Rare-earth-doped cesium zirconium fluoride-based up-conversion luminescent nano material and preparation method thereof

A technology of rare earth doping and nanomaterials, applied in the direction of luminescent materials, chemical instruments and methods, etc., to achieve the effect of good repeatability, good dispersion, and easy control of synthesis conditions

Pending Publication Date: 2021-10-08
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the research on rare earth-doped fluoride luminescent host materials mainly focuses on sodium yttrium fluoride (NaYF 4 ), sodium gadolinium fluoride (NaGdF 4 ) or lithium yttrium fluoride (LiYF 4 ) and other alkali metal rare earth fluoride systems, there are still few reports on alkali metal transition metal fluoride systems, especially the research on alkali metal transition metal fluoride systems based on transition metal zirconium

Method used

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  • Rare-earth-doped cesium zirconium fluoride-based up-conversion luminescent nano material and preparation method thereof
  • Rare-earth-doped cesium zirconium fluoride-based up-conversion luminescent nano material and preparation method thereof
  • Rare-earth-doped cesium zirconium fluoride-based up-conversion luminescent nano material and preparation method thereof

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Experimental program
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Embodiment 1

[0025] A preparation of Cs 2 ZrF 6 :20mol%Yb 3+ ,2mol%Er 3+ A method for preparing an upconversion luminescent nanomaterial, comprising the following steps:

[0026] Weigh 0.3804g of zirconium acetylacetonate, 0.007g of erbium acetate and 0.0845g of ytterbium acetate into a 100mL three-neck flask at room temperature, add 8mL of oleic acid and 12mL of octadecene, and stir to make them evenly mixed. Under the protection of nitrogen flow, the above mixture was heated to 150°C and kept at this temperature for 60 minutes to completely dissolve the zirconium acetylacetonate and rare earth acetate to obtain a transparent clear solution. After cooling to room temperature, 15 mL of a methanol solution in which 0.4887 g of cesium carbonate and 0.2223 g of ammonium fluoride were dissolved was added dropwise, stirred and allowed to react at room temperature for 30 minutes. Then the mixed solution was heated to 50° C. and kept for 30 minutes to remove methanol in the reaction system. ...

Embodiment 2

[0031] a Cs 2 ZrF 6 :20mol%Yb 3+ ,2mol%Tm 3+ A method for preparing an upconversion luminescent nanomaterial, comprising the following steps:

[0032] Weigh 0.3804g of zirconium acetylacetonate, 0.0072g of thulium acetate and 0.0845g of ytterbium acetate into a 100mL three-neck flask at room temperature, add 8mL of oleic acid and 12mL of octadecene, and stir to mix evenly. Under the protection of nitrogen flow, the above mixture was heated to 150°C and kept at this temperature for 60 minutes to completely dissolve the zirconium acetylacetonate and rare earth acetate to obtain a transparent clear solution. After cooling to room temperature, 15 mL of a methanol solution in which 0.4887 g of cesium carbonate and 0.2223 g of ammonium fluoride were dissolved was added dropwise, stirred and allowed to react at room temperature for 30 minutes. Then the mixed solution was heated to 50° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was re...

Embodiment 3

[0034] a Cs 2 ZrF 6 :20mol%Yb 3+ ,2mol%Ho 3+ A method for preparing an upconversion luminescent nanomaterial, comprising the following steps:

[0035] Weigh 0.3804g of zirconium acetylacetonate, 0.0068g of holmium acetate and 0.0845g of ytterbium acetate into a 100mL three-neck flask at room temperature, add 8mL of oleic acid and 12mL of octadecene, and stir to mix evenly. Under the protection of nitrogen flow, the above mixture was heated to 150°C and kept at this temperature for 60 minutes to completely dissolve the zirconium acetylacetonate and rare earth acetate to obtain a transparent clear solution. After cooling to room temperature, 15 mL of a methanol solution in which 0.4887 g of cesium carbonate and 0.2223 g of ammonium fluoride were dissolved was added dropwise, stirred and allowed to react at room temperature for 30 minutes. Then the mixed solution was heated to 50° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was remo...

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Abstract

The invention discloses a rare earth doped cesium zirconium fluoride-based up-conversion luminescent nano material and a preparation method thereof. The rare-earth-doped cesium zirconium fluoride-based up-conversion luminescent nano material is a hexagonal-phase Cs2ZrF6 nano material with a particle size of 5-10 nm. According to the invention, zirconium acetylacetonate is adopted as a metal salt of Zr, a high-temperature coprecipitation method is utilized to synthesize the rare-earth-doped cesium zirconium fluoride-based up-conversion luminescent nano material, the synthesis conditions are easy to control, the repeatability is good, and the prepared luminescent nano material has good dispersibility, uniformity and luminescent property, can be used as an ideal matrix material for up-conversion luminescence, and has a wide application prospect in the fields of luminescence imaging, biological application and the like.

Description

technical field [0001] The invention relates to a rare earth-doped zirconium cesium fluoride-based up-conversion luminescent nanometer material and a preparation method thereof, belonging to the technical field of luminescent materials. Background technique [0002] Rare-earth-doped upconversion luminescent nanomaterials have the advantages of weak background interference, long fluorescence lifetime, low excitation energy and deep tissue penetration, so they show broad application prospects in the fields of lighting display, drug delivery, biomedical imaging, and biomarkers. It is a research hotspot at home and abroad in recent years. Rare-earth-doped nano-luminescent materials are composed of host materials and rare-earth dopant ions, and the host has a very important influence on the up-conversion luminescent properties of the material. Among the many host materials studied, fluoride has stable physical and chemical properties and low phonon energy, and is a good luminesc...

Claims

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Application Information

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IPC IPC(8): C09K11/67
CPCC09K11/7773
Inventor 刘敏付虎辉胡长河张焱森
Owner SHANGHAI INSTITUTE OF TECHNOLOGY
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