CN109273275B - Vanadium trioxide loaded nano nickel, preparation method thereof, electrode material prepared from vanadium trioxide loaded nano nickel and supercapacitor - Google Patents
Vanadium trioxide loaded nano nickel, preparation method thereof, electrode material prepared from vanadium trioxide loaded nano nickel and supercapacitor Download PDFInfo
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- CN109273275B CN109273275B CN201811182755.2A CN201811182755A CN109273275B CN 109273275 B CN109273275 B CN 109273275B CN 201811182755 A CN201811182755 A CN 201811182755A CN 109273275 B CN109273275 B CN 109273275B
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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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- 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
- H01G11/30—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
- H01G11/46—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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- 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 vanadium trioxide loaded nano nickel, a preparation method thereof, an electrode material prepared by the vanadium trioxide loaded nano nickel and a super capacitor, wherein the preparation method of the vanadium trioxide loaded nano nickel comprises the following steps: 1) mixing a vanadium source, a nickel salt and an organic ligand, and dissolving in a solvent to prepare mixed slurry; 2) transferring the mixed slurry into a kettle for reaction to obtain an organic framework compound containing vanadium and nickel, cooling, and then filtering, washing and drying; 3) and calcining the sample in inert gas to prepare the vanadium trioxide loaded nano nickel. The production process is simple, the reaction conditions are easy to control, the raw material cost is low, a template agent and a surfactant are not needed in the preparation process, the obtained product has good consistency and no environmental pollution, and batch production is facilitated; the specific capacitance of the vanadium trioxide loaded nano nickel used as an electrode material of a super capacitor can reach 478F/g at most, and the specific capacitance of the vanadium trioxide loaded nano nickel can still be maintained to be more than 94% after 3000 charging and discharging cycles.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of nano materials, and particularly relates to vanadium trioxide loaded nano nickel, a preparation method of the vanadium trioxide loaded nano nickel, an electrode material prepared by the vanadium trioxide loaded nano nickel and a super capacitor.
[ background of the invention ]
The rapid consumption of fossil fuels causes severe energy and environmental problems in the world, and further promotes the development and utilization of new energy. Although various new energy technologies such as wind energy, solar energy, tidal energy and the like are widely concerned, the distribution of the new energy on time, seasons and regions is discontinuous and non-uniform, so that the further development and application of the new energy are limited. In recent years, new electric energy storage devices such as lithium ion batteries, super capacitors, and the like, which can stably utilize them and convert them into a portable stored electric energy form, have been greatly promoted. The super capacitor is distinguished from the rechargeable battery by the characteristics of high power density, rapid charge and discharge capacity, ultra-long cycle stability and the like, and is paid extensive scientific research attention.
In the present day that environmental pollution is becoming more serious and fossil fuel is gradually exhausted, it becomes more important to seek energy storage devices with high energy density. Supercapacitors are one of the most reliable electrochemical energy storage systems, gaining wide attention due to their excellent energy density, and rapid charge and discharge performance. The electrode material is used as a core component of a super capacitor, and the composition, the structure and the properties of the electrode material play a decisive influence on the performance of the capacitor.
Although research and development of electrode materials of super capacitors are remarkably advanced, the electrode materials commonly used at present, such as carbon with single component, metal oxide, metal sulfide and the like, generally have a plurality of defects: for example, (1) the low specific surface area and porosity inhibit the direct contact of active components with the electrolyte, which weakens the capability of electron transfer and ion mass transfer, and leads to the difficulty in increasing the energy density and power density of the electrode material; (2) the utilization rate of the components of the electrode material is low, and the active elements in the block body cannot fully generate oxidation-reduction reaction in the rapid charging and discharging process, so that the multiplying power characteristic is poor. Therefore, how to construct an electrode material with high specific surface area and rich active sites and effectively improve the utilization rate of active components has important scientific value and practical significance for developing a novel super capacitor energy storage device.
