CN109786135A - A kind of copper oxide@nickel molybdate/foam copper combination electrode material and preparation method thereof - Google Patents
A kind of copper oxide@nickel molybdate/foam copper combination electrode material and preparation method thereof Download PDFInfo
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- Y02E60/13—Energy storage using capacitors
Abstract
A kind of copper oxide@nickel molybdate/foam copper combination electrode material and preparation method thereof, belongs to field of inorganic nonmetallic material.It is specifically grown in situ on the Kocide SD nano wire on foam copper surface and coats upper nickel-molybdenum presoma, calcining obtains the copper oxide@nickel molybdate/foam copper combination electrode material with nucleocapsid structure under atmosphere of inert gases.The core-shell structure copolymer nanowire array structure is grown directly upon on foam copper, the positive electrode as supercapacitor.For the present invention using copper oxide as core, nickel molybdate is coated on CuO surface as shell, increases the active site for participating in electrochemical process, improves the capacitance of electrode material.The material preparation process is simple, has excellent and stable chemical property, is suitable for the electrode material of supercapacitor, has wide application space in electrode material for super capacitor field.
Description
Technical field
The invention belongs to the preparation technical fields of inorganic non-metallic material, and in particular to a kind of copper oxide@nickel molybdate/foam
Copper combination electrode material and preparation method thereof.
Background technique
Supercapacitor is that one kind has high power density, excellent stable circulation performance and can realize fast charging and discharging
Model electrochemical energy storage device, used and the various fields tool such as storage system in hybrid vehicle, industrial electrical, national defence troops
There is huge potential using value.But its relatively low energy density greatly limits its application.How to design and prepares
Electrode material with excellent electrochemical property is the key point for solving supercapacitor existing issue.
There to be the nanostructure such as metal oxides such as nanometer sheet, nano wire or nanotube to be grown directly upon conductive substrates
On, and as the skeleton or bracket of other oxides, become for preparing the nanocomposite with composite construction
The new development trend of electrode material for super capacitor.
Foam copper as a kind of novel three-dimensional conductive substrates have unique macroporous structure and excellent electric conductivity, gradually by
To the concern of researcher.Pass through distinct methods currently, having focused largely in relation to foam copper in the research of super capacitor material
Preparation oxidation foam copper simultaneously directly grows simple (hydrogen) oxide of copper on its surface.However the capacitance of these electrode materials is big
It is difficult to meet the needs of supercapacitor more, by constructing there are the composite nano materials of nucleocapsid structure can well solve
This problem.
Summary of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, providing that a kind of method is simple, copper oxide@molybdic acid of excellent
Nickel/foam copper combination electrode material and preparation method thereof.
In order to achieve the above object, the present invention is achieved in the following ways:
("@" refers to that nano material is core-shell structure copolymer knot for a kind of preparation method of copper oxide@nickel molybdate/foam copper combination electrode material
Structure, "/" refer to that nano material is grown in conductive substrates surface), including with step:
(1) 15~25mmol sodium hydroxide and 1~3mmol ammonium persulfate are substantially dissolved in 30~50 ml deionized waters
In, it will clean and dried foam copper be immersed in above-mentioned mixed solution, obtain homoepitaxial at room temperature on foam copper surface
Kocide SD nano-wire array, be labeled as Kocide SD nano-wire array/foam copper；
(2) ratio by 1~2mmol nickel nitrate and 1~2mmol sodium molybdate with molar ratio for 1:1 be completely dissolved in 30~
In 50 ml deionized waters, Kocide SD nano-wire array/foam copper obtained by step (1) is immersed in the solution, carries out water
Thermal response, after natural cooling, will gained sample take out after wash and dry；
(3) step (2) products therefrom calcined to obtain copper oxide@nickel molybdate/foam copper compound under atmosphere of inert gases
Electrode material.
