CN115246659B - Preparation method of defect type hollow nickel cobalt oxide nanocube - Google Patents
Preparation method of defect type hollow nickel cobalt oxide nanocube Download PDFInfo
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- 230000007547 defect Effects 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- YTBWYQYUOZHUKJ-UHFFFAOYSA-N oxocobalt;oxonickel Chemical compound [Co]=O.[Ni]=O YTBWYQYUOZHUKJ-UHFFFAOYSA-N 0.000 title claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 5
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 4
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 3
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 8
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 8
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 6
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 6
- 229940112669 cuprous oxide Drugs 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000033116 oxidation-reduction process Effects 0.000 claims description 2
- 230000002950 deficient Effects 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 abstract 1
- 239000007772 electrode material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a preparation method of a defect type hollow nickel cobalt oxide nanocube. The invention aims to solve the problems of poor conductivity and fewer active sites of the existing nickel cobaltate, and provides a preparation method for improving the performance of a nickel cobaltate-based supercapacitor. The method comprises the following steps: the preparation method is characterized in that copper chloride, polyvinylpyrrolidone, sodium hydroxide, L-ascorbic acid, nickel chloride, cobalt chloride and sodium thiosulfate are used as raw materials, and a template method and a partial reduction method are adopted to prepare the defective hollow nickel cobaltate nanocube, so that the preparation method is provided for improving the performance of the existing nickel cobaltate-based supercapacitor.
Description
Technical Field
The invention relates to preparation of a defect type hollow nickel cobalt oxide nanocube.
Background
The super capacitor is a novel energy storage device between the traditional capacitor and the battery, stores energy through rapid ion adsorption and desorption or highly reversible Faraday redox reaction at an electrode material and electrolyte interface, and has wide application prospect. The core of the super capacitor is an electrode material, and nickel cobaltate has become one of research hot spots of energy materials because of high theoretical specific capacity. However, the conductivity and electrochemically active sites of nickel cobaltate remain to be improved. The hollow nickel cobaltate nanocube prepared by the template method improves the specific surface area, and improves the conductivity of the nickel cobaltate and enriches electrochemical active sites by constructing oxygen defects, so that the conductivity and the electrochemical performance of the hollow nickel cobaltate nanocube are improved, and the hollow nickel cobaltate nanocube has important research significance for solving the energy shortage problem.
Disclosure of Invention
The invention aims to solve the problems of poor conductivity and few reactive sites of nickel cobaltate, and provides a simple, novel and high-yield preparation method.
The preparation method of the defect type hollow nickel cobaltate nanocubes is completed according to the following steps:
(1) Dissolving polyvinylpyrrolidone in a cupric chloride solution, then dropwise adding a sodium hydroxide solution into the solution, stirring, dropwise adding an ascorbic acid solution into the solution, stirring, centrifugally washing and drying to obtain a cuprous oxide nanocube template;
(2) Putting the cuprous oxide template, nickel chloride and cobalt chloride into a water/ethanol mixed solution containing polyvinylpyrrolidone, stirring, dripping sodium thiosulfate, centrifuging, washing and drying to obtain a hollow nickel cobalt hydroxide nanocube;
(3) Calcining 0.2 g of the precipitate prepared in the step (2) in a muffle furnace to obtain a hollow nickel cobaltate nanocube; (4) And (3) respectively placing the hollow nickel cobaltate nanocubes and sodium hypophosphite obtained in the step (3) in two porcelain boats of a tube furnace, wherein the sodium hypophosphite is positioned at the upstream, and calcining under the protection of N 2 to obtain the defect type hollow nickel cobaltate nanocubes, namely the supercapacitor material.
In the step (1), the mass of cobalt nitrate and nickel nitrate is respectively 0.2-2 g, the volume of isopropanol is 30-100 ml, the volume of glycerin is 5-20 ml, the hydrothermal reaction temperature is 50-200 ℃, the reaction time is 5-20 hours, and the drying condition is that the drying is carried out for 10-20 hours at 50-80 ℃;
In the step (2), the mass of the cuprous oxide nanocubes is 50-150 mg, the mass of the nickel chloride is 10-30 mg, the mass of the cobalt chloride is 10-30 mg, the mass of the polyvinylpyrrolidone is 2-6 g, the volume of the ethanol/water mixed solution is 50-200 ml, the proportion of the ethanol is 30-70%, and the drying condition is that the drying is carried out for 2-10 hours at 50-80 ℃;
The calcination temperature in the step (3) is 300-500 ℃ and the calcination time is 1-4 hours;
In the step (4), the mass ratio of the hollow nickel cobaltate nanocubes to the sodium hypophosphite is 1:5, the calcination temperature of the tube furnace is 200-500 ℃ and the calcination time is 1-5 hours.
Compared with the prior art, the invention has the beneficial effects that: the invention prepares the electrode material of the defective hollow nickel cobaltate nanocube supercapacitor, and the material with complete structure and large specific surface area can be prepared in a short time in the preparation process.
Drawings
FIG. 1 is a transmission electron microscope image of a defective hollow nickel cobaltate nanocube of example 1;
FIG. 2 is a drawing showing nitrogen desorption of the defective hollow nickel cobaltate nanocubes of example 1;
FIG. 3 is a cyclic voltammogram of a defective hollow nickel cobaltate nanocube of example 1;
FIG. 4 is a constant current charge-discharge diagram of the defective hollow nickel cobaltate nanocube of example 1;
FIG. 5 is an electrochemical impedance plot of a defective hollow nickel cobaltate nanocube of example 1.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, which are only for illustrating the present invention and are not limited to the technical solution described in the examples of the present invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or equivalents substituted for elements thereof to achieve the same technical effect. As long as the use requirement is met, the invention is within the protection scope of the invention.
