Method for synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase

A rare earth fluoride, fluorescent nanotechnology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of large particle size of reaction products, reduced reaction efficiency, long-term grinding, etc., and is easy to master and control. The effect of reaction conditions, high purity and low production cost

Inactive Publication Date: 2010-10-20
WUHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in their methods, microwave heating is used for solid-phase synthesis, and the reactants need to be ground for a long time, and the reaction temperature is also high, which reduces the reaction efficiency, consumes more energy, and the particle size of the reaction product is relatively large.

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  • Method for synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase
  • Method for synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase
  • Method for synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase

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Effect test

Embodiment 1

[0024] (1) Yttrium chloride, ytterbium chloride, erbium chloride, sodium chloride, ammonium fluoride and surfactant polyethyleneimine are dissolved in ethylene glycol respectively, and the concentration of rare earth chloride is 0.5mol / L, The concentration of sodium chloride is 0.2mol / L, the concentration of ammonium fluoride is 1.6mol / L, and the volume ratio of the mass of polyethyleneimine to the solvent is 1g: 20mL;

[0025] (2) Mix 9mL ethylene glycol, 5mL polyethyleneimine solution, 2.5mL sodium chloride solution, 0.7mL yttrium chloride solution, 0.2mL ytterbium chloride solution, 0.1mL erbium chloride solution and 2.5mL ammonium fluoride solution After adding it into the reaction vessel and stirring for 20 minutes, it was heated under reflux with a microwave at 600W, and the temperature was controlled at 180°C for 20 minutes, then it was left to cool to room temperature, and then centrifuged to separate the nanomaterials;

[0026] (3) Wash the nanomaterials separated in ...

Embodiment 2

[0029] (1) Lanthanum chloride, cerium chloride, terbium chloride, ammonium fluoride and surfactant polyethyleneimine are dissolved in deionized water respectively, the concentration of rare earth chloride is 0.5mol / L, and the concentration of ammonium fluoride is 1.6mol / L, the volume ratio of the mass of polyethyleneimine to the solvent is 1g: 20mL;

[0030] (2) 13mL water, 5mL polyethyleneimine solution, 0.85mL lanthanum chloride solution, 0.1mL cerium chloride solution, 0.05mL terbium chloride solution and 1mL ammonium fluoride solution were added to the reaction vessel and stirred for 10 minutes, It was heated under reflux with microwave 600W and magnetically stirred, and reacted at 90°C for 20 minutes, then allowed to stand and cooled to room temperature, and then centrifuged to separate nanomaterials;

[0031] (3) Wash the nanomaterials separated in the previous step with absolute ethanol or deionized water to remove unreacted ions therein, and then vacuum-dry them to obt...

Embodiment 3

[0034] (1) Calcium chloride, cerium chloride, terbium chloride, sodium chloride, ammonium fluoride and surfactant polyethyleneimine are dissolved in ethylene glycol respectively, and the concentrations of rare earth chloride and sodium chloride are both 0.5mol / L, the concentration of ammonium fluoride is 1.6mol / L, and the volume ratio of the mass of polyethyleneimine to the solvent is 1g: 20mL;

[0035] (2) Mix 10.5mL ethylene glycol, 5mL polyethyleneimine solution, 1mL sodium chloride solution, 0.85mL sodium chloride solution, 0.1mL cerium chloride solution, 0.05mL terbium chloride solution and 2.5mL ammonium fluoride solution After adding it into the reaction vessel and stirring for 20 minutes, heat it under reflux with a microwave at 600W and nitrogen gas, control the temperature at 180°C for 20 minutes, then let it stand to cool to room temperature, and then centrifuge to separate the nanomaterials;

[0036] (3) Wash the nanomaterials separated by centrifugation in the pre...

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Abstract

The invention discloses a method for synthesizing fluorescent nano particles of rare earth chlorides by microwave aqueous phase. The method comprises the following steps: firstly, dispersing rare earth chlorides, a surface active agent, sodium chloride and ammonium fluoride in a hydrophilic solvent, then adding the obtained mixture into a microwave reactor according to certain proportion, stirring for 10-20 minutes, carrying out microwave heating, after the mixture reacts fully, centrifugally separating nano materials, using alcohol or deionized water to clean the nano materials so as to remove unreacted ions therein, then carrying out vacuum drying on the obtained nano materials, i.e. obtaining the needed water-soluble rare earth nano particles. The method has simple preparation technique, short production period, easy control of reaction conditions, no impurity introduction, low production cost and no fluoride-containing wastewater discharge, saves energy by 30%-50% compared with the prior art, and is beneficial to environmental protection and industrial production. The prepared fluorescent nano particles of rare earth chlorides have good uniformity, good dispersibility in water and small particle size, and can be used for the fields of biological fluorescent labeling, infrared detection and the like.

Description

technical field [0001] The invention belongs to the technical field of fluorescent nanometer material preparation, in particular to a preparation method of rare earth fluoride fluorescent nanoparticle. Background technique [0002] Rare earth fluoride is an important raw material for producing a single rare earth metal by metallothermic reduction, and it also has important uses in carbon arc rod luminescent agents, steel and non-ferrous metal alloy additives, etc. With the development and utilization of new materials such as fluoride optical fiber and infrared phosphor, the amount of rare earth fluoride is increasing day by day. In recent years, due to its special physical and chemical characteristics, as well as its high performance in ultramicronization, high-density integration, and high spatial resolution, nanotechnology has brought humans into a vibrant high-tech field-nanotechnology field. Nanoization brings various spectral characteristics to rare earth fluoride lum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85B82B3/00
Inventor 喻学锋何定飞向阳
Owner WUHAN UNIV
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