Preferably, the molar ratio of sodium hydroxide and ammonium persulfate is 8~20:1 in step (1)；
The temperature of hydro-thermal reaction is 90~120 DEG C in step (2), and the reaction time is 1~6 hour；
Inert gas is one of nitrogen or argon gas in step (3)；
Calcination temperature in step (3) is 350 DEG C~450 DEG C, and calcination time is 2~5 hours.
Present invention growth in situ metal with nucleocapsid structure of nano-scale on foam copper using mild method
Oxide electrode material, copper oxide are core, and nickel molybdate is coated on CuO surface as shell, increase and participate in electrochemical process
Active site improves the capacitance of electrode material.The copper oxide@nickel molybdate/foam copper combination electrode prepared using this method
Material has excellent and stable electrochemical properties, has wide application space in electrode material for super capacitor field.
Compared with prior art, the present invention has following features.
(1) present invention does not need that any conductive agent and adhesive is added, and the foam copper in the present invention is both used as conductive substrates
It is identified oneself in chemical reaction as reactant again, enhances the adhesive force between metal oxide and conductive substrates, reduce electricity
The resistance of pole material improves the electric conductivity of electrode material.
(2) copper oxide in the present invention can contribute the capacitor of entire electrode with nickel molybdate, can increase material
Whole specific capacitance.Meanwhile compared with single cupric oxide nano linear array, molybdic acid nickel nano film can make full use of copper oxide
Remaining space between nano wire increases the contact area with electrolyte, obtains superior chemical property.
(3) the copper oxide@nickel molybdate for obtaining the present invention/foam copper combination electrode carries out electrochemical properties test, 3,
5、8、10、20、40mA/cm2Current density under carry out constant current charge-discharge test respectively obtained 2600,2480,2317,
2177, the specific capacity of 1867,1829F/g.In 10mA/cm2Current density under carry out cyclical stability test 3000 times, remain to
Keep the 97.2% of its initial specific capacitance value.Above-mentioned test result shows that obtained electrode material of the present invention has excellent electrification
Learn property.
(4) the invention is simple and feasible, and raw material is cheap, and preparation process is simple, device dependence is low, and it is big to be suitable for exploitation industrialization
Large-scale production application.
Detailed description of the invention
The X-ray diffraction spectrogram of the foam copper of Kocide SD nano wire is covered in Fig. 1 embodiment 1；
The electron scanning micrograph of the foam copper of Kocide SD nano wire is covered in Fig. 2 embodiment 2；
Fig. 3 is by the X-ray diffraction spectrogram of the copper oxide molybdic acid nickel composite scraped in embodiment 3 from foam copper surface；
The electron scanning micrograph of the foam copper of copper oxide@nickel molybdate is covered in Fig. 4 embodiment 1；
The electron scanning micrograph of the foam copper of copper oxide@nickel molybdate is covered in Fig. 5 embodiment 4；
The electron scanning micrograph of the foam copper of copper oxide@nickel molybdate is covered in Fig. 6 embodiment 5；
Fig. 7 is by the transmission electron microscope of the copper oxide molybdic acid nickel composite scraped in embodiment 6 from foam copper surface
Photo；
Copper oxide@nickel molybdate/foam copper combination electrode cyclic voltammetry curve in Fig. 8 embodiment 1；
Copper oxide@nickel molybdate/foam copper combination electrode constant current charge-discharge curve in Fig. 9 embodiment 1；
Copper oxide@nickel molybdate/foam copper combination electrode circulation cyclical stability test result figure in Figure 10 embodiment 1.
Specific embodiment
The invention will be further described for following specific embodiments, but protection scope of the present invention be not only limited to it is following
The statement of content.
Embodiment 1:
(1) 20mmol sodium hydroxide and 2mmol ammonium persulfate are substantially dissolved in 40 ml deionized waters at room temperature, it will
It cleans and dried foam copper is immersed in above-mentioned mixed solution, obtain Kocide SD/foam carbon/carbon-copper composite material；
(2) 1.5mmol nickel nitrate is sufficiently dissolved in 40 ml deionized waters with 1.5mmol sodium molybdate, by step (1)
Gained Kocide SD nano-wire array/foam copper immerses in the above solution, hydro-thermal reaction 1 hour, natural cooling at 90 DEG C
Afterwards, gained sample is washed and is dried；
(3) step (2) products therefrom is calcined to 2 hours in 350 DEG C of nitrogen atmosphere to copper oxide@nickel molybdate/foam
Copper combination electrode material.
