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Method for Improving Rare Earth Ion Doped Inorganic Fluoride Upconversion Luminescence Intensity

A rare earth ion, luminous intensity technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of high cost and complicated operation, and achieve the effects of low cost, reduced defect content, and high efficiency

Active Publication Date: 2018-04-17
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the scope of application of these methods can only be applied to fluoride materials with a certain structure or size, and the operation is complicated and the cost is high

Method used

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  • Method for Improving Rare Earth Ion Doped Inorganic Fluoride Upconversion Luminescence Intensity
  • Method for Improving Rare Earth Ion Doped Inorganic Fluoride Upconversion Luminescence Intensity
  • Method for Improving Rare Earth Ion Doped Inorganic Fluoride Upconversion Luminescence Intensity

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 of the inventive method comprises the following steps:

[0024] (1) Using sodium citrate as rare earth ion complexing agent to hydrothermally synthesize β-NaYF 4 :20mol%Yb 3+ ,2mol%Er 3+ Fluoride powder crystals. Measure 2.6ml of Y(NO 3 ) 3 solution, 2.0ml concentration of 0.1M Yb(NO 3 ) 3 Solution, 0.4ml concentration 0.05M Er(NO 3 ) 3 Solution, 10ml of aqueous solution, 0.5882g of sodium citrate dihydrate were mixed and stirred for 30min. Then add 15 ml of NaF aqueous solution containing 0.5249 g to this solution, and mix and stir for 15 min. Finally, the mixed solution was transferred to a 50ml polytetrafluoroethylene bottle, put into a stainless steel autoclave, sealed, heated to 180°C, and kept warm for 24h. Naturally cooled to room temperature, the synthesized crystals were obtained by centrifugation, with a size of about 2.5 μm and a hexagonal disk shape. Dry it in an oven at 80°C for 12 hours before use. Weigh 0.0902 g of the synthesized...

Embodiment 2

[0029] Embodiment 2 of the inventive method comprises the following steps:

[0030] (1) Select the β-NaYF synthesized in Example 1 for use 4 :20mol%Yb 3+ ,2mol%Er 3+ Fluoride powder crystal is used as the object to be modified, weighing 0.4806g. Select NaF and NH 4 HF 2 As the carrier of alkali metal cations and fluoride ions, weigh NaF0.1105g, NH 4 HF 2 0.2744g.

[0031] (2) Measure 4.0ml of H 2 O, added to the solid mixture, mixed and stirred for 5min.

[0032] (3) The mixed system was transferred to a 25ml polytetrafluoroethylene bottle, put into a stainless steel autoclave, sealed, heated to 200°C, and reacted for 24h.

[0033] (4) After the reaction, cool naturally to room temperature, perform centrifugal washing with water, and dry at 60° C. to obtain a modified rare earth ion-doped inorganic fluoride. The luminescence spectra of the synthesized crystals under 980nm laser excitation before and after the modification reaction are in figure 2 displayed in .

Embodiment 3

[0035] Embodiment 3 of the inventive method comprises the following steps:

[0036] (1) Select the β-NaYF synthesized in Example 1 for use 4 :20mol%Yb 3+ ,2mol%Er 3+ Fluoride powder crystal is used as the object to be modified, weighing 0.1605g. LiF was selected as the alkali metal cation and fluoride ion carrier, weighing 0.1541g.

[0037] (2) Measure 1.6ml of H 2 O, added to the solid mixture, mixed and stirred for 5min.

[0038] (3) The mixed system was transferred to a 25ml polytetrafluoroethylene bottle, put into a stainless steel autoclave, sealed, heated to 220°C, and reacted for 16h.

[0039] (4) After the reaction, cool naturally to room temperature, perform centrifugal washing with water, and dry at 60° C. to obtain a modified rare earth ion-doped inorganic fluoride. The luminescence spectra of the synthesized crystals under 980nm laser excitation before and after the modification reaction are in image 3 displayed in .

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Abstract

The invention discloses a method for improving up-conversion luminescence intensity of rare earth ion doped inorganic fluoride. According to the method, pre-synthesized rare earth doped inorganic fluoride is mixed with a solution containing alkali metal cations and fluoride ions, an obtained mixture is subjected to a sufficient reaction at a high temperature, the alkali metal cations and the fluoride ions added to the solution all participate in material modification, luminescence quenching centers in the inorganic fluoride can be reduced, and the up-conversion luminescence intensity and the quantum efficiency of the rare earth ion doped inorganic fluoride can be improved greatly.

Description

technical field [0001] The invention relates to an up-conversion luminescent material, in particular to a method for increasing the up-conversion luminous intensity of a rare earth ion-doped inorganic fluoride. Background technique [0002] Rare earth ion-doped inorganic fluoride is one of the most efficient rare earth-doped up-conversion luminescent material hosts, which can achieve high-efficiency emission in the visible band under near-infrared light excitation. Inorganic fluoride. Rare earth-doped inorganic fluorides have important applications in the fields of bioimaging and medicine, solar cells, visible displays, optical storage and encryption, and short-wave laser materials. For example: Rare earth-doped inorganic fluoride can be simultaneously excited and detected in the biological light-transmitting window band (700-1100nm), which is a new type of high signal-to-noise ratio, large detection depth, good stability, and non-toxic biological probes , The application ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85
CPCC09K11/7773
Inventor 范少华胡丽丽孙洪涛王世凯王朋
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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