Vanadium trioxide (V)2O3) Due to excellent optical, electrical and magnetic properties, the material has wide application in various fields such as electrical, magnetic and optical switches, gas sensors, storage materials, resistance materials and the like. The nano nickel has small size, large specific surface area, high surface activity and good electrical conductivity and thermal conductivity, so that the nano nickel is widely used in catalysts, hard alloy binders, conductive slurry raw materials, additives of solid fuel propellants, magnetic liquid raw materials and the like in hydrogenation reaction and battery material (nickel-hydrogen battery) industries, and has excellent performances which are not possessed by some conventional crude nickel powders.
A single nano vanadium trioxide is reported in many documents at present, for example, CN105621485B (a preparation method of vanadium trioxide powder) is synthesized by a hydrothermal method by using a vanadium source, thioglycolic acid and distilled water as raw materials; CN106006733B (a method for preparing vanadium trioxide by a hydrothermal method) is prepared by hydrothermal reaction of hydrogen and a high-valence vanadium solution at high temperature and high pressure. The vanadium trioxide materials synthesized by the common methods often have the defect that the preparation cost is increased by adding a reducing agent, and the application of actual functional materials cannot be met due to single phase of the synthesized materials. The vanadium trioxide-based composite nano material has wide application prospect as an excellent functional material, but the current literature reports are less. For example, the vanadium trioxide/carbon electrode material reported in patent CN104078247B (composite electrode material vanadium trioxide/carbon, supercapacitor and method for preparing the same) has complicated preparation steps, and adopts two-step calcination, wherein one step is calcination for preparing a carbon source, and the other step is calcination for preparing a finished product. How to synthesize the vanadium trioxide nano composite material by adopting cheap raw materials through a simple preparation process is an important research topic. The supported vanadium trioxide nano composite material is an excellent photoelectric material, and particularly, the electrochemical activity of the composite material can be effectively improved by the support of metal nano ions. For the nano nickel particles loaded on the surface of vanadium trioxide, vanadium trioxide and nano simple substance nickel are in a reduction state, and are difficult to prepare by a common reducing agent, so that the preparation and research of the composite material are significant.
[ summary of the invention ]
The invention aims to solve the problems of complex preparation steps and the like, and provides a vanadium trioxide loaded nano nickel, a preparation method, an electrode material prepared by the vanadium trioxide loaded nano nickel and a supercapacitor. The vanadium trioxide loaded nano nickel material has high specific capacitance, good conductivity and good electrochemical performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of vanadium trioxide loaded nano nickel comprises the following steps:
1) dissolving vanadium salt, nickel salt and organic ligand in a solvent, and stirring at room temperature to obtain mixed slurry;
2) transferring the mixed slurry prepared in the step 1) into an autoclave, carrying out constant temperature reaction at the temperature of 120-160 ℃, wherein the reaction time is 8-20h, obtaining a crude organic framework compound containing vanadium and nickel, naturally cooling to room temperature, and then sequentially carrying out filtration, organic solvent washing and vacuum drying treatment on the obtained crude organic framework compound containing vanadium and nickel to obtain the organic framework compound containing vanadium and nickel, wherein the vacuum degree of vacuum drying is-0.1 MPa, and the drying time is 3-8 h;
3) and (3) placing the organic frame compound sample containing vanadium and nickel prepared in the step 2) into a tubular furnace, and calcining in argon or nitrogen at the temperature of 600 ℃ for 180min at the temperature of 400-.
The technical principle is as follows: according to the preparation method of the vanadium trioxide loaded nano nickel, a vanadium source, a nickel source and an organic ligand which are cheap and easy to obtain are adopted to prepare an organic-inorganic framework compound precursor through hydrothermal reaction, and then calcination is carried out to prepare the vanadium trioxide loaded nano nickel composite material, wherein in the process of calcining the organic-inorganic framework compound precursor, carbon generated by calcination is used as reducing atmosphere to reduce high-valence vanadium into vanadium trioxide, nickel salt is reduced into simple substance nano nickel, and then nano nickel is loaded on the surface of vanadium trioxide to form the composite material. Two reduced nanometer material components are obtained simultaneously through the calcination of an organic-inorganic framework compound precursor, the component units are compounded to form a composite nanometer material, and the reaction mechanism literature is rarely reported. The composite material has good electrochemical activity, high specific capacitance and good cycling stability as a super capacitor electrode material, and is expected to be used as an electrode material with great potential in the fields of energy storage, electrocatalysis and the like.
