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Preparing process of monodisperse nano metal oxide particle

A nanoparticle and oxide technology, applied in the field of nanomaterials, can solve the problems of difficult to control the pH value of the reaction solution, unfavorable for industrialized production, small single output, etc., and achieve controllable particle size, short reaction time and simple operation. Effect

Inactive Publication Date: 2007-06-27
TIANJIN UNIV
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Problems solved by technology

The existing thermal decomposition method of metal organics has a small unit yield, generally less than 1g, and the reaction reagents and media are expensive and highly toxic. Sometimes it needs to be operated under strict conditions such as vacuum or inert gas protection, which is not conducive to industrial production.
The disadvantage of the gel method is that the pH value of the reaction solution is difficult to control, and precipitation is easy to form, and the obtained particles need to be further roasted and ground.

Method used

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  • Preparing process of monodisperse nano metal oxide particle

Examples

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Effect test

Embodiment 1

[0020] Embodiment 1 Preparation of iron oxide monodisperse nanoparticles

[0021] FeCl 3 ·6H 2 O reacts with sodium stearate to form iron stearate, and then disperses iron stearate and stearic acid in the double-distilled diesel oil at 298-352°C with a molar ratio of 2:1, wherein the concentration of iron stearate is 0.05mol / L. The reactants were heated from room temperature, and the heating rate of the nucleation stage was controlled to be 3 °C min -1 . Heat up to the nucleation temperature of 200°C, stop heating, and react at this temperature for 1h. After a large amount of nucleation, control the temperature rise rate in the growth stage to 5°C min -1 Heat the dispersion medium containing crystal nuclei to boiling, react at this temperature for 30 minutes, and the final boiling temperature is 268°C. The reaction solution was cooled to room temperature to obtain a stable nanoparticle dispersion system. The size of the iron oxide nanoparticles is 5nm, and the dispersio...

Embodiment 2

[0022] The preparation of embodiment 2 copper oxide monodisperse nanoparticles

[0023] First react copper sulfate pentahydrate with sodium oleate to generate copper oleate, then disperse copper oleate and oleic acid in the redistilled liquid paraffin of 311-354°C fraction in a molar ratio of 3:1, wherein the concentration of copper oleate is 0.25mol / L. The reactants start from room temperature at 5°C·min -1 The heating rate is slow heating. Heat up to the nucleation temperature of 230°C, stop heating, and react within this temperature range for 30 minutes. Continue heating after a large number of crystal nuclei are formed, and control the heating rate to 9°C min -1 Heat the dispersion medium containing crystal nuclei to boiling, and react at this temperature for 50 minutes, and the final boiling temperature is 289°C. After the reaction, add 2 to 3 times the volume of methanol to precipitate, centrifuge for 15 minutes, and dry to obtain nano-copper oxide powder, which can ...

Embodiment 3

[0024] The preparation of embodiment 3 zinc oxide nanoparticles

[0025] Zinc acetate and palmitic acid are dispersed in double-distilled kerosene or double-distilled camphor oil at 328-370° C. in a molar ratio of 4:1, wherein the concentration of zinc acetate is 0.30 mol / L. The reactants start from room temperature at 6°C·min -1 The heating rate is slow heating. Heat up to the nucleation temperature of 300°C and stop heating, and react within this temperature range for 3.5 hours. After a large amount of nucleation, control the heating rate to 12°C min -1 Rapidly heat the dispersion medium containing crystal nuclei to boiling, and react at this temperature for 5 hours, and the final boiling temperature is 370°C. After the reaction, add 2 to 3 times the volume of ethanol to precipitate, centrifuge for 20 minutes, and dry to obtain nano-zinc oxide powder, which can be re-dispersed in a mixed solution of toluene and xylene to obtain stable nano-particle dispersion system. . ...

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Abstract

The process of preparing monodisperse nanometer metal oxide particle includes the following steps: 1. preparing solution with surfactant 0.25-1 weight portions and dispersing medium 2-10 weight portions, adding metal oxide to the concentration of 0.05-0.5 mol / L, and heating in the temperature raising rate of 3-6 deg.c / min to the nucleation temperature 150-300 deg.c to react for 0.5-3.5 hr; and 2. heating to the dispersing medium boiling temperature 210-370 deg.c in the temperature raising rate of 5-12 deg.c / min for controlling the growth and reflux reaction in boiling state for 0.5-5 hr to form the monodisperse nanometer metal oxide particle. The present invention realizes the preparation of monodisperse nanometer particle, and may be used in preparing different kinds of nanometer metal oxide particle.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a method for preparing monodisperse metal oxide nanoparticles. Background technique [0002] Monodisperse nanoparticles have become a research hotspot at home and abroad because of their significance in the field of basic scientific research and attractive application prospects. For nanomaterials, the size and particle size distribution of nanoparticles are very important, because many properties of nanoparticles, such as optics and magnetism, depend on the particle size scale. Therefore, the preparation of monodisperse nanoparticles with particle size deviation <5% is a difficult task. The main preparation method in the early stage was hydrothermal synthesis. However, the obtained particles need to be further calcined, and the particle size is large and widely distributed, which is difficult to control. At present, the gel method and the thermal decomposition m...

Claims

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Application Information

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IPC IPC(8): C01G1/02
Inventor 高建平王雅琦刘妍
Owner TIANJIN UNIV
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