CN115246659A - Preparation method of defective hollow nickel cobaltate nanocube - Google Patents
Preparation method of defective hollow nickel cobaltate nanocube Download PDFInfo
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- CN115246659A CN115246659A CN202111210862.3A CN202111210862A CN115246659A CN 115246659 A CN115246659 A CN 115246659A CN 202111210862 A CN202111210862 A CN 202111210862A CN 115246659 A CN115246659 A CN 115246659A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 230000002950 deficient Effects 0.000 title claims description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- 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
- 230000007547 defect Effects 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 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 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 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 10
- 238000003756 stirring 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 7
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 7
- 229940112669 cuprous oxide Drugs 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 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
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 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 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002211 L-ascorbic acid Substances 0.000 abstract description 2
- 235000000069 L-ascorbic acid Nutrition 0.000 abstract description 2
- 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
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005247 gettering Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
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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
-
- 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
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- 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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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C01P2006/40—Electric properties
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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
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Abstract
The invention relates to a preparation method of a defect type hollow nickel cobaltate nanocube. The invention aims to solve the problems of poor conductivity and few 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 defect type hollow nickel cobaltate nanocube is prepared by taking copper chloride, polyvinylpyrrolidone, sodium hydroxide, L-ascorbic acid, nickel chloride, cobalt chloride and sodium thiosulfate as raw materials and adopting a template method and a partial reduction method, and a preparation method is provided for improving the performance of the conventional nickel cobaltate-based supercapacitor.
Description
Technical Field
The invention relates to preparation of a defective hollow nickel cobaltate nanocube.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a battery, stores energy through rapid ion absorption and desorption or highly reversible Faraday redox reaction at an electrode material and electrolyte interface, and has a wide application prospect. The core of the super capacitor is an electrode material, and nickel cobaltate has high theoretical specific capacity and is one of the research hotspots of energy materials. However, the conductivity and electrochemical active sites of nickel cobaltate still need to be improved. The hollow nickel cobaltate nanocube prepared by the template method improves the specific surface area, improves the conductivity of the nickel cobaltate and enriches electrochemical active sites by constructing oxygen defects, thereby improving the conductivity and electrochemical properties of the nickel cobaltate nanocube, and having important research significance for solving the problem of energy shortage.
Disclosure of Invention
The invention aims to overcome the problems of poor conductivity and few reactive active sites of nickel cobaltate and provides a simple, novel and high-yield preparation method.
The preparation method of the defect type hollow nickel cobaltate nanocube is completed according to the following steps:
(1) Dissolving polyvinylpyrrolidone in a copper 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 a 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) Putting 0.2 g of the precipitate prepared in the step (2) into a muffle furnace for calcining to obtain a hollow nickel cobaltate nanocube; (4) Respectively placing the hollow nickel cobaltate nanocubes and sodium hypophosphite obtained in the step (3) into two porcelain boats of a tube furnace, wherein the sodium hypophosphite is positioned at the upstream and is positioned at N 2 Calcining under the protection condition to obtain the defect type hollow nickel cobaltate nanocubes, namely the supercapacitor material.
In the step (1), the mass of the cobalt nitrate and the mass of the nickel nitrate are respectively 0.2 to 2 g, the volume of the isopropanol is 30 to 100 ml, the volume of the glycerol is 5 to 20 ml, the hydrothermal reaction temperature is 50 to 200 ℃, the reaction time is 5 to 20 hours, and the drying condition is that the cobalt nitrate and the nickel nitrate are dried for 10 to 20 hours at the temperature of 50 to 80 ℃;
in the step (2), the weight of the cuprous oxide nanocube is 50-150 mg, the weight of the nickel chloride is 10-30 mg, the weight of the cobalt chloride is 10-30 mg, the weight of the polyvinylpyrrolidone is 2-6 g, the volume of the ethanol/water mixed solution is 50-200 ml, the proportion of ethanol is 30-70%, and the drying condition is that the drying is carried out for 2-10 hours at 50-80 ℃;
in the step (3), the calcining temperature is 300-500 ℃, and the calcining time is 1-4 hours;
the mass ratio of the hollow nickel cobaltate nanocubes to the sodium hypophosphite in the step (4) is 1:5, the calcining temperature of the tube furnace is 200-500 ℃, and the calcining time is 1-5 hours.
Compared with the prior art, the invention has the beneficial effects that: the defect type hollow nickel cobaltate nanocube supercapacitor electrode material prepared by the invention can be prepared into a material with a complete structure and a large specific surface area only in a short time in the preparation process, in addition, the synthesis of the material does not need complex equipment, and the prepared material has an excellent energy storage effect.
Drawings
FIG. 1 is a TEM image of example 1 defective hollow nickel cobaltate nanocubes;
FIG. 2 is a drawing showing nitrogen desorption of defective hollow nickel cobaltate nanocubes according to example 1;
FIG. 3 is a cyclic voltammogram of the defective hollow nickel cobaltate nanocubes of example 1;
FIG. 4 is a constant current charge and discharge diagram of the defective hollow nickel cobaltate nanocubes of example 1;
fig. 5 is an electrochemical impedance plot of the defective hollow nickel cobaltate nanocubes of example 1.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, which are only used for illustrating the present invention and are not limited to the technical solutions described in the embodiments of the present invention. It will be understood by those skilled in the art that the present invention may be modified and equivalents substituted for elements thereof to achieve the same technical effect. So long as the use requirements are met, the method is within the protection scope of the invention.