Preferably, the vanadium salt in the preparation step 1) is one of ammonium metavanadate, vanadyl sulfate or sodium metavanadate; the nickel salt is one of sulfate, chloride or nitrate containing nickel.
Preferably, the organic ligand in the preparation step 1) is one or a mixture of more than two of trimesic acid, terephthalic acid, oxalic acid and citric acid in any proportion.
Preferably, the solvent in the preparation step 1) is a mixed solution of distilled water and an organic solvent, the organic solvent is one of N, N' -dimethylformamide, ethanol or methanol, and the volume ratio of the organic solvent to the distilled water is 1: 10-20.
Preferably, the molar ratio of the vanadium salt, the nickel salt and the organic ligand in the preparation step 1) is 1:2-3.6: 1-1.5.
Preferably, the organic solvent washed in the preparation step 2) is one of ethanol or N, N' -dimethylformamide.
The invention also provides the vanadium trioxide loaded nano nickel prepared according to the method.
The invention also provides a supercapacitor electrode material prepared by loading nano nickel on vanadium trioxide according to the claim, and the preparation method comprises the following steps:
mixing vanadium trioxide loaded nano nickel, a conductive agent and a binder according to the weight ratio of 70-80:10:10-20, wherein the conductive agent is acetylene black, the binder is polyvinylidene fluoride to prepare a mixed slurry, coating the mixed slurry on a current collector, and then drying in vacuum to obtain the electrode material of the supercapacitor.
Preferably, the current collector is made of nickel foam.
The invention also provides a super capacitor prepared from the super capacitor electrode material.
The invention has the following beneficial effects:
(1) the preparation method of the vanadium trioxide loaded nano nickel has the characteristics of simple process, easily controlled reaction conditions, low raw material cost, convenient operation, easy industrial production and the like, does not need a template agent and a surfactant in the preparation process, has good consistency of the obtained product and no environmental pollution, and is favorable for batch production of the vanadium trioxide loaded nano nickel.
(2) In the vanadium trioxide loaded nano nickel, vanadium trioxide is of a sheet structure, spherical nano nickel is loaded on the surface of the sheet structure, and the vanadium trioxide loaded nano nickel has a sheet structure, so that the vanadium trioxide loaded nano nickel has huge specific capacitance, high rate performance and cycle performance, is good in conductivity and has good electrochemical performance.
(3) Compared with the prior art, the invention has the advantages of obvious technical progress, simple preparation process, cheap raw materials and the like in preparation strategy, and is beneficial to industrial scale-up production. The invention adopts a hydrothermal-calcining method to solve the problem that the vanadium trioxide in a double reduction state loaded with the nano nickel composite nano material which cannot be prepared by the conventional reducing agent. The idea of directly obtaining the nano nickel-loaded vanadium trioxide composite nano material by calcining the organic-inorganic framework compound precursor in an inert atmosphere is novel and has not been reported in documents. The specific capacitance of the vanadium trioxide loaded nano nickel composite electrode material can reach 478F/g to the maximum, more than 94% of the specific capacitance can be still maintained after 3000 times of charge-discharge cycle, and the vanadium trioxide loaded nano nickel composite electrode material can be used as a super capacitor electrode material; the composite electrode material has the advantages of simple and controllable preparation process, mild conditions and low production cost, and is suitable for industrial production.
[ description of the drawings ]
Fig. 1 is an X-ray diffraction (XRD) pattern of the vanadium trioxide supported nano nickel prepared in example 1, in which: the top line is the standard nickel diffraction peak and the bottom line is the standard V2O3A diffraction peak; the middle line is the diffraction peak of the vanadium trioxide loaded nano nickel prepared by the invention. As can be seen from figure 1, the vanadium trioxide loaded nano nickel prepared by the method has good crystallinity and high purity.