As can be seen that step (1) success is in foam from x-ray diffraction pattern Fig. 1 and electron scanning micrograph Fig. 2
Copper surface has synthesized Kocide SD nano-wire array, which is vertically grown in foam copper surface.Spread out from X-ray
It penetrates spectrogram 3 and electron scanning micrograph Fig. 4, Fig. 5, Fig. 6 and transmission electron microscope photo Fig. 7 can be seen that process
After the hydro-thermal reaction of step (2) and the calcination process of step (3), copper oxide molybdic acid nickel composite material, molybdic acid are successfully synthesized
Nickel nano film is grown directly upon cupric oxide nano line surface, forms the nano-wire array with nucleocapsid structure.In addition, single oxygen
The diameter for changing copper@nickel molybdate core-shell structure copolymer nano wire is about 180~300nm.
Embodiment 2:
(1) 40mmol sodium hydroxide and 2mmol ammonium persulfate are substantially dissolved in 40 ml deionized waters at room temperature, it will
It cleans and dried foam copper is immersed in above-mentioned mixed solution, obtain Kocide SD/foam carbon/carbon-copper composite material；
(2) 1.5mmol nickel nitrate is sufficiently dissolved in 40 ml deionized waters with 1.5mmol sodium molybdate, by step (1)
Gained Kocide SD nano-wire array/foam copper immerses in the above solution, hydro-thermal reaction 2 hours, natural cooling at 90 DEG C
Afterwards, gained sample is washed and is dried；
(3) step (2) products therefrom is calcined to 2 hours in 350 DEG C of nitrogen atmosphere to copper oxide@nickel molybdate/foam
Copper combination electrode material.
The copper oxide@nickel molybdate nano-array obtained under the conditions of embodiment 2 with it is almost the same in embodiment 1.
Embodiment 3:
(1) 20mmol sodium hydroxide and 2mmol ammonium persulfate are substantially dissolved in 40 ml deionized waters at room temperature, it will
It cleans and dried foam copper is immersed in above-mentioned mixed solution, obtain Kocide SD/foam carbon/carbon-copper composite material；
(2) 1.5mmol nickel nitrate is sufficiently dissolved in 40 ml deionized waters with 1.5mmol sodium molybdate, by step (1)
Gained Kocide SD nano-wire array/foam copper immerses in the above solution, hydro-thermal reaction 6 hours, natural cooling at 90 DEG C
Afterwards, gained sample is washed and is dried；
(3) step (2) products therefrom is calcined to 2 hours in 450 DEG C of nitrogen atmosphere to copper oxide@nickel molybdate/foam
Copper combination electrode material.
The copper oxide@nickel molybdate nano-array and embodiment 1 obtained under the conditions of embodiment 3 is obtained essentially identical,
But the nanowire diameter that embodiment 3 obtains can be slightly higher than nanowire diameter obtained in embodiment 1, and (about 330~380nm is left
It is right).
Embodiment 4:
(1) 20mmol sodium hydroxide and 2mmol ammonium persulfate are substantially dissolved in 40 ml deionized waters at room temperature, it will
It cleans and dried foam copper is immersed in above-mentioned mixed solution, obtain Kocide SD/foam carbon/carbon-copper composite material；
(2) 1.5mmol nickel nitrate is sufficiently dissolved in 40 ml deionized waters with 1.5mmol sodium molybdate, by step (1)
Gained Kocide SD nano-wire array/foam copper immerses in the above solution, hydro-thermal reaction 1 hour, natural cooling at 120 DEG C
Afterwards, gained sample is washed and is dried；
(3) step (2) products therefrom is calcined to 2 hours in 350 DEG C of argon atmosphere to copper oxide@nickel molybdate/foam
Copper combination electrode material.