The preparation method of the defect type hollow nickel cobaltate nanocube of the embodiment is completed according to the following steps:
(1) Dissolving 5.1 g of polyvinylpyrrolidone in 300 ml of 0.01 mol/L copper chloride solution, then dropwise adding 30 ml of 2 mol/L sodium hydroxide solution into the solution, stirring for 0.5 hour, dropwise adding 30 ml of 0.6 mol/L ascorbic acid solution into the solution, stirring for three hours, centrifugally washing and drying, wherein all the operations are carried out under the heating and stirring of 55 ℃ water bath;
(2) Adding 100 mg of cuprous oxide, 17 mg of nickel chloride and 17 mg of cobalt chloride into a 100 ml ethanol/water (1;
(3) Putting 0.2 g of the precipitate prepared in the step (2) into a muffle furnace, and calcining for 2 hours at 350 ℃ to obtain a hollow nickel cobaltate nanocube;
(4) 0.2 g of the hollow nickel cobaltate nanocube obtained in the step (3) and sodium hypophosphite are respectively placed in two porcelain boats of a tube furnace, and the mass ratio is 1:5, wherein sodium hypophosphite is located upstream, at N 2 Calcining for 1 hour at 250 ℃ under the protection condition to obtain the defective hollow nickel cobaltate nanocubes, namely the supercapacitor material.
The invention is further described with reference to the following drawings and examples:
figure 1 is a transmission electron microscope image of example 1 defective hollow nickel cobaltate nanocubes. The hollow nickel cobaltate nanocubes are regular hollow nanocubes.
Figure 2 is a drawing of nitrogen gettering from example 1 defective hollow nickel cobaltate nanocubes. P/P 0 Hysteresis loop appeared after =0.4, indicating that the material has mesopores and the material has a thickness of 50.99m 2 High specific surface area per gram.
Figure 3 is a cyclic voltammogram of the defective hollow nickel cobaltate nanocubes of example 1. Along with the increase of the scanning rate, the shape surrounded by the cyclic voltammetry curve is not obviously distorted, which shows that the multiplying power performance of the material is good; the oxidation reduction peak is symmetrical, which shows that the material has good reversibility and high stability.
Fig. 4 is a constant current charge and discharge diagram of the defective hollow nickel cobaltate nanocubes in example 1. Under different current densities, the charge and discharge capacity time of the electrode material is approximately equal, which shows that the material has excellent reversibility and coulombic efficiency; under the current density of 0.5A/g, the hollow nickel cobaltate nanocubes have the specific capacitance as high as 1714.4F/g, which shows that the material has excellent supercapacitor performance.
Fig. 5 is an electrochemical impedance plot of the defective hollow nickel cobaltate nanocubes of example 1. The intersection point of the curve and the abscissa is the internal resistance of the material, the arc radius is the transfer internal resistance of electrons, and the slope represents the transmission transfer rate of electrolyte ions, so that the internal resistance of the electrode material is small, and the conductivity is high.
Claims (5)
1. The preparation method of the defective hollow nickel cobaltate nanocube is completed according to the following steps:
(1) Dissolving polyvinylpyrrolidone in a copper 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 a 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) Putting 0.2 g of the precipitate prepared in the step (2) into a muffle furnace for calcining to obtain a hollow nickel cobaltate nanocube;
(4) Respectively placing the hollow nickel cobaltate nanocubes and sodium hypophosphite obtained in the step (3) into two porcelain boats of a tube furnace, wherein the sodium hypophosphite is positioned at the upstream and is positioned at N 2 Calcining under the protection condition to obtain the defect type hollow nickel cobaltate nanocubes, namely the supercapacitor material.
2. The method for preparing the defective hollow nickel cobaltate nanocube according to claim 1, wherein the method comprises the following steps: in the step (1), the mass of the cobalt nitrate and the mass of the nickel nitrate are respectively 0.2-2 g, the volume of the isopropanol is 30-100 ml, the volume of the glycerol 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 cobalt nitrate and the nickel nitrate are dried for 10-20 hours at 50-80 ℃.
3. The method for preparing the defective hollow nickel cobaltate nanocube according to claim 1, wherein the method comprises the following steps: in the step (2), the cuprous oxide nanocubes are 50-150 mg in mass, the nickel chloride is 10-30 mg in mass, the cobalt chloride is 10-30 mg in mass, the polyvinylpyrrolidone is 2-6 g in mass, the volume of the ethanol/water mixed solution is 50-200 ml, the proportion of ethanol is 30-70%, and the drying is carried out for 2-10 hours at the temperature of 50-80 ℃.
4. The method for preparing the defective hollow nickel cobaltate nanocube according to claim 1, wherein the method comprises the following steps: in the step (3), the calcining temperature is 300-500 ℃, and the calcining time is 1-4 hours.
5. The method for preparing the defective hollow nickel cobaltate nanocube according to claim 1, wherein the method comprises the following steps: the mass ratio of the hollow nickel cobaltate nanocubes to the sodium hypophosphite in the step (4) is 1:5, the calcining temperature of the tube furnace is 200-500 ℃, and the calcining time is 1-5 hours.
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