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A preparation method of rare earth-doped yttrium potassium fluoride upconversion luminescent nanomaterial

A yttrium-potassium fluoride, rare earth doping technology, applied in the directions of luminescent materials, chemical instruments and methods, can solve the problems of high pollution, high energy consumption, low yield and the like, achieve enhanced luminescence performance, overcome the preparation process, and reduce production costs Effect

Inactive Publication Date: 2016-01-06
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation methods for the synthesis of rare earth-doped upconversion nanomaterials mainly include co-precipitation, hydrothermal / solvothermal and thermal decomposition methods, etc., and the co-precipitation method generally requires subsequent high-temperature heat treatment above 600 °C, which is energy-intensive and easy to produce. A large number of nanocrystals are agglomerated; the materials synthesized by the hydrothermal method in one step are difficult to reach the nanometer level, which limits their further application in bio-nano imaging; the precursor solvents and by-products used in the thermal decomposition method are highly toxic
Facing the research status quo of high energy consumption, low yield, and high pollution in many preparation processes, the development of a green and low-cost preparation method is still a key issue in the synthesis of ultrafine, high-quality, high-fluorescence up-conversion luminescent materials. where the
[0005] In summary, there is no report on the relevant patent application for the synthesis of ultra-fine, high-quality, and high-fluorescence yttrium-potassium fluoride-based upconversion luminescent materials by a green, environmentally friendly, and low-cost preparation method.

Method used

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  • A preparation method of rare earth-doped yttrium potassium fluoride upconversion luminescent nanomaterial
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Embodiment 1

[0035] A method for preparing yttrium potassium fluoride up-conversion luminescent nanomaterials by thermal injection, the specific steps are as follows:

[0036] 1) Weigh 0.4mol of yttrium oxide (Y 2 o 3 ) and 4mol of potassium bifluoride (KHF 2 ) into a 50ml three-necked flask containing oleic acid / oleylamine solvent system, the reaction was carried out under a closed system, and after a period of vacuuming at normal temperature, the vacuum valve was closed, and then argon gas was passed into the reactor, and the reaction was carried out at 20°C / The temperature was raised to 160° C. at a heating rate of 1 min, and kept at a stirring rate of 1000 rpm / min for 30 minutes. Wherein the volume ratio of oleic acid / oleylamine is 2:1, and the amount of total solvent is 15ml;

[0037] 2) Weigh 0.2mol of ytterbium fluoride (YbF 3 ) and 0.02mol of erbium fluoride (ErF 3 ) into a 50ml three-necked flask containing oleic acid / oleylamine solvent system, the reaction was carried out u...

Embodiment 2

[0042] A method for preparing yttrium potassium fluoride up-conversion luminescent nanomaterials by thermal injection, the specific steps are as follows:

[0043] 1) Weigh 0.4mol of yttrium oxide (Y 2 o 3 ), 4mol of potassium acetate (C 2 h 3 KO 2 ) and 4mol of ammonium bifluoride (NH 4 .HF 2 ) into a 50ml three-necked flask containing oleic acid / oleylamine solvent system, the reaction was carried out under a closed system, and after a period of vacuuming at normal temperature, the vacuum valve was closed, and then argon gas was passed into the reactor, and the reaction was carried out at 20°C / The temperature was raised to 160° C. at a heating rate of 1 min, and kept at a stirring rate of 1000 rpm / min for 30 minutes. Wherein the volume ratio of oleic acid / oleylamine is 2:1, and the amount of total solvent is 15ml;

[0044] 2) Weigh 0.2mol of ytterbium fluoride (YbF 3 ) and 0.02mol of erbium fluoride (ErF 3 ) into a 50ml three-necked flask containing oleic acid / oleyla...

Embodiment 3

[0049] A method for preparing yttrium potassium fluoride up-conversion luminescent nanomaterials by thermal injection, the specific steps are as follows:

[0050] 1) Weigh 0.4mol of yttrium oxide (Y 2 o 3 ), 4mol of potassium hydrogen fluoride (KHF 2 ) into a 50ml three-necked flask containing oleic acid / oleylamine solvent system, the reaction is carried out under a closed system, and after vacuuming for a period of time at normal temperature, the vacuum valve is closed, and then argon gas is passed into the reactor, with 10 to 20 Temperature rise rate of °C / min Raise the temperature to 160 °C and keep the temperature for 30 minutes at a stirring rate of 1000 rpm / min. Wherein the volume ratio of oleic acid / oleylamine is 2:1, and the amount of total solvent is 15ml;

[0051] 2) Weigh 0.4mol of ytterbium fluoride (YbF 3 ) and 0.04mol of erbium fluoride (ErF 3 ) into a 50ml three-necked flask containing oleic acid / oleylamine solvent system, the reaction was carried out under...

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Abstract

The invention relates to a method for preparing a rare-earth doped potassium yttrium fluoride up-conversion luminescence nano material. The method comprises the following steps: 1) weighing yttrium oxide, sylvite and a fluorine source, adding in an oleic acid / oleylamine-containing solvent system, stirring and mixing, thus obtaining a first uniform solution; 2) weighing ytterbium fluoride and a rare-earth activator, adding in the oleic acid / oleylamine-containing solvent system, stirring and mixing, thus obtaining a second uniform solution; 3) rapidly heating the first uniform solution to a high temperature, and meanwhile rapidly filling the second uniform solution, and sufficiently stirring to react, thus obtaining a third uniform solution; and 4) cooling the obtained solution to room temperature, performing centrifugal separation, washing, and drying, thus obtaining the rare-earth doped potassium yttrium fluoride up-conversion luminescence nano material. The method has the beneficial effects that the preparation period of the material is effectively shortened, new ideas and ways are provided for preparing the up-conversion luminescence nano material, large-scale popularization and application are facilitated, and the purposes of controllable the monodisperse particle size, high quantum yield and the like are solved.

Description

technical field [0001] The invention relates to the technical field of up-conversion luminescent materials, in particular to a preparation method of rare-earth-doped yttrium potassium fluoride up-conversion luminescent nanomaterials. Background technique [0002] Rare-earth up-conversion luminescent materials are a kind of fluorescent materials that can emit light shorter than the excitation wavelength when excited by light. It has shown broad research and application value, especially its remarkable characteristics such as large light penetration depth (0.3-7 μm), no autofluorescence of biological tissue, and almost no damage to biological tissue, so it is expected to replace traditional bioluminescence labeling materials , has broad application prospects in biomedical fields such as bioimaging, detection, drug loading, and instant diagnostic device development. [0003] Compared with traditional luminescent materials, up-conversion luminescent materials have the following...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85
Inventor 王友法周斌夏冬林熊真敏刘星李乾柯明鑫
Owner WUHAN UNIV OF TECH
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