Method for preparing monoclinic Sm2O3 nanocrystal through solvothermal method

A solvothermal method and monoclinic phase technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of low raw material utilization rate, easy powder agglomeration, long sol-gel process cycle, etc., to achieve Avoiding the introduction of impurities and structural defects, avoiding agglomeration, and the effect of strong absorption

Inactive Publication Date: 2013-01-30
SHAANXI UNIV OF SCI & TECH
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  • Description
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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
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 monoclinic Sm2O3 nanocrystal through solvothermal method

Examples

Experimental program
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Effect test

Embodiment 1

[0021] 1) The analytically pure SmCl 3 ·6H 2 O was added to absolute ethanol and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.1mol / L;

[0022] 2) Heat and stir solution A at 40°C, adjust the pH value of solution A to 6 with NaOH solution with a concentration of 1mol / L, and continue stirring for 1 hour to form a precursor solution;

[0023] 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 solvent heat temperature to 120°C, and the pressure to be 8MPa, react for 48 hours, naturally cool to room temperature after the reaction;

[0024] 4) Turn on the hydrothermal kettle, take out the product, wash it with deionized water and centrifuge it, then wash it with deionized ethanol and centrifuge it, repeat the washing with deionized water and absolute ethanol for 6 times, and then place it in ...

Embodiment 2

[0026] 1) The analytically pure SmCl 3 ·6H 2 O was added to absolute ethanol and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.5mol / L;

[0027] 2) Heat and stir solution A at 60°C, adjust the pH value of solution A to 9 with NaOH solution with a concentration of 2mol / L, and continue stirring for 1.5 hours to form a precursor solution;

[0028] 3) Pour the precursor solution into the hydrothermal kettle, the filling degree is controlled at 55%, then seal the hydrothermal kettle, put it into the DHG-9075A electric blast drying oven, control the solvent heat temperature to 200 ℃, and the pressure to be 15MPa, react for 60 hours, naturally cool to room temperature after the reaction;

[0029] 4) Open the hydrothermal kettle, take out the product, wash it with deionized water and centrifuge it, then wash it with anhydrous ethanol and centrifuge it, repeat the washing with deionized water and anhydrous ethanol 4 times in turn, and place it ...

Embodiment 3

[0031] 1) The analytically pure SmCl 3 ·6H 2 O was added to ethanol aqueous solution and stirred with a magnetic stirrer to obtain Sm3+ Solution A with a concentration of 0.3mol / L;

[0032] Among them, water and ethanol in the ethanol aqueous solution are V 水 :V 乙醇 =1 volume ratio mixed to get;

[0033] 2) Heat and stir solution A at 50°C, adjust the pH value of solution A to 10 with NaOH solution with a concentration of 3.5mol / L, and continue to stir for 2 hours to form a precursor solution;

[0034] 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 solvent heat temperature to 160°C, and the pressure to be 204);

[0035] 4) Open the hydrothermal kettle, take out the product, wash it with deionized water and centrifuge it, then wash it with anhydrous ethanol and centrifuge it, wash it with deionized water and anhydrous etha...

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Abstract

The invention relates to a method for preparing a monoclinic Sm2O3 nanocrystal through a solvothermal method, which comprises the following steps: adding SmCl3.6H2O into anhydrous ethanol or an ethanol water solution to prepare a solution A; regulating the pH value of the solution A with an NaOH solution until the pH value is 6-12, and then further stirring to form a precursor solution; pouring the precursor solution into a hydrothermal kettle, then sealing the hydrothermal kettle, reacting for 6-60 hours while controlling the solvothermal temperature at 120-240 DEG C and the pressure at 2-20 MPa, and naturally cooling to room temperature when the reaction is finished; and taking out the product, washing with deionized water, performing centrifugal separation, then washing with anhydrous ethanol, performing centrifugal separation, repeatedly washing with deionized water and anhydrous ethanol sequentially, and then drying at 50-80 DEG C to obtain the monoclinic Sm2O3 nanocrystal. The preparation reaction of the Sm2O3 nanocrystal is finished in the liquid phase in one step without later crystallization heat treatment, so that the defects possibly caused in the heat treatment process of the Sm2O3 nanocrystal, such as aggregation, grain growth coarsening, impurity introduction due to atmosphere reaction and the like, can be avoided; and the technological equipment is simple.

Description

Technical field: [0001] The invention relates to a method for preparing monoclinic Sm 2 o 3 Nanocrystalline method, in particular to a solvothermal method for the preparation of monoclinic Sm 2 o 3 nanocrystal approach. 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 a monoclinic crysta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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