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Process for temperature-control pressure-control microwave synthesis of water soluble cobaltosic oxide nano crystal

A nanometer and microwave synthesis technology of cobalt trioxide, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., to achieve the effect of mild conditions, simple operation and high crystallinity

Inactive Publication Date: 2006-09-27
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to address the defects of the current solid phase reaction method and water phase synthesis method, to provide a temperature-controlled and pressure-controlled microwave synthesis method for water-soluble cobalt tetroxide nanocrystals, and to synthesize high-quality cobalt tetroxide magnetic nanocrystals in the water phase, which has a synthesis speed Fast, good water solubility and high crystallinity

Method used

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Experimental program
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Embodiment 1

[0015] 1. Preparation of reaction precursor solution:

[0016] Using water as a solvent, mix cobalt nitrate solution with a concentration of 0.1 mol / liter and mercaptopropionic acid, the molar ratio of cobalt ions to mercaptopropionic acid is 1:5, and adjust the pH value of the solution to 12 with sodium hydroxide.

[0017] 2. Microwave synthesis of cobalt tetraoxide nanocrystals:

[0018] The above precursor solution is placed in a closed polytetrafluoroethylene tank, and reacted in a temperature-controllable and pressure-controllable microwave reactor to generate cobalt trioxide nanocrystals.

[0019] The microwave heating conditions are:

[0020] Microwave oscillation frequency: 2450MHZ

[0021] Microwave power: 400W,

[0022] Heating time: 4 hours

[0023] Heating temperature: 140 degrees Celsius.

Embodiment 2

[0025] 1. Preparation of reaction precursor solution:

[0026] Prepare a 0.04 mol / liter cobalt sulfate aqueous solution, add mercaptoethanol as a stabilizer, and control the molar ratio of cobalt ions to mercaptoethanol at 1:2. The pH of the solution was adjusted to 8 with sodium hydroxide.

[0027] 2. Microwave synthesis of cobalt tetraoxide nanocrystals:

[0028] The above precursor solution is placed in a closed polytetrafluoroethylene tank, and reacted in a temperature-controllable and pressure-controllable microwave reactor to generate cobalt trioxide nanocrystals.

[0029] The microwave heating conditions are:

[0030] Microwave oscillation frequency: 2450MHZ

[0031] Microwave power: 600W

[0032] Heating time: 30 minutes,

[0033] Heating temperature: 160 degrees Celsius.

Embodiment 3

[0035] 1. Preparation of reaction precursor solution:

[0036] Prepare a 0.04 mol / L cobalt chloride aqueous solution, add mercaptoethanol as a stabilizer, control the molar ratio of cobalt ions to mercaptoethanol at 1:3, and adjust the pH value of the solution to 10.

[0037] 2. Microwave synthesis of cobalt tetraoxide nanocrystals:

[0038] The above precursor solution is placed in a closed polytetrafluoroethylene tank, and reacted in a temperature-controllable and pressure-controllable microwave reactor to generate cobalt trioxide nanocrystals.

[0039] The microwave heating conditions are:

[0040] Microwave oscillation frequency: 2450MHZ

[0041] Microwave power: 100W

[0042] Heating time: 2 hours

[0043] Heating temperature: 200 degrees Celsius.

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Abstract

The method refers to a temperature and pressure control microwave synthesis of water-soluble cobaltic-cobaltous oxide nanocrystal, using water as solvent, dissolving cobalt salt in water, adding water-soluble mercapto compound as stabilizer, controlling the mol ratio of cobalt ion and water-soluble mercapto compound as 1:10 to 1:1, adjusting solution's pH value to 5-12, getting precursor solution. Afterwards placing the precursor solution in hermetic polytetrafluoroethylene tank, reacting in microwave reactor of temperature and pressure controlled, quickly synthesize cobaltic-cobaltous oxide nanocrystal. The operation of this invention method is simple, the condition is gentle, the cost is low, and the synthetic product cobaltic-cobaltous oxide nanocrystal has the characters of good water-solubility, equal dimension distribution, adjustable size, high degree of crystallization and so on.

Description

technical field [0001] The invention relates to a temperature-controlled and pressure-controlled microwave synthesis method for water-soluble cobalt trioxide nanocrystals. Cobalt salt is used as a raw material to prepare cobalt trioxide magnetic nanocrystals by means of temperature-controlled and pressure-controlled microwave synthesis technology, which belongs to the technical field of nanomaterial preparation. Background technique [0002] co 3 o 4 Widely used in catalysts, pigments, magnetism, electrodes and energy storage materials. When the particle size reaches the nanometer level, due to the scale quantum effect and dielectric confinement effect, they exhibit a series of special magnetic and optical properties, and the large specific surface area makes them have significant advantages in the application of catalysts. [0003] co 3 o 4 The synthesis of commonly used solid phase reaction method and aqueous phase synthesis method. The solid-state reaction method gen...

Claims

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Application Information

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IPC IPC(8): C01G51/04
Inventor 任吉存李良
Owner SHANGHAI JIAO TONG UNIV
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