The copper oxide@nickel molybdate nano-array obtained under the conditions of embodiment 4 with it is almost the same in embodiment 1.
Embodiment 5:
(1) 20mmol sodium hydroxide and 2mmol ammonium persulfate are substantially dissolved in 40 ml deionized waters at room temperature, it will
It cleans and dried foam copper is immersed in above-mentioned mixed solution, obtain Kocide SD/foam carbon/carbon-copper composite material；
(2) 1.5mmol nickel nitrate is sufficiently dissolved in 40 ml deionized waters with 1.5mmol sodium molybdate, by step (1)
Gained Kocide SD nano-wire array/foam copper immerses in the above solution, hydro-thermal reaction 4 hours, natural cooling at 90 DEG C
Afterwards, gained sample is washed and is dried；
(3) step (2) products therefrom is calcined to 5 hours in 350 DEG C of nitrogen atmosphere to copper oxide@nickel molybdate/foam
Copper combination electrode material.
The copper oxide@nickel molybdate nano-array obtained under the conditions of embodiment 5 with it is almost the same in embodiment 1.
Embodiment 6:
(1) 40mmol sodium hydroxide and 2mmol ammonium persulfate are substantially dissolved in 40 ml deionized waters at room temperature, it will
It cleans and dried foam copper is immersed in above-mentioned mixed solution, obtain Kocide SD/foam carbon/carbon-copper composite material；
(2) 1mmol nickel nitrate is sufficiently dissolved in 30 ml deionized waters with 1mmol sodium molybdate, it will be obtained by step (1)
Kocide SD nano-wire array/foam copper immerses in the above solution, hydro-thermal reaction 1 hour at 90 DEG C, will after natural cooling
Gained sample is washed and is dried；
(3) step (2) products therefrom is calcined to 5 hours in 450 DEG C of nitrogen atmosphere to copper oxide@nickel molybdate/foam
Copper combination electrode material.
The copper oxide@nickel molybdate nano-array obtained under the conditions of embodiment 6 with it is almost the same in embodiment 1.
Electrochemical properties test:
Work electricity of the copper oxide@nickel molybdate/foam copper combination electrode that embodiment 1 is obtained directly as supercapacitor
Pole carries out electrochemical properties test.
The content of electrochemical properties test includes that cyclic voltammetry, constant current charge-discharge test and cyclical stability are surveyed
Examination.Above all of electrochemical properties test uses Shanghai Chen Hua electrochemical workstation, using three-electrode system, with preparation
Copper oxide@nickel molybdate/foam copper combination electrode is made as working electrode, saturated calomel electrode as reference electrode, platinum plate electrode
For auxiliary electrode.Above-mentioned electrochemical properties test is used in the potassium hydroxide aqueous solution of 2mol/L as electrolyte.
Fig. 8 be the obtained electrode of embodiment 1 as supercapacitor working electrode in -0.2V~0.7V potential windows
The cyclic voltammetry curve figure being scanned respectively with the sweep speed of 5,10,20 and 40mV/s in mouthful, as the result is shown not
Copper oxide@nickel molybdate/foam copper combination electrode shows apparent redox peaks under same scanning speed, shows the electrode
Redox reaction has occurred in material during the test.
Fig. 9 is specific capacity and current density of the obtained electrode of embodiment 1 as the working electrode of supercapacitor
Relational graph, it can be seen from the figure that in 3,5,8,10,20 and 40mA/cm2Current density under obtain specific capacitance value difference energy
Enough reach the specific capacity of 2600,2480,2317,2177,1867,1829F/g, which has specific capacity value high in this way
Illustrate that it has very high application potential in electrode of super capacitor field.
Figure 10 is copper oxide@nickel molybdate/foam copper combination electrode circulation cyclical stability test result in embodiment 1
Figure, it can be seen from the figure that by electrode material in 10mA/cm2Current density under after cycle charge-discharge 3000 times, specific volume
Amount is still able to maintain the 97.2% of initial capacity, shows that obtained electrode material has good cyclical stability.