FIG. 2 is a Scanning Electron Microscope (SEM) image of the vanadium trioxide loaded nano-nickel prepared in example 2. As can be seen from the figure, most of vanadium trioxide in the composite material is in a sheet structure, nano nickel is loaded on the sheet structure, the nano nickel is in a spherical structure, and the particle size is 30-50 nm.
FIG. 3 is a cyclic voltammogram of the vanadium trioxide-loaded nano-nickel electrode material prepared in example 3.
[ detailed description ] embodiments
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
The preparation method of the vanadium trioxide loaded nano nickel comprises the following steps:
1) dissolving vanadium salt, nickel salt and organic ligand in a solvent, and stirring at room temperature to obtain mixed slurry;
2) transferring the mixed slurry prepared in the step 1) into an autoclave, carrying out constant temperature reaction at the temperature of 120-160 ℃, wherein the reaction time is 8-20h, obtaining a crude organic framework compound containing vanadium and nickel, naturally cooling to room temperature, and then sequentially carrying out filtration, organic solvent washing and vacuum drying treatment on the obtained crude organic framework compound containing vanadium and nickel to obtain the organic framework compound containing vanadium and nickel, wherein the vacuum degree of vacuum drying is-0.1 MPa, and the drying time is 3-8 h;
3) and (3) placing the organic frame compound sample containing vanadium and nickel prepared in the step 2) into a tubular furnace, and calcining in argon or nitrogen at the temperature of 600 ℃ for 180min at the temperature of 400-.
The vanadium salt in the preparation step 1) is one of ammonium metavanadate, vanadyl sulfate or sodium metavanadate; the nickel salt is one of sulfate, chloride or nitrate containing nickel.
The organic ligand in the preparation step 1) is one or a mixture of more than two of trimesic acid, terephthalic acid, oxalic acid and citric acid in any proportion.
The solvent in the preparation step 1) is a mixed solution of distilled water and an organic solvent, the organic solvent is one of N, N' -dimethylformamide, ethanol or methanol, and the volume ratio of the organic solvent to the distilled water is 1: 10-20.
The molar ratio of the vanadium salt, the nickel salt and the organic ligand in the preparation step 1) is 1:2-3.6: 1-1.5.
The organic solvent washed in the preparation step 2) is one of ethanol or N, N' -dimethylformamide.
The preparation method of the supercapacitor electrode material prepared by loading nano nickel on vanadium trioxide comprises the following steps:
mixing vanadium trioxide loaded nano nickel, an acetylene black conductive agent and a polyvinylidene fluoride binder according to a weight ratio of 70-80:10:10-20 to prepare mixed slurry, coating the mixed slurry on a current collector made of foamed nickel, then carrying out vacuum drying to obtain a super capacitor electrode material, and preparing the super capacitor by using the electrode material.
The following is a more specific example.
The specific embodiments were carried out according to the following procedure, with the parameters given in the following table.
A preparation method of vanadium trioxide loaded nano nickel comprises the following steps:
1) dissolving vanadium salt, nickel salt and organic ligand in a solvent, and stirring at room temperature to obtain mixed slurry;
2) transferring the mixed slurry into an autoclave, carrying out constant temperature reaction at the temperature of 120-160 ℃, wherein the reaction time is 8-20h, obtaining a crude organic framework compound containing vanadium and nickel, naturally cooling to room temperature, and then sequentially carrying out filtration, organic solvent washing and vacuum drying treatment on the obtained crude organic framework compound containing vanadium and nickel to obtain the organic framework compound containing vanadium and nickel, wherein the washed organic solvent is one of ethanol or DMF (N, N' -dimethylformamide), the vacuum degree of vacuum drying is-0.1 MPa, and the drying time is 3-8 h;
3) and (3) placing the organic framework compound sample containing vanadium and nickel in a tubular furnace, and calcining in argon or nitrogen at the temperature of 600 ℃ for 180min at the temperature of 400-.
