Method for preparing spherical Sm2O3 semiconductor nanocrystals by means of complex hydrothermal method

A hydrothermal and semiconductor technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of easy powder agglomeration process cycle, low utilization rate of raw materials, nanocrystal agglomeration, etc., to avoid the introduction of impurities and Structural defects, strong uptake, fully developed effects

Inactive Publication Date: 2013-01-30
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The low-temperature self-propagating combustion method and the sol-gel method are high-temperature synthesis of Sm under oxygen atmosphere 2 o 3 , the powder is easy to agglomerate and the sol-gel process cycle is long, for Sm 2 o 3 The utilization rate of raw materials is very small; and the solid phase sintering method is sintered under reducing atmosphere conditions, which will also cause the agglomeration of nanocrystals and abnormal growth of particles
At the same time, the precursor prepared by the microemulsion method also needs high temperature heat treatment to obtain Sm 2 o 3 Nano-crystalline, which is easy to introduce impurities, and the powder is easy to agglomerate

Method used

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  • Method for preparing spherical Sm2O3 semiconductor nanocrystals by means of complex hydrothermal method
  • Method for preparing spherical Sm2O3 semiconductor nanocrystals by means of complex hydrothermal method

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Experimental program
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Effect test

Embodiment 1

[0020] 1) The analytically pure SmCl 3 ·6H 2 O was added to deionized water and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.1mol / L;

[0021] 2) Heat and stir solution A at 35°C and use NaOH solution with a concentration of 1mol / L to adjust the pH value of solution A to 6 to form a precursor solution; then add trisodium citrate to the precursor solution, the amount of which is the same as the theoretical yield of the product The ratio of the amount of the substance is n=0.2; the pH value of the precursor solution is determined to be 6 again;

[0022] 3) Pour the precursor solution into the hydrothermal kettle, the filling degree is controlled at 50%, then seal the hydrothermal kettle, put it into a DHG-9075A electric blast drying oven, control the hydrothermal temperature to 140°C, and the pressure 8MPa, reacted for 48 hours, and naturally cooled to room temperature after the reaction;

[0023] 4) Turn on the hydrothermal kettle, ta...

Embodiment 2

[0025] 1) The analytically pure SmCl 3 ·6H 2 O was added to deionized water and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.5mol / L;

[0026] 2) Heat and stir solution A at 45°C and use NaOH solution with a concentration of 2 mol / L to adjust the pH value of solution A to 7 to form a precursor solution; then add trisodium citrate to the precursor solution, the amount of which is the same as the theoretical yield of the product The ratio of the amount of the substance is n=1; the pH value of the precursor solution is determined to be 7 again;

[0027] 3) Pour the precursor solution into the hydrothermal kettle, the filling degree is controlled at 55%, then seal the hydrothermal kettle, put it into a DHG-9075A electric blast drying oven, control the hydrothermal temperature to 200°C, and the pressure 15MPa, reacted for 60 hours, and naturally cooled to room temperature after the reaction;

[0028] 4) Open the hydrothermal kettle, take ...

Embodiment 3

[0030] 1) The analytically pure SmCl 3 ·6H 2 O was added to deionized water and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 1.5mol / L;

[0031] 2) Heat and stir solution A at 40°C and use NaOH solution with a concentration of 3.5mol / L to adjust the pH value of solution A to 8 to form a precursor solution; then add trisodium citrate to the precursor solution, the amount added is consistent with the product theory The ratio of the amount of substance produced is n=0.6; the pH value of the precursor solution is determined to be 8 again;

[0032] 3) Pour the precursor solution into the hydrothermal kettle, the filling degree is controlled at 60%, then seal the hydrothermal kettle, put it into a DHG-9075A electric blast drying oven, control the hydrothermal temperature to 160°C, and the pressure 20MPa, reacted for 72 hours, and naturally cooled to room temperature after the reaction;

[0033] 4) Open the hydrothermal kettle, take out the pro...

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Abstract

A method for preparing spherical Sm2O3 semiconductor nanocrystals by means of a complex hydrothermal method includes the following steps: analytically pure SmC13.6H2O is added into deionized water, so that solution A is prepared; after NaOH solution is used for regulating the pH value of the solution A to 6 to 10, precursor solution is formed, the precursor solution is then added with trisodium citrate and poured into a hydrothermal kettle, the hydrothermal kettle is then sealed, the hydrothermal temperature is controlled at 140 DEG C to 240 DEG C, the pressure is 2MPa to 20MPa, reaction is carried out for 6 to 72 hours, and after reaction is finished, the hydrothermal kettle is naturally cooled to room temperature; product is taken out, washed with deionized water, centrifugalized, then washed with absolute ethyl alcohol and centrifugalized, and after deionized water and absolute ethyl alcohol are sequentially adopted to repetitively wash the product and the product is dried, the spherical Sm2O3 semiconductor nanocrystals are obtained. Since the reaction for preparing the spherical Sm2O3 semiconductor nanocrystals is carried out in one step in the liquid phase without needing later-stage crystallization heat treatment, agglomeration, grain coarsening, impurities introduced into atmospherical reaction and other defects probably caused in the process of Sm2O3 nanocrystal heat treatment are prevented, and moreover, the process equipment is simple.

Description

Technical field: [0001] The present invention relates to a Sm 2 o 3 A method for preparing semiconductor nanocrystals, in particular to a complex hydrothermal method for preparing spherical Sm 2 o 3 Methods for semiconductor nanocrystals. 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, semiconductor materials and high-performance catalyst materials. Nano Sm 2 o 3 Can also be used for ceramic capacitors. In terms of magnetic materials, nano Sm 2 o 3 It is mainly used to prepare rare earth permanent magnet materials; in addition, Sm 2 o 3 Thin films can also be used in electronic devices, magnetic materials and optical filters of special glass, and have broad development prospects. [0003] SM 2 o 3 The crystal has three crystal forms, which belong to the oxide of polycrystalline phase transformation. It is ...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y30/00
Inventor 殷立雄黄剑锋郝巍李嘉胤吴建鹏曹丽云费杰
Owner SHAANXI UNIV OF SCI & TECH
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