CN110289178A - Two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material and its application - Google Patents
Two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material and its application Download PDFInfo
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- CN110289178A CN110289178A CN201910392012.6A CN201910392012A CN110289178A CN 110289178 A CN110289178 A CN 110289178A CN 201910392012 A CN201910392012 A CN 201910392012A CN 110289178 A CN110289178 A CN 110289178A
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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
- H01G11/26—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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- 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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- 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 nanocomposite preparation technical fields, it is related to a kind of two-step method and prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: disperses nickel acetate, cobalt acetate and N doping carbon dots in deionized water and be stirred into mixed solution；It is subsequently placed in reaction kettle, 170~190 DEG C of 8~12 h of reaction are cooled to room temperature, separating, washing, drying obtain presoma；It is finally placed in tube furnace, is warming up to 300~400 DEG C in an inert atmosphere, calcine 1~3 h, after cooling to obtain the final product.Electrode of the present invention also by obtained composite material, applied to supercapacitor.Operation of the present invention simple process, raw material is cheap, is easy to industrializing implementation.Prepared thickness of composite material is only several nanometers, has ultra-high capacity characteristic, in 1 A/g, 1775 F/g of its specific capacitance, still there is good stability after recharge-discharge 10000 times circulations, while there is excellent capacitive property, had a good application prospect in supercapacitor field.
Description
Technical field
The invention belongs to nanocomposite preparation technical fields, are related to the preparation of electrode material, in particular to one kind two
Footwork prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material and its application.
Background technique
Currently, the electrochemical energy storage technology found efficiently, inexpensive is especially urgent, wherein battery, fuel cell and electrification
It learns supercapacitor and has obtained extensive concern.Compared to battery and fuel cell, supercapacitor possesses longer cycle life
With wide operating temperature range, and higher power density, fast charging rate can be provided, be subjected to people increasingly
More concerns.Important component of the electrode material as supercapacitor directly determines the performance of supercapacitor.Therefore,
The emphasis that preparation is cheap, environmentally friendly, high performance electrode material is current supercapacitor research.
Transition metal oxide is caused people and is greatly paid close attention to due to cheap and environmental-friendly.In these materials, have
There are the NiO and the preferable Co of stability of superelevation theoretical capacity3O4The broad interest of researcher is attracted.With single component oxide NiO
Or Co3O4It compares, NiO/Co3O4Compound can combine NiO and Co3O4The advantages of, richer redox active position is provided
Point, and show bigger electro-chemical activity.
Although transistion metal compound is furtherd investigate always as electrode material, there are poorly conductives and storage for itself
The disadvantages of volume change is big during energy causes the cycle life of these materials and high rate performance not ideal.In order to overcome
These disadvantages usually improve its chemical property for these transistion metal compounds and carbon material are compound.The addition of carbon material
The specific surface area, electric conductivity and surface wettability of transistion metal compound can be increased.But and not all carbon component all can
It plays a positive role to composite material chemical property, since the capacitor of carbon material itself is smaller, excessive carbon component can drop
Low whole performance；Also, fine and close carbon-coating may hinder the reaction between metal compound particles and electrolyte.
Carbon dots are called carbon quantum dot, are a new class of carbon allotropes formed by intensive carbon atom, by sp2/sp3
The carbon atom of hydridization forms, and is the spheric granules of monodisperse, zero dimension.A large amount of function functional group is contained on carbon dots surface, has height
Regulatable surface chemistry is spent, there are also overstable photoluminescence properties, become a kind of attractive material, closely
Nian Lai is widely used in fields such as bio-imaging, photodetector and photocatalysis.In addition, carbon dots are also considered to be kind
Novel environmental protection electrode material, typically exhibits stronger hydrophily, it improves the electron-transport of electrode material, ion fortune
It is dynamic, and the contact area between electrode and electrolyte is expanded, the new opplication in energy conversion and storage, flexible apparatus also obtains
To more and more concerns.In recent years, different types of carbon dots have been successfully applied to energy energy storage field, such as lithium-ion electric
Pond, sodium-ion battery, supercapacitor and fuel cell field.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is with nickel acetate, cobalt acetate, N doping carbon dots
(NCDs) it is raw material, nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer is prepared by hydro-thermal-heat treatment two-step method
Plate electrode material.
