Method for improving up-conversion luminescence intensity of rare earth ion doped inorganic fluoride

A rare earth ion, luminous intensity technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of complex operation and high cost, and achieve the effect of reducing defect content, low cost, and wide applicability

Active Publication Date: 2016-08-24
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 up-conversion luminescence intensity of rare earth ion doped inorganic fluoride
  • Method for improving up-conversion luminescence intensity of rare earth ion doped inorganic fluoride
  • Method for improving up-conversion luminescence intensity of rare earth ion doped inorganic fluoride

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Embodiment 1

[0023] Embodiment 1 of the method of the present invention includes the following steps:

[0024] (1) Hydrothermal synthesis of β-NaYF using sodium citrate as rare earth ion complexing agent 4 : 20mol% Yb 3+ ,2mol% Er 3+ Fluoride powder crystals. Measure 2.6ml Y(NO 3 ) 3 Solution, 2.0ml Yb(NO 3 ) 3 Solution, 0.4ml of Er(NO 3 ) 3 The solution, 10ml of aqueous solution, 0.5882g of sodium citrate dihydrate were mixed and stirred for 30min. Then 15ml of NaF aqueous solution containing 0.5249g was added to this solution, mixed and stirred for 15min. Finally, the mixed solution was transferred to a 50ml polytetrafluoroethylene bottle, put into a stainless steel autoclave, sealed, heated to 180°C, and kept for 24h. It is naturally cooled to room temperature, and the synthesized crystal is obtained by centrifugation, the size is about 2.5 μm, and it has a hexagonal disk shape. Dry in a drying oven at 80°C for 12 hours, set aside. Weigh 0.0902g of the synthesized rare earth doped fluor...

Embodiment 2

[0029] Embodiment 2 of the method of the present invention includes the following steps:

[0030] (1) Select the β-NaYF synthesized in Example 1 4 : 20mol% Yb 3+ ,2mol% Er 3+ The fluoride powder crystal was used as the modified object, weighing 0.4806 g. Select NaF and NH 4 HF 2 As a carrier of alkali metal cations and fluoride ions, weighing 0.1105g of NaF, NH 4 HF 2 0.2744g.

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

[0032] (3) Transfer the mixed system to a 25ml polytetrafluoroethylene bottle, put it into a stainless steel autoclave, seal, heat to 200°C, and react for 24 hours.

[0033] (4) After the reaction is completed, it is naturally cooled to room temperature, washed with water by centrifugation, and dried at 60° C. to obtain modified rare earth ion-doped inorganic fluoride. The luminescence spectrum of the synthesized crystal under 980nm laser excitation before and after the modification reaction is shown in figure 2 Sh...

Embodiment 3

[0035] Embodiment 3 of the method of the present invention includes the following steps:

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

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

[0038] (3) Transfer the mixed system to a 25ml polytetrafluoroethylene bottle, put it into a stainless steel autoclave, seal, heat to 220°C, and react for 16h.

[0039] (4) After the reaction is completed, it is naturally cooled to room temperature, washed with water by centrifugation, and dried at 60° C. to obtain modified rare earth ion-doped inorganic fluoride. The luminescence spectrum of the synthesized crystal under 980nm laser excitation before and after the modification reaction is shown in image 3 Show 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 improving the up-conversion luminescence intensity of rare earth ion doped inorganic fluoride. Background technique [0002] Rare earth ion-doped inorganic fluoride is currently one of the most efficient rare earth-doped up-conversion luminescent material substrates, which can achieve high-efficiency emission in the visible wavelength range under near-infrared light excitation, hereinafter referred to as rare-earth ion-doped with up-conversion luminescence Inorganic fluoride. Rare earth-doped inorganic fluorides have important applications in bioimaging and medicine, solar cells, visible displays, optical storage and encryption, shortwave laser materials and other fields. For example: rare earth-doped inorganic fluoride can achieve excitation and detection at the same time in the biological light-transmitting window band (700-1100nm). It is a new type of high sign...

Claims

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Application Information

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Patent Type & Authority Applications(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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