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Method for preparing Sm2O3 nano crystals by solvent thermal method

A solvothermal method and nanocrystal technology, applied in nanotechnology, chemical instruments and methods, rare earth metal compounds, etc., can solve the problems of easy powder agglomeration, low raw material utilization rate, long sol-gel process cycle, etc., to achieve Avoid agglomeration, avoid the introduction of impurities and structural defects, the effect of light agglomeration

Inactive Publication Date: 2013-08-14
江苏润辉物流有限公司
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  • Summary
  • 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
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 Sm2O3 nano crystals by solvent thermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1: Add analytically pure SmCl 3 ·6H 2 O was added to isopropanol and stirred with a magnetic stirrer to prepare Sm 3+ Solution A with a concentration of 0.5mol / L;

[0019] Step 2: Heat and stir solution A at 40°C, adjust the pH value of solution A to 8 with 5mol / L NaOH solution, and continue stirring for 3 hours to form a precursor solution;

[0020] Step 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 vacuum drying oven, control the solvent heat temperature to 200°C, and the pressure to be 2MPa, react for 48 hours, naturally cool to room temperature after the reaction;

[0021] Step 4: Open the hydrothermal kettle, take out the product, wash with deionized water and centrifuge, then wash with absolute ethanol and centrifuge, repeat washing with deionized water and absolute ethanol for 6 times in turn, and then place it in vacuum drying at 60...

Embodiment 2

[0023] Step 1: Add analytically pure SmCl 3 ·6H 2 O was added to a mixed solvent of isopropanol and water and stirred with a magnetic stirrer to obtain Sm 3+ Solution A with a concentration of 0.3mol / L;

[0024] Wherein, the mixed solvent of isopropanol and water by volume ratio V 水 :V 异丙醇 = 3;

[0025] Step 2: Heat and stir solution A at 50°C, adjust the pH value of solution A to 10 with 3mol / L NaOH solution, and continue stirring for 1 hour to form a precursor solution;

[0026] Step 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 vacuum drying oven, control the solvent heat temperature to 160°C, and the pressure to be 8MPa, react for 72 hours, naturally cool to room temperature after the reaction;

[0027] Step 4: Open the hydrothermal kettle, take out the product, wash with deionized water and centrifuge, then wash with absolute ethanol and centri...

Embodiment 3

[0029] Step 1: Add analytically pure SmCl 3 ·6H 2 O was added to a mixed solvent of isopropanol and water and stirred with a magnetic stirrer to obtain Sm 3+ Solution A with a concentration of 0.6mol / L;

[0030] Wherein, the mixed solvent of isopropanol and water by volume ratio V 水 :V 异丙醇 = 2;

[0031] Step 2: Heat and stir solution A at 60°C, adjust the pH of solution A to 9 with 1mol / L NaOH solution, and continue stirring for 2 hours to form a precursor solution;

[0032] Step 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 vacuum drying oven, control the solvent heat temperature to 240°C, and the pressure to be 12MPa, react for 12 hours, naturally cool to room temperature after the reaction;

[0033] Step 4: Open the hydrothermal kettle, take out the product, wash with deionized water and centrifuge, then wash with absolute ethanol and centrifuge,...

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Abstract

The invention discloses a method for preparing Sm2O3 nano crystals by a solvent thermal method. The method comprises the following steps of: adding analytically pure SmCl3.6H2O into isopropyl alcohol or a mixed solvent of the isopropyl alcohol and water to obtain a solution A; adjusting the pH value of the solution A by using NaOH to form a precursor solution; pouring the precursor solution into a hydrothermal kettle, sealing the hydrothermal kettle, putting into an electric heating vacuum drying oven, and naturally cooling to room temperature after a solvent thermal reaction; and taking a product out, washing by using deionized water, performing centrifugal separation, washing by using absolute ethanol, performing centrifugal separation, repeatedly washing, drying under vacuum, and thus obtaining the Sm2O3 nano crystals. The Sm2O3 nano crystals prepared by the method react in a liquid phase at a time without later-stage crystallization thermal treatment, so that the defects of agglomeration and crystal grain coarsening possibly caused during thermal treatment of the Sm2O3 nano crystals, impurity introduction in an atmosphere reaction and the like are overcome, and process equipment is simple. Agglomeration degrees are relatively low, so that an appropriate chemical measurement ratio and a crystal grain state are easy to obtain; cheaper raw materials can be used; and high-temperature calcination and ball-milling processes are eliminated, so that an impurity introduction defect and a structural defect are overcome.

Description

technical field [0001] The present invention relates to a kind of preparation Sm 2 o 3 The method of nanocrystal, especially relates to a kind of solvothermal method to prepare 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] The currently reported preparation of Sm 2 o 3 The method of nanocrystals is mainly the low-temperature self-propagating combustion method [Bo Lili, Y...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82Y40/00
Inventor 黄剑锋郝巍殷立雄曹丽云吴建鹏
Owner 江苏润辉物流有限公司
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