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Cobaltosic oxide columnar structure material and preparation method thereof

A technology of tricobalt tetroxide and columnar structure, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of uneven appearance, low purity, and low yield of solvothermal method, and achieve uniform dispersion, high purity, and easy large-scale The effect of industrial production

Active Publication Date: 2013-01-02
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] One of the objectives of the present invention is to provide a solvothermal synthesis method of cobalt tetroxide columnar structure material for the defects of the current cobalt tetroxide synthesis method. This method not only has controllable shape, uniform distribution, high crystallinity and low energy consumption, etc. The advantages of the typical solution thermal method, and overcome the defects of low yield, low purity and uneven morphology of the solvothermal method, suitable for large-scale industrial production

Method used

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  • Cobaltosic oxide columnar structure material and preparation method thereof
  • Cobaltosic oxide columnar structure material and preparation method thereof

Examples

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Embodiment 1

[0048] Accurately weigh 5mmol of cobalt acetate, add it to 20ml of distilled water and stir mechanically for 10 minutes to fully dissolve the cobalt acetate, then add 10ml of glycerol into the cobalt acetate solution and mechanically stir for 20 minutes, accurately weigh Dissolve 5 mmol of urea into the above mixed solution and mechanically stir for 1 hour, put the uniformly dispersed mixed solution into an autoclave and seal it, keep it at a reaction temperature of 150°C for 5 hours, and then wash it with distilled water and absolute ethanol for 5 hours. First, dry at 80°C for 12 hours in a vacuum drying oven to obtain a cobalt carbonate precursor with a columnar structure, and place the precursor in a muffle furnace for calcination at 350°C for 3 hours to obtain a columnar structure cobalt tetroxide material with a particle diameter of 8~10μm, the cobalt content in the particles is 74.31~74.48%.

Embodiment 2

[0050] Accurately weigh 6.5mmol of cobalt acetate, add it to 25ml of distilled water and mechanically stir for 10 minutes to fully dissolve the cobalt acetate, then add 5ml of glycerol into the cobalt acetate solution and mechanically stir for 20 minutes, accurately Weigh 5mmol of urea and dissolve it into the above mixed solution and stir it mechanically for 2 hours, put the uniformly dispersed mixed solution into an autoclave and seal it, keep it at a reaction temperature of 160°C for 15 hours, and then wash it with distilled water and absolute ethanol respectively 5 times, dry in a vacuum oven at 80°C for 20 hours to obtain a cobalt carbonate precursor with a columnar structure, and place the precursor in a muffle furnace for calcination at 250°C for 3 hours to obtain a columnar structure cobalt tetroxide material with a particle size of 9~ 12μm, the cobalt content in the particles is 74.35~74.50%.

Embodiment 3

[0052] Accurately weigh 7.5mmol of cobalt acetate, add it to 20ml of distilled water and stir mechanically for 10 minutes to fully dissolve the cobalt acetate, then add 10ml of glycerol into the cobalt acetate solution and mechanically stir for 20 minutes, accurately Weigh 5mmol of urea and dissolve it into the above mixed solution and stir it mechanically for 1 hour, put the uniformly dispersed mixed solution into an autoclave and seal it, keep it at a reaction temperature of 180°C for 5 hours, and then wash it with distilled water and absolute ethanol respectively 5 times, dry in a vacuum oven at 60°C for 24 hours to obtain a cobalt carbonate precursor with a columnar structure, and place the precursor in a muffle furnace for calcination at 400°C for 3 hours to obtain a columnar structure cobalt tetroxide material with a particle size of 8~ 9μm, the cobalt content in the particles is 74.32~74.49%. .

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Abstract

The invention provides a cobaltosic oxide columnar structure material and a preparation method thereof and belongs to the field of inorganic materials. The preparation method specifically includes adding glycerol with a certain volume ratio in a cobaltous acetate aqueous solution, fully mixing, adding an appropriate amount of urea to serve as a precipitating agent, uniformly dispersing, sealing a mixed solution in a high-pressure autoclave, reacting for a certain time at the specific temperature, performing suction filtration, washing, drying, and performing calcination in the air in a muffle furnace to obtain the cobaltosic oxide with the columnar structure. According to the cobaltosic oxide columnar structure material and the preparation method thereof, the operation process of the method is simple, the productivity is high, the cost is low, any surface active agent is not added, the material is free of pollution, the prepared cobaltosic oxide is neat in appearance, uniform in dispersion, high in particle density, and the cobaltosic oxide columnar structure material and the preparation method thereof are expected to be widely used in the fields of lithium ion batteries, supercapacitor, gas sensors, biosensing and catalysis and the like.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular, the invention relates to a tricobalt tetroxide material and a preparation method thereof. Background technique [0002] co 3 o 4 The appearance of the powder is black or gray black, the theoretical cobalt content is 73.43%, the oxygen content is 26.57%, and the bulk density is 0.5~1.5g / cm 3 , tap density 6.0~6.2g / cm 3 . co 3 o 4 As a typical spinel-type transition metal oxide, due to its special structure and properties, it has a wide range of applications in the fields of electrochemistry, catalysis, gas sensing, biosensing, magnetic materials, and electrochromic thin films. [0003] Co 3 o 4 There are many methods of powder preparation, including solvothermal method, spray thermal decomposition method, reduction oxidation method, uniform precipitation method, mechanical ball milling method, room temperature solid-phase reaction method and hydrothermal method, etc. Among...

Claims

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Application Information

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IPC IPC(8): C01G51/04
Inventor 谭强强刘少军
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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