The preparation method of the defect type hollow nickel cobaltate nanocubes in the embodiment is completed by the following steps:
(1) 5.1 g of polyvinylpyrrolidone is dissolved in 300 ml of 0.01 mol/L copper chloride solution, then 30 ml of 2 mol/L sodium hydroxide solution is dropwise added into the solution, after stirring for 0.5 hour, 30 ml of 0.6 mol/L ascorbic acid solution is dropwise added into the solution, after stirring for three hours, centrifugal washing and drying are carried out, and all the operations are carried out under the condition of heating and stirring in a water bath at 55 ℃;
(2) 100 mg of cuprous oxide, 17 mg of nickel chloride and 17 mg of cobalt chloride are added to a mixed solution of 100 ml of ethanol/water (1:1) containing 3.3 g of polyvinylpyrrolidone, and after stirring for 0.5 hours, 40 ml of 1 mol/L sodium thiosulfate solution is added dropwise to the above solution, and the solution is centrifugally washed and dried;
(3) Placing 0.2 g of the precipitate prepared in the step (2) into a muffle furnace, and calcining at 350 ℃ for 2 hours to obtain a hollow nickel cobaltate nanocube;
(4) 0.2g of the hollow nickel cobaltate nanocubes and sodium hypophosphite obtained in the step (3) are respectively placed in two porcelain boats of a tube furnace, and the mass ratio is 1: and 5, calcining the sodium hypophosphite at 250 ℃ for 1 hour under the protection of N 2, wherein the sodium hypophosphite is positioned at the upstream, and obtaining the defect type hollow nickel cobaltate nanocube which is the supercapacitor material.
The invention is further described with reference to the accompanying drawings and examples:
FIG. 1 is a transmission electron microscope image of a defective hollow nickel cobaltate nanocube of example 1. The hollow nickel cobaltate nanocubes are regular hollow nanocubes.
FIG. 2 is a drawing showing nitrogen desorption of the defective hollow nickel cobaltate nanocubes of example 1. Hysteresis appears after P/P 0 =0.4, indicating that the material has mesopores and has a high specific surface area of 50.99m 2/g.
FIG. 3 is a cyclic voltammogram of a defective hollow nickel cobaltate nanocube of example 1. Along with the improvement of the scanning rate, the shape enclosed by the cyclic voltammetry curve is not obviously distorted, which indicates that the multiplying power performance of the material is good; the oxidation-reduction peaks are symmetrical, which shows that the reversibility and the stability of the material are good.
Fig. 4 is a constant current charge-discharge diagram of the defective hollow nickel cobaltate nanocube in example 1. The charge-discharge capacity time of the electrode material is approximately equal under different current densities, which indicates that the material has excellent reversibility and coulombic efficiency; at a current density of 0.5A/g, the hollow nickel cobaltate nanocubes have a specific capacitance of up to 1714.4F/g, indicating that the material has excellent supercapacitor properties.
FIG. 5 is an electrochemical impedance plot of a defective hollow nickel cobaltate nanocube in example 1. The intersection point of the curve and the abscissa is the internal resistance of the material, the radius of the circular arc is the transfer internal resistance of electrons, the slope represents the transfer rate of electrolyte ions, and the electrode material has small internal resistance and high conductivity.
Claims (1)
1. The application of the defect type hollow nickel cobalt oxide nanocube is characterized in that the defect type hollow nickel cobalt oxide nanocube is used as a supercapacitor material, has a high specific surface area of 50.99m 2/g, has excellent reversibility and coulombic efficiency, and has good rate capability; the oxidation-reduction peaks are symmetrical, the reversibility is good and the stability is high; under the current density of 0.5A/g, the hollow nickel cobaltate nanocubes have specific capacitance of up to 1714.4F/g, small internal resistance and high conductivity; the preparation method is completed according to the following steps:
(1) Dissolving 5.1 g of polyvinylpyrrolidone in 300ml of 0.01 mol/L copper chloride solution, dropwise adding 30ml of 2 mol/L sodium hydroxide solution into the solution, stirring for 0.5 hour, dropwise adding 30ml of 0.6 mol/L ascorbic acid solution into the solution, stirring for three hours, centrifuging, washing and drying, and heating and stirring in a water bath at 55 ℃ to obtain the cuprous oxide nanocube template;
(2) Adding 100 mg of cuprous oxide nanocube template, 17 mg of nickel chloride and 17 mg of cobalt chloride into 100 ml of ethanol/water mixed solution containing 3.3 g of polyvinylpyrrolidone, stirring for 0.5 hour, dropwise adding 40 ml of 1 mol per liter of sodium thiosulfate solution into the solution, centrifuging, washing and drying to obtain a hollow nickel cobalt hydroxide nanocube;
(3) Placing 0.2 g of the hollow nickel cobalt hydroxide nanocube prepared in the step (2) into a muffle furnace, and calcining at 350 ℃ for 2 hours to obtain the hollow nickel cobalt oxide nanocube;
(4) And (3) respectively placing 0.2 g of the hollow nickel cobaltate nanocubes and sodium hypophosphite obtained in the step (3) into two porcelain boats of a tube furnace, wherein the mass ratio is 1:5, wherein sodium hypophosphite is positioned at the upstream, and calcining for 1 hour at 250 ℃ under the protection of N 2 to obtain the defect type hollow nickel cobaltate nanocube.
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