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Method for preparing Sm2O3 nano powder by microwave-hydrothermal method

A technology of microwave hydrothermal method and nano-powder, which is applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve the problems of low utilization rate of raw materials, expensive equipment and equipment, and high equipment requirements, and achieve low cost and high particle size. The effect of uniformity and simple process equipment

Inactive Publication Date: 2011-03-02
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two methods have very high requirements on equipment, and the equipment and instruments are relatively expensive. Since evaporation exists in the entire container, it is difficult for Sm 2 o 3 The utilization rate of raw materials is very small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1: First, analytically pure SmCl 3 ·6H 2 O was added to deionized water, stirred on a magnetic stirrer to dissolve, and Sm 3+ A transparent solution A with a concentration of 0.8mol / L; secondly, stir the transparent solution A at 55°C for 3 hours, and adjust the pH value of the solution to 5.4 to form a solution B with a mass percentage of 8% ammonia solution; then, the solution B is poured into the microwave hydrothermal reactor, the filling degree is controlled at 80%, the microwave hydrothermal kettle is sealed, and it is put into the MDS-8 temperature-pressure dual-control microwave hydrothermal reactor, and the hydrothermal temperature is controlled at 110°C. React for 4 hours, cool down to room temperature naturally after the reaction is over; finally, turn on the hydrothermal kettle, centrifuge the product at 4000 rpm, then wash 4 times with absolute ethanol to make the product particles indirect and loose, and place at 100°C Sm can be obtained after dr...

Embodiment 2

[0012] Example 2: First, analytically pure SmCl 3 ·6H 2 O was added to deionized water, stirred on a magnetic stirrer to dissolve, and Sm 3+ A transparent solution A with a concentration of 1.7mol / L; secondly, stir the transparent solution A at 48°C for 4 hours, and adjust the pH value of the solution to 5.6 by using a 5% ammonia solution by mass percentage to form a solution B; then, the solution B is poured into the microwave hydrothermal kettle, the filling degree is controlled at 75%, the microwave hydrothermal kettle is sealed, and it is put into the MDS-8 temperature-pressure dual-control microwave hydrothermal reactor, and the hydrothermal temperature is controlled at 180°C. React for 2 hours, cool down to room temperature naturally after the reaction is over; finally, turn on the hydrothermal kettle, centrifuge the product at 4000 rpm, then wash with isopropanol 4 times to make the product particles indirect and loose, and place at 80°C Sm can be obtained after dryin...

Embodiment 3

[0013] Example 3: First, analytically pure SmCl 3 ·6H 2 O was added to deionized water, stirred on a magnetic stirrer to dissolve, and Sm 3+ A transparent solution A with a concentration of 1.0 mol / L; secondly, stir the transparent solution A at 52° C. for 5 hours, and adjust the pH value of the solution to 5.9 with a mass percentage of 9% ammonia solution to form a solution B; then, the solution B is poured into a microwave hydrothermal kettle, the filling degree is controlled at 67%, the microwave hydrothermal kettle is sealed, and it is put into an MDS-8 temperature-pressure dual-control microwave hydrothermal reactor, and the hydrothermal temperature is controlled at 150°C. React for 3 hours, cool down to room temperature naturally after the reaction is over; finally, turn on the hydrothermal kettle, centrifuge the product at 4000 rpm, then wash 4 times with absolute ethanol to make the product particles indirect and loose, and place at 120°C Sm can be obtained after dry...

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Abstract

The invention discloses a method for preparing Sm2O3 nano powder by a microwave hydro-thermal method, wherein, analytically pure SmCl3 question mark 6H2O is added into de-ionized water and stirred in a magnetic stirring apparatus to obtain a transparent solution A; the transparent solution A is heated and the pH value of the solution A is adjusted to be 5.4 to 6.0 by an ammonia solution so as to form a solution B; the solution B is poured into a microwave hydro-thermal kettle which is then sealed and put into an MDS-8 type warm-pressing dual-control microwave hydro-thermal reactor for carrying out hydro-thermal reaction, and then naturally cooled to the room temperature after the completion of the reaction; the hydro-thermal kettle is opened and products are centrifugalized with the speedof 4,000 rev. / minute so as to ensure that indirect and loose product particles are obtained; and then the product particles are arranged in a vacuum drying chamber for drying. As the reaction for preparing Sm2O3 nano powder is completed by one-time operation in liquid phase, post annealing heat treatment is not needed. Furthermore, the method has simple processing equipment and low cost, the prepared nano material has uniform particle size which ranges from 10nm to 50nm, and is evenly distributed.

Description

technical field [0001] The present invention relates to a kind of preparation Sm 2 o 3 The method for nanopowder, particularly relates to a kind of microwave hydrothermal preparation Sm 2 o 3 nanopowder method. Background technique [0002] SM 2 o 3 It is a light yellow powder, easy to deliquescence, insoluble in water, soluble in inorganic acid. SM 2 o 3 It is a new generation of energy conversion materials and photoelectric thin film materials. SM 2 o 3 Thin films can be used to prepare optical switches, data storage, photoelectric conversion elements and electrical switches, etc.; Sm 2 o 3 Thin films can also be used in filters of electronic devices, magnetic materials and special glasses; in addition, nano-Sm 2 o 3 It can also be used in ceramic capacitors and catalysts, and has broad development prospects [0003] The currently reported preparation of Sm 2 o 3 The method of optical film is mainly the method of vacuum evaporation [V.A.Rozhkov, A.Yu.Truso...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 殷立雄黄剑锋曹丽云李娟莹黄艳马小波朱佳
Owner SHAANXI UNIV OF SCI & TECH