Method for preparing nanometer-level cube-like cobaltosic oxide

A technology of cobalt tetroxide and cubes, which is applied in the field of preparing nano-cubic cobalt tetroxide, which can solve the problems of complex synthesis process, difficulty in controlling particle shape, and difficulty in reaching nanometer scale, and achieve simple preparation process, easy large-scale preparation, and low price Effect

Inactive Publication Date: 2014-12-10
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the traditional hydrothermal synthesis method can realize the industrial synthesis of cobalt tetroxide particles, it has disadvantages such as complex synthesis process, low metal recovery rate, and the need for further high-temperature calcination in air, and the obtained cobalt tetroxide has a large size, and the particle shape is difficult to control. Inhomogeneous size distribution, difficult to reach true nanoscale

Method used

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  • Method for preparing nanometer-level cube-like cobaltosic oxide
  • Method for preparing nanometer-level cube-like cobaltosic oxide
  • Method for preparing nanometer-level cube-like cobaltosic oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Disperse 0.3 g of dimethylglyoxime in 30 ml of absolute ethanol, and adjust the pH value of the dimethylglyoxime solution to 13.0 with 0.5 M sodium hydroxide ethanol solution. Dissolve 0.3 g of nickel chloride hexahydrate in 1 liter of water, and add the dimethylglyoxime solution dropwise into the nickel chloride solution under ultrasonic conditions to obtain a red flocculent substance. The above-mentioned red flocculent product was suction-filtered, washed and dried, and then calcined at 500°C for 1 h under Ar atmosphere to obtain a black powder. The nickel oxide and nickel in the black powder are etched away with 2.0mol / L hydrochloric acid to obtain nanostructured porous carbon, and its scanning electron microscope photo is as follows: figure 1 Shown:

Embodiment 2

[0032] Add 0.3 mg of porous carbon to 40 ml of distilled water for ultrasonic dispersion, then add 28.0 mg of cobalt nitrate and 36.0 mg of urea, stir evenly, transfer to a 60 ml hydrothermal reaction kettle, react at 120 ° C for 12 hours, and naturally cool to room temperature Afterwards, after centrifugation and washing, nano-scale cubic cobalt tetroxide powder is obtained, and its scanning electron microscope and transmission electron microscope photos are as follows: figure 2 Shown:

Embodiment 3

[0034] In the absence of porous carbon, add 28.0mg of cobalt nitrate and 36.0mg of urea to 40ml of distilled water, stir evenly, transfer to a 60ml hydrothermal reaction kettle, react at 120°C for 12 hours, cool to room temperature naturally, and centrifuge After separation and washing, cobalt trioxide powder of irregular shape is obtained, and its scanning electron microscope photo is as follows: image 3 Shown:

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Abstract

The invention discloses a method for preparing nanometer-level cube-like cobaltosic oxide. The method comprises the following synthetic steps in sequence: dispersing a certain amount of porous carbons into deionized water; ultrasonically dispersing; transferring into a reacting kettle containing the mixed solution of cobalt salt, urea and deionized water; fully stirring and mixing; placing the reacting kettle into an oven; carrying out hydrothermal reaction for a certain time; naturally cooling to reach the room temperature; and centrifugally separating and washing the reaction product by water at a plurality of times, thus obtaining the cube-like cobaltosic oxide powder in a one-step hydrothermal synthesis way. The cube-like cobaltosic oxide powder can be roasted at a high temperature in the air, thus obtaining the porous nanometer-level cube-like cobaltosic oxide. Compared with the conventional synthetic technique, the cobaltosic oxide synthesized by the method disclosed by the invention has the advantages that the porous nanometer-level cube-like structure is provided, the shape and the appearance can be controlled, the dimension is uniformly distributed, the specific surface area is large, the synthesizing process is simple, the repeatability is high, and high characteristics are shown in the field of supercapacitors.

Description

technical field [0001] The invention relates to a method for preparing nano-scale cubic cobalt tetroxide by hydrothermal synthesis. Background technique [0002] Nanomaterials refer to the general term for granular materials with at least one dimension in the three-dimensional space in the nanoscale range (1-100 nanometers) or composed of substances in this scale range as basic units. The unique functions and effects of nanoparticles make nanomaterials not only of great significance in scientific development, but also have good application prospects in practical applications. As an excellent catalyst and battery cathode material, cobalt trioxide nanomaterials have been widely used in photocatalysis, biosensing, supercapacitors, etc. [0003] Hydrothermal synthesis is the main method for preparing cobalt tetroxide. In recent years, uniform precipitation method, solid salt pyrolysis method, sol-gel method, solution heat method, solution atomization oxidation method, non-hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/04B82Y30/00B82Y40/00
Inventor 董晓臣黄维刘湘梅龙庆
Owner NANJING TECH UNIV
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