitrogen-doped carbon combination electrode material.
The XRD spectrum of the combination electrode material is as shown in Fig. 1, obtained diffraction maximum and standard card 32-0671 phase
It is corresponding, illustrate to have obtained high-purity monoclinic phase MoO2.Attached drawing 2 is scanning electron microscopic picture, it can be seen that MoO2In nanometer band structure,
Pattern is uniform.Attached drawing 3 is transmission electron microscope photo, it can be clearly seen that carbon-coating is uniformly coated on MoO2Surface.
It is carried out using the molybdenum dioxide of preparation and nitrogen-doped carbon combination electrode material as the negative electrode material of electrochemical capacitor
Electrochemical Characterization is as follows: being tested using two electrode systems, wherein electrolyte is the LiClO of 1 M4, it is lithium to electrode
Piece.Cyclic voltammetry curve under different scanning rates as shown in figure 4, with sweep speed increase, the shape of cyclic voltammetry curve
Shape is able to maintain substantially, illustrates preferable high rate performance.Corresponding capacity under different scanning rates is as shown in figure 5, in 1 mV/
Under the sweep speed of s, the molybdenum dioxide of preparation and the capacity of nitrogen-doped carbon combination electrode can reach 1317 C/g, when scanning speed
Capacity still is able to retain about 90 C/g when rate is up to 2000 mV/s, shows good fast charging and discharging ability.Fig. 6 is preparation
Molybdenum dioxide and long-term cycle stability test result of the nitrogen-doped carbon combination electrode under high sweep speed, in 50 mV/s
High sweep speed under, by during 20000 circulations, capacity is slowly increased (capacity boost about 80%) in preceding 8000 circle, so
It keeps stablizing afterwards, has shown the cycle life of overlength.
Embodiment 2
The band presoma of molybdenum trioxide nano obtained in embodiment 1 is distributed to 30 min of magnetic agitation in deionized water, is placed in
In ice bath, the mass ratio control of molybdenum trioxide nano band and pyrrole monomer is 2:1, and pyrrole monomer is added and continues to stir 30 min,
In 10 mmol/L ammonium persulfate is added, the molar ratio control of pyrroles and ammonium persulfate are 2:1, and magnetic force stirs in the concentration control of pyrroles
1 h is mixed, is filtered by vacuum, with being dried after deionized water and ethanol washing.Then in tube furnace nitrogen atmosphere protection under with 5 DEG C/
The heating rate of min is raised to 500 DEG C, keeps the temperature 1 hour, is down to room temperature naturally, obtains molybdenum dioxide and nitrogen-doped carbon combination electrode
Material.
MoO in the combination electrode material2In nanometer band structure, pattern is uniform (referring to Fig. 2), and carbon-coating uniformly coats
In MoO2Surface (refer to Fig. 3).
Embodiment 3
The band presoma of molybdenum trioxide nano obtained in embodiment 1 is distributed to 30 min of magnetic agitation in deionized water, is placed in
In ice bath, the mass ratio control of molybdenum trioxide nano band and pyrrole monomer is 1:2, and pyrrole monomer is added and continues to stir 30 min,
In 15 mmol/L ammonium persulfate is added, the molar ratio control of pyrroles and ammonium persulfate are 4:1, and magnetic force stirs in the concentration control of pyrroles
12 h are mixed, are filtered by vacuum, with being dried after deionized water and ethanol washing.Then with 5 under nitrogen atmosphere is protected in tube furnace
DEG C/heating rate of min is raised to 600 DEG C, 5 hours are kept the temperature, room temperature is down to naturally, it is compound with nitrogen-doped carbon to obtain molybdenum dioxide
Electrode material.
MoO in the combination electrode material2In nanometer band structure, pattern is uniform (referring to Fig. 2), and carbon-coating uniformly coats
In MoO2Surface (refer to Fig. 3).
Embodiment 4
The band presoma of molybdenum trioxide nano obtained in embodiment 1 is distributed to 30 min of magnetic agitation in deionized water, is placed in
In ice bath, the mass ratio of molybdenum trioxide nano band and pyrrole monomer is 2:1, and pyrrole monomer is added and continues to stir 30 min, pyrroles
Concentration control in 20 mmol/L, ammonium persulfate is added, the molar ratio control of pyrroles and ammonium persulfate are 1:1, magnetic agitation 24
H, vacuum filtration, with being dried after deionized water and ethanol washing.Then with 10 DEG C/min under nitrogen atmosphere is protected in tube furnace
Heating rate be raised to 400 DEG C, keep the temperature 10 hours, be down to room temperature naturally, obtain molybdenum dioxide and nitrogen-doped carbon combination electrode material
Material.