The obtained vanadium trioxide loaded nano nickel electrode material is used as a working electrode, saturated calomel is used as a reference electrode, and a platinum sheet is used as a counter electrode to form a three-electrode system. Electrochemical tests were performed in 3M KOH electrolyte solution using CHI660E electrochemical workstation from Chenghua, Shanghai, with a sweep voltage range of 0-0.65V during the test, and the results are shown in the following table.
From the above table, it can be seen that: the specific capacitance of the vanadium trioxide loaded nano nickel used as an electrode material of a super capacitor can reach 478F/g at most, and the specific capacitance of the vanadium trioxide loaded nano nickel can still be maintained to be more than 94% after 3000 charging and discharging cycles.
The above description should not be taken as limiting the invention to the embodiments, but rather, as will be apparent to those skilled in the art to which the invention pertains, numerous simplifications or substitutions may be made without departing from the spirit of the invention, which shall be deemed to fall within the scope of the invention as defined by the claims appended hereto.
Claims (9)
1. A preparation method of vanadium trioxide loaded nano nickel is characterized by comprising the following steps:
1) dissolving a vanadium salt, a nickel salt and an organic ligand in a solvent, and stirring at room temperature to obtain mixed slurry, wherein the molar ratio of the vanadium salt to the nickel salt to the organic ligand is 1:2-3.6: 1-1.5;
2) transferring the mixed slurry prepared in the step 1) into an autoclave, carrying out constant temperature reaction at the temperature of 120-160 ℃, wherein the reaction time is 8-20h, obtaining a crude organic framework compound containing vanadium and nickel, naturally cooling to room temperature, and then sequentially carrying out filtration, organic solvent washing and vacuum drying treatment on the obtained crude organic framework compound containing vanadium and nickel to obtain the organic framework compound containing vanadium and nickel, wherein the vacuum degree of vacuum drying is-0.1 MPa, and the drying time is 3-8 h;
3) and (3) placing the organic frame compound sample containing vanadium and nickel prepared in the step 2) into a tubular furnace, and calcining in argon or nitrogen at the temperature of 600 ℃ for 180min at the temperature of 400-.
2. The method for preparing vanadium trioxide supported nano nickel according to claim 1, characterized in that: the vanadium salt in the preparation step 1) is one of ammonium metavanadate, vanadyl sulfate or sodium metavanadate; the nickel salt is one of sulfate, chloride or nitrate containing nickel.
3. The method for preparing vanadium trioxide supported nano nickel according to claim 1, characterized in that: the organic ligand in the preparation step 1) is one or a mixture of more than two of trimesic acid, terephthalic acid, oxalic acid and citric acid in any proportion.
4. The method for preparing vanadium trioxide supported nano nickel according to claim 1, characterized in that: the solvent in the preparation step 1) is a mixed solution of distilled water and an organic solvent, the organic solvent is one of N, N' -dimethylformamide, ethanol or methanol, and the volume ratio of the organic solvent to the distilled water is 1: 10-20.
5. The method for preparing vanadium trioxide supported nano nickel according to claim 1, characterized in that: the organic solvent washed in the preparation step 2) is one of ethanol or N, N' -dimethylformamide.
6. Nano-nickel supported on vanadium trioxide prepared according to the process of any one of claims 1 to 5.
7. The supercapacitor electrode material prepared by loading nanometer nickel on vanadium trioxide according to claim 6, wherein the preparation method comprises the following steps:
mixing vanadium trioxide loaded nano nickel, a conductive agent and a binder according to the weight ratio of 70-80:10:10-20, wherein the conductive agent is acetylene black, the binder is polyvinylidene fluoride to prepare a mixed slurry, coating the mixed slurry on a current collector, and then drying in vacuum to obtain the electrode material of the supercapacitor.
8. The supercapacitor electrode material prepared from vanadium trioxide loaded with nano nickel according to claim 7, characterized in that: the current collector is made of nickel foam.
9. A supercapacitor made from the supercapacitor electrode material according to claim 7 or 8.
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