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, including as follows
Step:
(1) it disperses nickel acetate, cobalt acetate and N doping carbon dots in 35 mL deionized waters and is stirred into mixed solution；
(2) mixed solution is placed in reaction kettle, 170~190 DEG C of reactions 8~12 h, preferably 10 h are cooled to room temperature, separation
Washing, drying, obtain presoma；
(3) presoma is placed in tube furnace, is warming up to 300~400 in an inert atmosphere with the heating rate of 2 DEG C/min
DEG C, calcine 1~3 h, preferably 350 DEG C 2 h of calcining, after cooling to obtain the final product.
In the more excellent disclosed example of the present invention, step (1) the N doping carbon dots are used using citric acid, ethylenediamine as raw material
Hydro-thermal method is prepared, and existing patent CN109545575 discloses synthetic method, specifically: by 1.05 g citric acids and 335 μ L
Ethylenediamine is dissolved in 10 mL deionized waters, and mixed solution is transferred in reaction kettle in 220 DEG C of 12 h of reaction, N doping is obtained
Carbon dots.
In the more excellent disclosed example of the present invention, the total amount of step (1) nickel acetate and cobalt acetate is 0.5 g, mass ratio 4:1
~1:4.
In the more excellent disclosed example of the present invention, the quality of step (1) the N doping carbon dots is 2~6 mg.
In the more excellent disclosed example of the present invention, step (3) inert atmosphere is argon gas or nitrogen.
Nickel oxide/cobaltosic oxide made from the method/N doping carbon dots composite material according to the present invention, pattern is super
Thin nanometer sheet two-dimensional structure, with a thickness of several nanometers.
A further object of the invention is the electrode by obtained composite material, applied to supercapacitor.
Beneficial effect
Operation of the present invention simple process, raw material is cheap, is easy to industrializing implementation.Prepared nickel oxide/cobaltosic oxide/nitrogen is mixed
Miscellaneous carbon dots ultrathin nanometer piece thickness is only several nanometers, and the capacitance characteristic with superelevation, in 1 A/g, specific capacitance is up to 1775
F/g in addition, the composite material still has good stability after recharge-discharge 10000 times circulations, while having excellent
Capacitive property has a good application prospect in supercapacitor field.
Detailed description of the invention
Fig. 1 is nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material X- prepared by embodiment 1
X ray diffraction (XRD) map.
Fig. 2 is that nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material prepared by embodiment 1 is swept
Retouch Electronic Speculum (SEM) photo.
Fig. 3 is that nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material prepared by embodiment 1 is saturating
Radio mirror (TEM) photo.
Fig. 4 is nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material of the preparation of embodiment 1 in 3 M
The charging and discharging curve tested in KOH electrolyte.
Fig. 5 is nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material of the preparation of embodiment 1 15
A g-1Current density under charge and discharge 10000 times cyclical stability figures.
Specific embodiment
The embodiment of the present invention is described in detail with reference to the accompanying drawing, but protection scope of the present invention is not limited to these
Embodiment.
In disclosed embodiment of this invention, N doping carbon dots (NCDs) the preparation method comprises the following steps: by 1.05 g citric acids and
335 μ L ethylenediamines are dissolved in 10 mL deionized waters, and mixed solution is transferred in reaction kettle in 220 DEG C of 12 h of reaction, is obtained
N doping carbon dots.
Embodiment 1
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.2 g
Nickel acetate, 0.3 g cobalt acetate and 4 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 180 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 350 DEG C under argon gas with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.
Fig. 1 is the XRD diagram of composite material, it can be seen that nickel oxide corresponds to cubic system NiO(JCPDS in composite material:
65-5745), cobaltosic oxide corresponds to cubic system Co3O4(JCPDS:42-1467).
Fig. 2 is that the SEM of composite material schemes, it is clear that composite material is ultra-thin class graphene-structured.
Fig. 3 is that the TEM of composite material schemes, the fold that can be clearly observed on thin slice.While this pattern is almost
Be it is transparent, show that there is ultra-thin property, thickness is only several nanometers.The nano-complex ultrathin nanometer piece is by a large amount of nanometer
Particle composition, wherein lattice fringe is 0.245 nm and 0.15 nm, with Co3O4(311) face and NiO (220) crystal face it is good
Matching.The lattice fringe of 0.22 nm can belong to (100) crystal face of N doping carbon dots.
Fig. 4 is composite material in 3 M KOH electrolyte, the charge and discharge tested using mercury/mercuric oxide electrode as reference electrode
Curve.It is from left to right followed successively by charging and discharging curve when 20 A/g, 15 A/g, 10 A/g, 5 A/g, 2 A/g and 1 A/g, this is multiple
Condensation material shows excellent capacitive property, and in 1 A/g, specific capacitance is up to 1775 F/g.
