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Preparation process of nanometer RE oxide particle

A technology of rare earth fluorides and nanoparticles, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc.

Active Publication Date: 2010-12-22
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can control the size of nanocrystals within a certain range, it is not suitable for the preparation of other rare earth fluorides due to its narrow application range.
In 2005 in "Inorg.Chem." magazine, Li Yadong's group reported the use of hydrothermal technology to synthesize a series of rare earth fluorides. This method can prepare monodisperse nanoparticles, but the process uses the volatile organic solvent cyclohexane amines, in addition, the product yield obtained by this method is also very small
However, the preparation of the precursor is complex and the reaction conditions are harsh
[0003] To sum up, most of the reported methods for synthesizing rare earth fluorides use volatile organic solvents, and the reaction conditions are relatively harsh, and there is uneven morphology , low output and other issues

Method used

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  • Preparation process of nanometer RE oxide particle
  • Preparation process of nanometer RE oxide particle
  • Preparation process of nanometer RE oxide particle

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Take 1mL of 0.3g / mL cerium nitrate ethanol solution, add it to 10mL 1-octyl-3-methyl-hexafluorophosphate, stir the mixture evenly, then add it into a 18mL stainless steel pressure-resistant reactor, After reacting at ℃ for 10 hours, the reaction solution was diluted with 3 times the volume of the reaction solution in absolute ethanol, the product was centrifuged, washed with absolute ethanol, and dried to obtain a rare earth fluoride nanoparticle. The XRD pattern confirms the product

[0025] For cerium trifluoride. The product obtained by SEM observation is disc-like nanoparticles with uniform size, about 200 nanometers in diameter and about 20 nanometers in thickness.

Embodiment 2

[0027] Take 3mL of 0.02g / mL ethanol solution of lanthanum nitrate, add it to 15mL 1-hexyl-3-methyl-hexafluorophosphate, stir the mixture evenly, then add it to a 18mL stainless steel pressure-resistant reaction kettle, After reacting for 12 hours, dilute the reaction solution with 3 times the volume of the reaction solution in absolute ethanol, centrifuge to separate the product, wash with absolute ethanol, and dry to obtain a rare earth fluoride nanoparticle. The XRD pattern confirmed that the product was lanthanum trifluoride. The product observed by SEM is a disk-shaped particle with a diameter of about 50-100 nanometers and a thickness of about 10 nanometers.

Embodiment 3

[0029] Take 2mL of 0.1g / mL praseodymium nitrate ethanol solution, add it to 10mL 1-butyl-3-methyl-hexafluorophosphate, stir the mixture evenly, then add it into a 18mL stainless steel pressure-resistant reaction kettle, at 50 After reacting at ℃ for 10 hours, the reaction solution was diluted with 3 times the volume of the reaction solution in absolute ethanol, the product was centrifuged, washed with absolute ethanol, and dried to obtain a rare earth fluoride nanoparticle. The XRD spectrum confirmed that the product was praseodymium trifluoride. The product observed by SEM is a disc-shaped particle with a diameter of about 150 nanometers.

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Abstract

The present invention provides preparation process of nanometer RE fluoride particle. Alcohol solution of RE compound is dispersed in fluorine-containing ionic liquid, and the ionic liquid is heated to decompose and to produce fluorine ion combined with RE ion, so as to prepare great amount of nanometer RE fluoride particles in homogeneous shape. The prepared nanometer particles have size of 50-200 nm and may find wide application in biology, catalyst, lubricant, analysis, optics and other fields. The present invention completes reaction in a green solvent system, and is environment friendly.

Description

technical field [0001] The invention relates to a method for preparing nanoparticles, in particular to a method for preparing rare earth fluoride nanoparticles. Background technique: [0002] Rare earth fluoride nanomaterials are widely used in luminescence, medicine, biology, lubrication and other fields. Various methods for the synthesis of fluoride nanoparticles have been developed. For example, Jan W. Stouwdam et al published in Nano Letter in 2002 the synthesis of doped lanthanum fluoride nanoparticles by a liquid-phase method using dioctadecyl ammonium dithiophosphate as a ligand. The size and shape of the product are not uniform. In 2004, Yi Guangshun and others reported in Nano Letter that Yb and Er-doped NaYF were prepared by reacting EDTA-coordinated rare earth ions with sodium fluoride. 4 Nanocrystalline. Although this method can control the size of nanocrystals within a certain range, its application is narrow and it is not suitable for preparing other rare ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
CPCY02P20/54
Inventor 陈继张弨
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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