High-efficiency preparation method of rare-earth fluoride nanoparticle

A technology of rare earth fluorides and nanoparticles, applied in the fields of rare earth metal compounds, chemical instruments and methods, nanotechnology, etc., can solve the problems of large size, increased average particle size, and inability to meet small size nanoparticles, and achieve synthesis efficiency High, fast reduction effect

Inactive Publication Date: 2013-05-01
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] From the current point of view, the methods for synthesizing rare earth fluoride nanoparticles mainly include: hydrothermal synthesis method, the specific operation is: dissolving rare earth oxide powder in a volume fraction of A clear and transparent solution was obtained in 10% nitric acid solution, solid NaF was added to form a colloidal precipitate, and the molar ratio of F to rare earth element Ln was controlled at 3:1. Then the pH value was adjusted to 4 with 10% KOH solution .0-5. 0. Finally, put the jelly mixture into a 100 mL hydrothermal reaction kettle with a polytetrafluoroethylene liner, seal it and keep it at 100°C for 16 h. Centrifugal separation and deionized water were fully washed and collected and dried; the reaction was subject to hydrothermal reaction conditions, and when other conditions were kept constant, the average particle size increased with the increase of hydrothermal reaction temperature; hydrothermal synthesis has an operational The advantages of simplicity, but the average particle size of spherical or quasi-spherical particles is 35-39 nm, which is large in size and cannot meet the growing demand for small-sized nanoparticles

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of hyperbranched polymers: choose the hydrophobic bromine-containing hyperbranched polyether with a branching degree of 20% as the macromolecular initiator, choose copper bromide as the catalyst, and choose hexamethyltriethylenetetramine as the polynitrogen ligand; Put the bromine-containing hyperbranched polyether and copper bromide into a dry reaction test tube, inject tetrahydrofuran into the test tube with a syringe as a medium-grade solvent, and the amount of tetrahydrofuran added is to ensure that the bromine-containing hyperbranched polyether is completely dissolved in it. , and then inject hexamethyltriethylenetetramine dropwise until the solution turns blue, then inject polydiethylamino ethyl methacrylate dropwise; when the temperature of the solution is controlled between 65°C, the reactant Reaction occurs until the viscosity of the solution is 0.18 Pa·s, stop injecting polydiethylamino ethyl methacrylate; after the reaction, further dilute with t...

Embodiment 2

[0029] Synthesis of hyperbranched polymers: choose the hydrophobic bromine-containing hyperbranched polyether with a branching degree of 30% as the macromolecular initiator, choose copper bromide as the catalyst, and choose hexamethyltriethylenetetramine as the polynitrogen ligand; Put the bromine-containing hyperbranched polyether and copper bromide into a dry reaction test tube, inject tetrahydrofuran into the test tube with a syringe as a medium-grade solvent, and the amount of tetrahydrofuran added is to ensure that the bromine-containing hyperbranched polyether is completely dissolved in it. , and then inject hexamethyltriethylenetetramine dropwise until the solution turns blue, then inject polydiethylamino ethyl methacrylate dropwise; when the temperature of the solution is controlled between 70 ° C, the reactant React between them until the viscosity of the solution is 0.20 Pa·s, stop injecting polydiethylamino ethyl methacrylate; after the reaction, further dilute with ...

Embodiment 3

[0034] Synthesis of hyperbranched polymers: choose the hydrophobic bromine-containing hyperbranched polyether with a branching degree of 40% as the macromolecular initiator, choose copper bromide as the catalyst, and choose hexamethyltriethylenetetramine as the polynitrogen ligand; Put the bromine-containing hyperbranched polyether and copper bromide into a dry reaction test tube, inject tetrahydrofuran into the test tube with a syringe as a medium-grade solvent, and the amount of tetrahydrofuran added is to ensure that the bromine-containing hyperbranched polyether is completely dissolved in it. , and then inject hexamethyltriethylenetetramine dropwise until the solution turns blue, then inject polydiethylamino ethyl methacrylate dropwise; when the temperature of the solution is controlled between 75 ° C, the reactant Reaction occurs until the viscosity of the solution is 0.22Pa·s, and the injection of polydiethylamino ethyl methacrylate is stopped; after the reaction is c...

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Abstract

The invention relates to an organic preparation method of a multifunctional nano-material and especially relates to a high-efficiency preparation method of a rare-earth fluoride nanoparticle. The rare-earth fluoride nanoparticle obtained by the high-efficiency preparation method has a core-shell structure and high photoelectric conversion performances and anti-wear performances. The high-efficiency preparation method of the rare-earth fluoride nanoparticles comprises that trivalent rare earth ions are reduced spontaneously by a hyperbranched polymer in a normal-temperature aqueous solution so that the rare-earth fluoride nanoparticle is produced. The rare-earth fluoride nanoparticle has a core-shell structure composed of a nanoparticle and a hyperbranched compound wrapping the nanoparticle. The reaction system is arranged in an ultrasonic field so that reaction time is reduced and a reaction rate is improved.

Description

technical field [0001] The invention relates to an organic preparation method of a multifunctional nanomaterial. The prepared material has a core-shell structure, and has high photoelectric conversion performance and wear reduction performance; Preparation method: In an aqueous solution at room temperature, a hyperbranched polymer spontaneously reduces trivalent rare earth ions to generate rare earth fluoride nanoparticles, and the product has a core-shell structure of "hyperbranched particles wrapping nanoparticles"; the reaction system is placed in an ultrasonic field It can shorten the reaction time and increase the reaction rate. Background technique [0002] Due to the 4f electronic properties of rare earth elements, rare earth elements and their compounds have many special physical, chemical, electronic and optical properties, so they are widely used in the fields of electronics, magnetic materials, energy storage materials, catalysis and tribology; Compared with bulk ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C08G81/02B82Y30/00
Inventor 李桂荣王宏明李月明
Owner JIANGSU UNIV
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