MoO in the combination electrode material2In nanometer band structure, pattern is uniform (referring to Fig. 2), and carbon-coating uniformly coats
In MoO2Surface (refer to Fig. 3).
The foregoing is only a preferred embodiment of the present invention, not does restriction in any form to the present invention.It is all
Any equivalent variation that those skilled in the art makes above-described embodiment using technical solution of the present invention is modified or is drilled
Become etc., all of which are still within the scope of the technical scheme of the invention.
Claims (9)
1. a kind of preparation method of high-performance electric chemistry capacitor anode material molybdenum dioxide and nitrogen-doped carbon composite material, special
Sign is, includes the following steps: that (1) prepares molybdenum trioxide nano band；(2) polypyrrole is grown in molybdenum trioxide nano belt surface；
(3) by under inert atmosphere protection in-situ reducing obtain the molybdenum dioxide and nitrogen-doped carbon composite material.
2. preparation method according to claim 1, which is characterized in that described to prepare molybdenum trioxide nano band in step (1)
Process be that molybdenum powder is added in hydrogenperoxide steam generator into cold bath or ice bath environment, obtained after oxidation reaction by hydro-thermal reaction
To molybdenum trioxide nano band.
3. preparation method according to claim 1, which is characterized in that described in molybdenum trioxide nano band table in step (2)
It looks unfamiliar the detailed process of long polypyrrole are as follows: the molybdenum trioxide nano band obtained in step (1) is evenly dispersed in water, then
It sequentially adds pyrrole monomer and ammonium persulfate carries out polymerization reaction, obtain surface growth polypyrrole by suction filtration, washing and drying
Molybdenum trioxide nano band.
4. preparation method according to claim 3, which is characterized in that 1 ~ 24 h of polymerization reaction, molybdenum trioxide nano band with
The mass ratio of pyrrole monomer is 1:2~2:1, and the molar ratio of pyrroles and ammonium persulfate is 1:1~4:1；The concentration of pyrroles is 10 ~ 20
mmol/L。
5. preparation method according to claim 1, which is characterized in that in step (3), the temperature of the in-situ sintering reduction
It is 400 DEG C~600 DEG C, keeps the temperature 1~10 h, and the speed to heat up is 1 ~ 10 DEG C/min.
6. preparation method according to claim 1, which is characterized in that inert atmosphere described in step (3) is nitrogen or argon
Gas.
7. high-performance electric chemistry capacitor anode material molybdenum dioxide made from any one of the claim 1-6 preparation method and
Nitrogen-doped carbon composite material.
8. the application of molybdenum dioxide described in claim 7 and nitrogen-doped carbon composite material in manufacture capacitor.
9. application according to claim 8, which is characterized in that the electrolyte of the capacitor is lithium salts.
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Cited By (5)
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| CN112850789A (en) * | 2021-01-05 | 2021-05-28 | 西南大学 | Metal oxide/nitrogen-phosphorus co-doped carbon composite material, preparation method thereof and application thereof in negative electrode material of sodium-ion battery |
| CN114420459A (en) * | 2022-01-06 | 2022-04-29 | 重庆文理学院 | Carbon/manganese dioxide composite material for super capacitor and preparation method thereof |
| CN114743807A (en) * | 2022-05-19 | 2022-07-12 | 江苏大学 | Inside and outside raw MoO2Preparation method of/three-dimensional carbon composite material |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
| CN115092962A (en) * | 2022-05-20 | 2022-09-23 | 江苏师范大学 | Molybdenum dioxide/carbon composite electrode material and preparation method and application thereof |
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| CN112850789A (en) * | 2021-01-05 | 2021-05-28 | 西南大学 | Metal oxide/nitrogen-phosphorus co-doped carbon composite material, preparation method thereof and application thereof in negative electrode material of sodium-ion battery |
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| CN115092962A (en) * | 2022-05-20 | 2022-09-23 | 江苏师范大学 | Molybdenum dioxide/carbon composite electrode material and preparation method and application thereof |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
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