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Synthetic method for monodispersed cobalt dioxide nanocrystalline

A cobaltous oxide nanometer and synthesis method technology, which is applied in the field of synthesis of inorganic compounds, can solve problems such as high cost, complicated process, and difficult control of particle size

Inactive Publication Date: 2015-09-23
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is aimed at the shortcomings of the existing method for preparing cobaltous oxide, such as high cost, complicated process, and difficult control of particle size.

Method used

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  • Synthetic method for monodispersed cobalt dioxide nanocrystalline
  • Synthetic method for monodispersed cobalt dioxide nanocrystalline
  • Synthetic method for monodispersed cobalt dioxide nanocrystalline

Examples

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Effect test

Embodiment 1

[0035] Under the mixed atmosphere of hydrogen and argon (the hydrogen gas fraction is 10%, the mixed gas flow rate is 40ml / min), put 56mmol dodecylamine (10.4g) and 0.56mmol cobalt (III) acetylacetonate (0.2g) into the three-neck Mix the flask, heat to 80°C in an oil bath for 8 minutes to dissolve cobalt(III) acetylacetonate in dodecylamine to form a uniform reddish-brown solution, then raise the temperature to 200°C and reflux for 1.5h at a heating rate of 10°C / min.

[0036] Stop heating, centrifuge when the solution is cooled to 70°C, and remove the supernatant. The obtained reddish-brown solid was washed with ethanol for 3 times, each time using 15 ml. The collected solid was transferred to a crucible, placed in an oven, and dried at 60° C. for 5 h to obtain the product with a yield of 100%.

Embodiment 2

[0038] Under the mixed atmosphere of hydrogen and argon (hydrogen gas fraction is 20%, mixed gas flow rate 40ml / min), 56mmol tetradecylamine (12g) and 5.6mmol cobalt (II) acetylacetonate (1.44g) are put into three-necked flask Mix and heat to 100°C in an oil bath for 2 minutes to dissolve cobalt(II) acetylacetonate in tetradecylamine to form a uniform reddish-brown solution, then raise the temperature to 200°C and reflux for 3 hours at a heating rate of 10°C / min.

[0039] Stop heating, centrifuge when the solution is cooled to 70°C, and remove the supernatant. The obtained reddish-brown solid was washed with ethanol for 3 times, each time using 15 ml. The collected solid was transferred to a crucible, placed in an oven, and dried at 60° C. for 5 h to obtain the product with a yield of 100%.

Embodiment 3

[0041]Under the mixed atmosphere of hydrogen and argon (hydrogen gas fraction is 40%, mixed gas flow rate 40ml / min), 56mmol octadecylamine (15.1g) and 2.24mmol cobalt (II) acetylacetonate (0.576g) are put into the three neck Mix the flask, heat to 100°C in an oil bath for 2 minutes to dissolve cobalt(II) acetylacetonate in octadecylamine to form a uniform reddish-brown solution, then raise the temperature to 200°C and reflux for 1.5h at a heating rate of 10°C / min.

[0042] Stop heating, centrifuge when the solution is cooled to 70°C, and remove the supernatant. The obtained reddish-brown solid was washed with ethanol for 3 times, each time using 15 ml. The collected solid was transferred to a crucible, placed in an oven, and dried at 60° C. for 5 h to obtain the product with a yield of 100%.

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Abstract

The invention relates to the technical field of synthetic method for inorganic compound, and in particular discloses a synthetic method for a monodispersed cobalt dioxide nanocrystalline. The method main overcomes the defects that the cost is high, the procedures are complex, and the capsule diameter is uneven in an existing method. According to the synthetic method for the monodispersed cobalt dioxide nanocrystalline, long-chain organic amine is used as a thermal solvent, organic cobalt salt is used as a cobalt source, the temperature is lifted to different temperatures to conduct thermal decomposition after uniform mixing is conducted under a certain temperature, and a product is obtained after centrifugation and washing are conducted for many times. By adjusting molar ratio of the solvent and a precursor, the molar ratio range of the thermal solvent and the cobalt source differs from 5:1 to 1600:1, the monodispersed cobalt dioxide nanocrystallines with different diameters are obtained, dispersing is good, the size distribution is narrow, the yield is comparatively high, and the monodispersed cobalt dioxide nanocrystallines can be used for industrial manufacture of nanoscale cobalt dioxide.

Description

technical field [0001] The invention relates to the technical field of synthesis methods of inorganic compounds, in particular to a synthesis method of monodisperse cobaltous oxide nanocrystals. Background technique [0002] As a special transition metal oxide, cobaltous oxide has excellent catalytic performance and unique magnetic properties. Since the 1980s, cobalt powder has been widely used in the field of rechargeable batteries as an activator for charging and discharging high-energy batteries. In the early 1990s, scientists from Japan, Germany and other countries successfully added cobaltous oxide materials to battery raw materials, making it a high-value, high-tech product for the research and development of the battery industry. As a battery material additive with excellent performance, cobalt compounds such as cobalt powder and cobalt oxide powder can improve the proton conductance of Ni(OH)2, reduce the oxidation potential, and increase the oxygen evolution potenti...

Claims

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Application Information

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IPC IPC(8): C01G51/04B82Y30/00
Inventor 王立吕帅李金林张煜华
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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