Fig. 5 shows that in 3 M KOH electrolyte, current density is 15 A g-1When recharge-discharge 10000 times circulations
Curve can be clearly seen that the electrode material has good cyclical stability.
Embodiment 2
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.4 g
Nickel acetate, 0.1 g cobalt acetate and 4 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 180 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 350 DEG C under argon gas with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 941 F/g.
Embodiment 3
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.25
G nickel acetate, 0.25 g cobalt acetate and 4 mg N doping carbon dots are scattered in 35 mL deionized waters；Acquired solution is placed in 50 mL
In reaction kettle, in 180 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma,
It is warming up to 350 DEG C under argon gas with the heating rate of 2 DEG C/min again, obtains nickel oxide/tetra- oxidations three after calcining 2 h
Cobalt/N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 1450 F/g.
Embodiment 4
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.1 g
Nickel acetate, 0.4 g cobalt acetate and 4 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 180 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 350 DEG C under argon gas with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 1034 F/g.
Embodiment 5
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.2 g
Nickel acetate, 0.3 g cobalt acetate and 2 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 180 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 350 DEG C under argon gas with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 1517 F/g.
Embodiment 6
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.2 g
Nickel acetate, 0.3 g cobalt acetate and 6 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 180 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 300 DEG C under argon gas with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 1626 F/g.
Embodiment 7
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.2 g
Nickel acetate, 0.3 g cobalt acetate and 4 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 170 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 400 DEG C under argon gas with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 1718 F/g.
Embodiment 8
A kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, comprising: by 0.2 g
Nickel acetate, 0.3 g cobalt acetate and 4 mg N doping carbon dots are scattered in 35 mL deionized waters；It is anti-that acquired solution is placed in 50 mL
It answers in kettle, in 190 DEG C of 10 h of reaction；Reaction terminates, and after cooling, by solid sample separating, washing, drying obtains presoma, then
It is warming up to 350 DEG C under a nitrogen with the heating rate of 2 DEG C/min, calcine obtain after 2 h nickel oxide/cobaltosic oxide/
N doping carbon dots ultrathin nanometer plate electrode material.In 1 A/g, specific capacitance is 1753 F/g.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (9)
1. a kind of two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material, feature exists
In including the following steps:
(1) it disperses nickel acetate, cobalt acetate and N doping carbon dots in 35 mL deionized waters and is stirred into mixed solution；
(2) mixed solution is placed in reaction kettle, 170~190 DEG C of 8~12 h of reaction are cooled to room temperature, separating, washing, baking
It is dry, obtain presoma；
(3) presoma is placed in tube furnace, is warming up to 300~400 in an inert atmosphere with the heating rate of 2 DEG C/min
DEG C, calcine 1~3 h, after cooling to obtain the final product.
2. two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material according to claim 1
Material, it is characterised in that: the total amount of step (1) nickel acetate and cobalt acetate is 0.5 g, and mass ratio is 4:1~1:4.
3. two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material according to claim 1
Material, it is characterised in that: the quality of step (1) the N doping carbon dots is 2~6 mg.
4. two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material according to claim 1
Material, it is characterised in that: step (2) is described to be placed in mixed solution in reaction kettle, and 170~190 DEG C of 10 h of reaction are cooled to room
Temperature, separating, washing, drying, obtains presoma.
5. two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material according to claim 1
Material, it is characterised in that: step (3) is described to be placed in presoma in tube furnace, in an inert atmosphere with the heating speed of 2 DEG C/min
Rate is warming up to 350 DEG C of 2 h of calcining, after cooling to obtain the final product.
6. two-step method prepares nickel oxide/cobaltosic oxide/N doping carbon dots ultrathin nanometer plate electrode material according to claim 1
Material, it is characterised in that: step (3) inert atmosphere is argon gas or nitrogen.
7. nickel oxide/cobaltosic oxide that -6 any the methods are prepared according to claim 1/N doping carbon dots are ultra-thin receives
Rice plate electrode material.
8. a kind of nickel oxide/cobaltosic oxide as claimed in claim 7/N doping carbon dots ultrathin nanometer plate electrode material, special
Sign is: pattern is ultrathin nanometer piece two-dimensional structure, with a thickness of several nanometers.
9. a kind of nickel oxide/cobaltosic oxide as described in claim 7 or 8/N doping carbon dots ultrathin nanometer plate electrode material
Using, it is characterised in that: the electrode of supercapacitor will be applied to.
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Application publication date: 20190927 |