The foregoing is only a preferred embodiment of the present invention, not does limitation in any form to the present invention.It is right
For those skilled in the art, without departing from the scope of the present invention, the present invention can have various changes and change
Change.But anything that does not depart from the technical scheme of the invention, the above case study on implementation is made according to the technical essence of the invention
Any simple modification, equivalent change and modification, still belong within the scope of technical solution of the present invention.
Claims (6)
1. a kind of preparation method of copper oxide@nickel molybdate/foam copper combination electrode material, its step are as follows:
(1) 15~25mmol sodium hydroxide and 1~3mmol ammonium persulfate are substantially dissolved in 30~50 ml deionized waters,
It will clean and dried foam copper be immersed in above-mentioned mixed solution, obtain homoepitaxial at room temperature in the hydrogen on foam copper surface
Nanowire array of copper oxide is labeled as Kocide SD nano-wire array/foam copper；
(2) ratio by 1~2mmol nickel nitrate and 1~2mmol sodium molybdate with molar ratio for 1:1 is completely dissolved in 30~50 millis
It rises in deionized water, Kocide SD nano-wire array/foam copper obtained by step (1) is immersed in the solution, it is anti-to carry out hydro-thermal
It answers, after natural cooling, is washed after gained sample is taken out and dry；
(3) step (2) products therefrom is calcined under atmosphere of inert gases and obtains copper oxide@nickel molybdate/foam copper combination electrode
Material.
2. a kind of preparation method of copper oxide@nickel molybdate/foam copper combination electrode material as described in claim 1, feature
Be: the molar ratio of sodium hydroxide and ammonium persulfate is 8~20:1 in step (1).
3. a kind of preparation method of copper oxide@nickel molybdate/foam copper combination electrode material as described in claim 1, feature
Be: the temperature of hydro-thermal reaction is 90~120 DEG C in step (2), and the reaction time is 1~6 hour.
4. a kind of preparation method of copper oxide@nickel molybdate/foam copper combination electrode material as described in claim 1, feature
Be: inert gas is one of nitrogen or argon gas in step (3).
5. a kind of preparation method of copper oxide@nickel molybdate/foam copper combination electrode material as described in claim 1, feature
Be: the calcination temperature in step (3) is 350 DEG C~450 DEG C, and calcination time is 2~5 hours.
6. a kind of copper oxide@nickel molybdate/foam copper combination electrode material, it is characterised in that: be by Claims 1 to 5 any one
Method described in is prepared.
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| CN110510655A (en) * | 2019-08-23 | 2019-11-29 | 华南理工大学 | A kind of copper oxide/copper-molybdenum oxidate nano heterogeneous structure material and preparation method thereof |
| CN111540616A (en) * | 2020-05-09 | 2020-08-14 | 中南大学 | Light enhancement effect transparent super capacitor and preparation method thereof |
| CN111575764A (en) * | 2020-05-19 | 2020-08-25 | 中国科学技术大学 | Composite nickel-tungsten-copper alloy, preparation method and application thereof |
| CN113637999A (en) * | 2021-08-19 | 2021-11-12 | 武汉工程大学 | Cu-based nano array composite nickel-molybdenum oxide electrode material and preparation method and application thereof |
| CN113818041A (en) * | 2021-09-17 | 2021-12-21 | 安徽师范大学 | Heterostructure material of ultrathin bimetal molybdate nanosheet coated nanotube, and preparation method and application thereof |
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| CN113818041A (en) * | 2021-09-17 | 2021-12-21 | 安徽师范大学 | Heterostructure material of ultrathin bimetal molybdate nanosheet coated nanotube, and preparation method and application thereof |
| CN113818041B (en) * | 2021-09-17 | 2023-03-07 | 安徽师范大学 | Heterostructure material of ultrathin bimetal molybdate nanosheet coated nanotube, and preparation method and application thereof |
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Application publication date: 20190521 |