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Potassium lutetium fluoride nanocrystal with delayed phase transition and greatly increased up-conversion luminescence intensity and preparation method thereof

A technology of potassium lutetium fluoride and luminous intensity, applied in the field of luminescent materials, can solve problems such as low luminous efficiency, reduced conversion luminescence, and phase transition

Active Publication Date: 2021-03-26
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, high-concentration ion doping can cause phase transitions that are not conducive to luminescent properties, such as β-NaYF 4 Highly doped La in the system 3+ Will cause a phase transition from hexagonal to cubic; KYb 2 f 7 Incorporation of Gd into nanocrystals 3+ It also causes a phase transition from orthorhombic to cubic. Since the luminous efficiency of the cubic system is much lower than that of the orthorhombic system in general, the upconversion luminescence of these systems is also greatly reduced when the phase transition occurs. Small
[0004] It can be seen that it is of far-reaching significance to realize the phase transition delay and improve the up-conversion luminescence under high doping concentration. This method not only realizes the simultaneous regulation of phase transition and up-conversion luminescence, but also can be extended to other up-conversion rare earth-based luminescent host systems. , so far there is no report on achieving delayed phase transition and improving upconversion luminescence in potassium lutetium fluoride nanocrystals

Method used

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  • Potassium lutetium fluoride nanocrystal with delayed phase transition and greatly increased up-conversion luminescence intensity and preparation method thereof
  • Potassium lutetium fluoride nanocrystal with delayed phase transition and greatly increased up-conversion luminescence intensity and preparation method thereof
  • Potassium lutetium fluoride nanocrystal with delayed phase transition and greatly increased up-conversion luminescence intensity and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Prepare rare earth ion highly doped lutetium potassium fluoride nanocrystals by a water-based hydrothermal method. The specific steps are as follows:

[0046] (1) (0.8ml / 0.72ml / 0.64ml / 0.56ml / 0.48ml / 0.32ml / 0.16ml / 0ml) 1M lutetium nitrate solution, 0.36ml 0.5M ytterbium nitrate solution, 0.2ml 0.1M erbium nitrate solution , and (0ml / 0.08ml / 0.16ml / 0.24ml / 0.32ml / 0.48ml / 0.64ml / 0.8ml) 1M nitrate (Y 3+ / Gd 3+ ) solution was added to 10 ml of deionized water, and after magnetic stirring for 10 minutes, 3.75 ml of 0.4M dipotassium EDTA solution was added, and a white cloudy liquid was formed after 10 minutes under magnetic stirring, and finally 2.4 ml of 5M fluorine was added. Potassium chloride solution was added, and deionized water was added so that the total volume of all solutions was 30 ml, and a transparent colloid was formed after 30 minutes of magnetic stirring.

[0047] (2) Transfer the colloid to a stainless steel reactor with a liner for hydrothermal reaction. T...

Embodiment 2

[0052] 1. Prepare rare earth ion highly doped lutetium potassium fluoride nanocrystals by oil-based hydrothermal method. The specific steps are as follows:

[0053] (1) First, 2 ml of oleic acid, 10 ml of absolute ethanol and 4 mmol of potassium hydroxide were mixed and stirred for 10 minutes to form clear solution A. Add (0.8ml / 0.72ml / 0.64ml / 0.56ml / 0.48ml / 0.32ml / 0.16ml / 0ml) 1M lutetium nitrate solution, 0.36ml 0.5M ytterbium nitrate solution, 0.2ml 0.1M erbium nitrate solution, and ( 0ml / 0.08ml / 0.16ml / 0.24ml / 0.32ml / 0.48ml / 0.64ml / 0.8ml) 1M gadolinium nitrate solution was added to 12ml deionized water and stirred magnetically for 10 minutes to form solution B. Then solution A and solution B were mixed, and a white cloudy solution was formed after 10 minutes under magnetic stirring. Finally, 2.4 ml of 5M potassium fluoride solution was added, and deionized water was added so that the total volume of all solutions was 30 ml. A transparent colloid formed after 30 minutes of magne...

Embodiment 3

[0059] 1. Use oil-based hydrothermal method to prepare rare earth ion highly doped lutetium potassium fluoride nanocrystals at high temperature. The specific steps are as follows:

[0060] (1) First, 2 ml of oleic acid, 10 ml of absolute ethanol and 4 mmol of potassium hydroxide were mixed and stirred for 10 minutes to form clear solution A. Add (0.8ml / 0.72ml / 0.64ml / 0.56ml / 0.48ml / 0.32ml / 0.16ml / 0ml) 1M lutetium nitrate solution, 0.36ml 0.5M ytterbium nitrate solution, 0.2ml 0.1M erbium nitrate solution, and ( 0ml / 0.08ml / 0.16ml / 0.24ml / 0.32ml / 0.48ml / 0.64ml / 0.8ml) 1M gadolinium nitrate solution was added to 12ml deionized water and stirred magnetically for 10 minutes to form solution B. Then solution A and solution B were mixed, and a white cloudy solution was formed after 10 minutes under magnetic stirring. Finally, 2.4 ml of 5M potassium fluoride solution was added, and deionized water was added so that the total volume of all solutions was 30 ml. A transparent colloid formed a...

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Abstract

The invention discloses a lutetium potassium fluoride nanocrystal with phase change delay and greatly improved up-conversion luminescence intensity. The chemical formula of the lutetium potassium fluoride nanocrystal is K(Lu<x>Y<1-x>)<2>F<7>:18%Yb<3+>,2%Er<3+> or K(Lu<x>Gd<1-x>)<2>F<7>:18%Yb<3+>,2%Er<3+>, wherein x=10-40 mmol%; a preparation method of the lutetium potassium fluoride nanocrystal comprises the steps of: S1, mixing lutetium nitrate, ytterbium nitrate, erbium nitrate and yttrium nitrate or a yttrium nitrate solution with deionized water, performing stirring, adding a chelating agent, performing stirring to form white turbid liquid, then adding a potassium fluoride solution, and performing stirring to form transparent colloid; S2, performing a hydrothermal reaction on the colloid at 180-260 DEG C for 10-15 hours; and S3, performing centrifugation on the turbid liquid obtained after the reaction is conducted, and performing washing and drying to obtain the lutetium potassiumfluoride nanocrystal doped with yttrium ions or high content of yttrium. The lutetium potassium fluoride nanocrystal has broad application prospects in fields of multicolor display, biomedicine, photocatalysis, solar energy and the like, and the preparation method has simple equipment and easy operation, and is suitable for large-scale production and promotion.

Description

technical field [0001] The invention belongs to the field of luminescent materials, and more particularly relates to a potassium lutetium fluoride nanocrystal with delayed phase transition and greatly improved up-conversion luminescence intensity and a preparation method thereof. Background technique [0002] Rare earth-based upconversion luminescent nanocrystals have attracted much attention due to their unique properties that convert low-energy photons into high-energy photons, extending their potential applications in multicolor imaging, biomarkers, photocatalysis, and solar energy. . And the optimization of luminescence performance, one of the important means is the choice of doping host. Currently, β-NaYF 4 It is recognized as the host material with the most efficient upconversion luminescence properties. In recent years, other rare earth fluorides, such as Gd-based and Lu-based fluorides, have also been extensively studied. Recently, the orthorhombic KYb 2 F 7 Na...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85B82Y20/00B82Y30/00B82Y40/00
CPCB82Y20/00B82Y30/00B82Y40/00C09K11/7773
Inventor 徐德康张曰理姚露林浩阳生红
Owner SUN YAT SEN UNIV
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