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Preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres

A three-dimensional flower-shaped, nano-sheet technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., to achieve the effect of simple operation, good experimental reproducibility, and easy operation

Inactive Publication Date: 2015-07-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far there is no report on the three-dimensional flower-like mesoporous microspheres self-assembled from ultra-thin nickel cobalt oxide nanosheets and their preparation methods and electrocatalytic applications

Method used

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  • Preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres
  • Preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres
  • Preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Weigh 1.4540g nickel nitrate hexahydrate Ni(NO 3 ) 2 ·6H 2 O (0.005mol) and 2.9100g cobalt nitrate hexahydrate Co(NO 3 ) 2 ·6H 2 O (0.010mol) was dissolved in 5mL of deionized water, ultrasonicated for 5min to prepare a mixed metal salt solution, then 75mL of isopropanol was added thereto, and magnetically stirred for 1h to obtain a mixed metal salt solution A, and 10mL of methanol was added to A to continue Stir for 0.5h to obtain mixed reaction solution B, wherein Ni 2+ and Co 2+ The total concentration is 0.167mol / L.

[0036] 2. Then transfer to a 100mL reactor, and conduct hydrothermal treatment at 120°C for 24h. After naturally cooling to room temperature, it was centrifuged, washed alternately with ethanol and deionized water for 3 times until the supernatant had a pH of 7, and dried in vacuum at 80°C for 24 hours to obtain a three-dimensional flower-like nanosheet microsphere precursor. Its SEM image is shown in figure 1 .

[0037] 3. The above precu...

Embodiment 2

[0040] Electrode materials prepared from three-dimensional flower-like nickel cobalt oxide nanosheet mesoporous microspheres and their electrochemical characterization

[0041] 1. Use the modified glassy carbon electrode as the working electrode. First, use 1.0 μm alumina polishing powder to rough polish the glassy carbon electrode on the polishing cloth for 3 minutes, and then use 0.05 μm alumina polishing powder to fine polish the glassy carbon electrode on buckskin for 3 minutes;

[0042] 2. After polishing, place the electrode in a nitric acid solution with a volume ratio of 1:1, anhydrous ethanol and deionized water for 3 minutes, and dry it at room temperature for use;

[0043] 3. Add 10 mg of the three-dimensional flower-shaped nickel cobaltate nanosheet mesoporous microsphere powder prepared in Example 1 into 0.9 mL of absolute ethanol and 0.1 mL of 0.5 wt % Nafion solution, and ultrasonically disperse evenly; Drop 1 μL of the suspension on the surface of the electrod...

Embodiment 3

[0049] 1. Weigh 1.4540g nickel nitrate hexahydrate Ni(NO 3 ) 2 ·6H 2 O (0.0050mol) and 2.9100g cobalt nitrate hexahydrate Co(NO 3 ) 2 ·6H 2 O (0.010mol) was dissolved in 5mL of deionized water, ultrasonicated for 5min to prepare a mixed metal salt solution, then 75mL of isopropanol was added thereto, and magnetically stirred for 1h to obtain a mixed metal salt solution A, and 10mL of methanol was added to A to continue Stir for 0.5h to obtain mixed reaction solution B, wherein Ni 2+ and Co 2+ The total concentration is 0.167mol / L.

[0050] 2. Then transfer to a 100mL reactor, and conduct hydrothermal treatment at 120°C for 12h. After naturally cooling to room temperature, it was centrifuged, washed alternately with ethanol and deionized water for 3 times until the supernatant had a pH of 7, and dried in vacuum at 80°C for 24 hours to obtain a three-dimensional flower-like nanosheet microsphere precursor.

[0051] 3. Calcinate the above precursor in an air atmosphere at...

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Abstract

The invention relates to a preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres, and relates to the technical field of multi-level structured nano-grade catalyst materials. First, nickel nitrate hexahydrate and cobalt nitrate hexahydrate are adopted as a nickel source and a cobalt source, a deionized water-isopropanol mixed phase with a proper proportion is adopted as a solvent, methanol is adopted as a reactant, and no additional base precipitating agent is adopted; a three-dimensional flower-shaped nano-sheet microsphere precursor is prepared in a Ni<2+>-Co<2+>-NH3-NH4<+>-SG<n->-H2O-IPA-CH3OH system (SG<n-> is CO3<2-> or HCOO<->); the temperature is increased to 300-400 DEG C in an air atmosphere with a speed of 1 DEG C / min, and the precursor is calcined for 2-3h, such that the three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres are obtained. According to the invention, co-precipitation of the formulated cobalt and nickel in the raw materials is realized. The prepared three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres are spinel cubic phases with high purity, and are formed by ultrathin nano-sheet self-assembly. The microspheres comprise rich mesopores, and have a large specific surface area. The method has the advantages of simple operation, appropriate conditions and easy control.

Description

technical field [0001] The invention belongs to the technical field of multi-level structure nano-catalyst materials, and in particular provides a preparation method of three-dimensional flower-shaped nickel cobaltate nanosheet mesoporous microspheres. Background technique [0002] The study of Direct Methanol Fuel Cell (DMFC) began in the 1950s. Methanol has attracted widespread attention due to its cheap and easy to obtain, easy to carry, and energy density close to that of gasoline. At present, most of the anode catalysts used are platinum, ruthenium, gold and other noble metals and their binary or multi-component composite materials. However, noble metals have disadvantages such as high price, limited resources, and easy CO poisoning, which seriously affect the commercial application of DMFC. Therefore, finding non-precious metal electrocatalysts with good catalytic activity, high stability and low cost as an alternative anode catalyst has become an important research di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00B82Y30/00B82Y40/00
Inventor 张慧陈高文
Owner BEIJING UNIV OF CHEM TECH
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