Method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by solvothermal method

A technology of tricobalt tetroxide flower and solvothermal method, which is applied in the direction of cobalt oxide/cobalt hydroxide, nanotechnology, etc., to achieve good reproducibility, convenient mass production, and good chemical stability

Inactive Publication Date: 2013-02-13
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is still a big challenge to develop a simple and reliable synthetic method to prepare porous materials with specific composition and controllable morphology.

Method used

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  • Method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by solvothermal method
  • Method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by solvothermal method
  • Method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by solvothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Cobalt tetroxide (Co 3 o 4 ) The preparation steps of the micron flower-shaped ball are as follows:

[0027] a. Put 2mmol cobalt nitrate into 35ml EG, add copper nitrate according to the ratio of cobalt nitrate: copper nitrate 2:1, and keep stirring until the solution is uniform;

[0028] b. Then add 2ml of ammonia water (25-28wt%) and stir until uniform;

[0029] c. Transfer to a polytetrafluoroethylene-lined reaction kettle, keep the temperature at 180°C for 12 hours, then cool naturally to obtain a hydrothermal product;

[0030] d. Centrifuge the hydrothermal product obtained above, and wash with absolute ethanol and deionized water for 3 times respectively;

[0031] e. Dry the centrifuged product in a vacuum oven at 60°C for 12 hours to obtain the precursor;

[0032] f. Put the precursor in the tube furnace with N 2 Calcined at 500°C for 3h to obtain the final product.

[0033]

[0034] co 3 o 4 The XRD of the micron flower-shaped ball product is shown in ...

Embodiment 2

[0039] Cobalt tetroxide (Co 3 o 4 ) The preparation steps of the micron flower-shaped ball are as follows:

[0040] a. Put 2mmol cobalt nitrate into 35ml EG, add copper nitrate according to the ratio of cobalt nitrate: copper nitrate 2:1, and keep stirring until the solution is uniform;

[0041] b. Then add 1ml of ammonia water (25-28wt%) and stir until uniform;

[0042] c. Transfer to a polytetrafluoroethylene-lined reaction kettle, keep the temperature at 180°C for 12 hours, and then cool naturally to obtain a hydrothermal product;

[0043] d. Centrifuge the hydrothermal product obtained above, and wash with absolute ethanol and deionized water for 3 times respectively;

[0044] e. Dry the centrifuged product in a vacuum oven at 60°C for 12 hours to obtain the precursor;

[0045] f. Put the precursor in the tube furnace with N 2 Protected and calcined at 500°C for 3h to obtain the final product.

Embodiment 3

[0047] Cobalt tetroxide (Co 3 o 4 ) The preparation steps of the micron flower-shaped ball are as follows:

[0048]a. Put 2mmol cobalt nitrate into 35ml EG, add copper nitrate according to the ratio of cobalt nitrate: copper nitrate 2:1, and keep stirring until the solution is uniform;

[0049] b. Then add 2ml of ammonia water (25-28wt%) and stir until uniform;

[0050] c. Transfer to a polytetrafluoroethylene-lined reaction kettle, keep the temperature at 160°C for 12 hours, and then cool naturally to obtain a hydrothermal product;

[0051] d. Centrifuge the hydrothermal product obtained above, and wash with absolute ethanol and deionized water for 3 times respectively;

[0052] e. Dry the centrifuged product in a vacuum oven at 60°C for 12 hours to obtain the precursor;

[0053] f. Put the precursor in the tube furnace with N 2 Protected and calcined at 500°C for 3h to obtain the final product.

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Abstract

The invention belongs to the technical field of nano-material synthesis, relates to a method for preparing microspheres having uniform morphology by a solvothermal method, and especially relates to a method for preparing multi-tunnel cobaltosic oxide flower-like microspheres by a solvothermal method. The method comprises the following steps of uniformly mixing cobalt nitrate, copper nitrate, ethylene glycol and ammonia water, transferring the mixture to a reactor with a Teflon lining, carrying out a high-temperature solvothermal reaction process, carrying out centrifugal separation, washing and vacuum drying of solvothermal reaction products, and carrying out calcination in a tubular furnace. The method utilizes ethylene glycol as a solvent and utilizes a solvothermal method to prepare a cobaltosic oxide material having a high yield and uniform morphology. The multi-tunnel cobaltosic oxide flower-like microspheres prepared by the method have good chemical stability and can be used for preparing an electrode material and a hydrogen production material of a storage battery. The method has simple processes and good reappearance and utilizes a cobalt inorganic compound as a cobalt source, wherein the cobalt inorganic compound has a low cost, can be acquired easily and satisfies environmental requirements. The method avoids pre-treatment processes such as aging, allows a low synthesis temperature, reduces energy consumption and a reaction cost, and is convenient for volume production.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial synthesis, and relates to a method for preparing microspheres with uniform appearance by a solvothermal method, in particular to a method for preparing porous cobalt trioxide flower-shaped microspheres by a solvothermal method. Background technique [0002] The structure, morphology and size control of inorganic nanomaterials have always attracted extensive attention of researchers, with the purpose of improving the performance of materials. In recent years, porous inorganic materials have received special attention in materials research, mainly due to their potential applications in different fields. Recently, porous materials have become a research hotspot because of their potential applications in catalysis, sensors, fuel cells, superconductors and other fields. Such as lithium-ion batteries, ion exchange and catalytic processes, etc. Cobalt oxide (CoO), as an important transition metal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04B82Y40/00
Inventor 施伟东蒋金辉张坤孙绍芳吴亚帆
Owner JIANGSU UNIV
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