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Luminous color variable upconversion nanometer luminescent material as well as preparation method and application thereof

A nano-luminescent material and luminescent color technology, applied in luminescent materials, color-changing fluorescent materials, chemical instruments and methods, etc., can solve the problems of damaged nanoparticles, cumbersome, impure luminescent color, etc., and achieve the effect that is difficult to imitate

Inactive Publication Date: 2017-08-01
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At different temperatures, this material can achieve the purpose of identifying authenticity by upconverting the change of luminescent color; however, the material luminescence is accompanied by a large number of non-radiative transitions, and the released heat will damage local nanoparticles. Affects luminous efficiency, and it is difficult to mix evenly, which will lead to impure luminous color
In addition, the current measurement method is only limited to the change of luminous color caused by temperature, which requires heat conduction to the material itself, which has limitations.
In terms of preparation methods, the zero-dimensional and one-dimensional nanocrystals in this composite up-conversion material need to be prepared separately, which is cumbersome.

Method used

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  • Luminous color variable upconversion nanometer luminescent material as well as preparation method and application thereof
  • Luminous color variable upconversion nanometer luminescent material as well as preparation method and application thereof
  • Luminous color variable upconversion nanometer luminescent material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of core-shell NaGd by pyrolysis 0.79 f 4 :Yb 0.2 ,Tm 0.01 @NaGd 0.79 f 4 :Yb 0.2 ,Ho 0.01 Up-conversion nano-luminescent particles, the process is as follows:

[0035] 1mmol rare earth acetate salt Ln(CH 3 COO) 3 (Ln=Gd 3+ ,Yb 3+ ,Tm 3+ (molar ratio Gd 3+ :Yb 3+ :Tm 3+ =79:20:1)) dissolved in a mixed solution of 10mL oleic acid and 15mL 1-octadecene, heated to 110°C and stirred for 30min to form a transparent and uniform solution; after the above mixed solution was cooled to 50°C, NH 4 The methanol solution of F and the methanol solution of NaOH were stirred for about 30 minutes, the methanol in the solution was removed, the temperature of the solution was raised to 290°C and reacted for 90 minutes, and after cooling to room temperature, centrifugal cleaning was performed to obtain the nuclear structure NaGd 0.79 f 4 :Yb 0.2 ,Tm 0.01 Upconverting nanoparticles. Among them, NH 4 F. The molar ratios of NaOH to rare earth acetate are 4:1 and...

Embodiment 2

[0042] Preparation of core-shell NaGd by pyrolysis 0.79 f 4 :Yb 0.2 ,Ho 0.01 @NaGd 0.79 f 4 :Yb 0.2 ,Tm 0.01 Up-conversion nano-luminescent particles, the process is as follows:

[0043] 1mmol rare earth acetate salt Ln(CH 3 COO) 3 (Ln=Gd 3+ ,Yb 3+ ,Ho 3+ (molar ratio Gd 3+ :Yb 3+ :Ho 3+ =79:20:1)) dissolved in a mixed solution of 10mL oleic acid and 15mL 1-octadecene, heated to 110°C and stirred for 30min to form a transparent and uniform solution; after the above mixed solution was cooled to 50°C, NH 4 The methanol solution of F and the methanol solution of NaOH were stirred for about 30 minutes, the methanol in the solution was removed, the temperature of the solution was raised to 290°C and reacted for 90 minutes, and after cooling to room temperature, centrifugal cleaning was performed to obtain the nuclear structure NaGd 0.79 f 4 :Yb 0.2 ,Ho 0.01 Upconverting nanoparticles. Among them, NH 4 F. The molar ratios of NaOH to rare earth acetate are 4:1 and...

Embodiment 3

[0047] Preparation of core-shell NaGd by pyrolysis0.64 Ce 0.15 f 4 :Yb 0.2 ,Ho 0.01 @NaGd 0.79 f 4 :Yb 0.2 ,Tm 0.01 Up-conversion nano-luminescent particles, the process is as follows:

[0048] 1mmol rare earth acetate salt Ln(CH 3 COO) 3 (Ln=Gd 3+ , Ce 3+ ,Yb 3+ ,Ho 3+ (molar ratio Gd 3+ : Ce 3+ :Yb 3 + :Ho 3+ =64:15:20:1)) Dissolve in a mixed solution of 10mL oleic acid and 15mL 1-octadecene, heat to 110°C and stir for 30min to form a transparent and uniform solution; when the above mixed solution is cooled to 50°C, add NH 4 The methanol solution of F and the methanol solution of NaOH were stirred for about 30 minutes, the methanol in the solution was removed, the temperature of the solution was raised to 290°C and reacted for 90 minutes, and after cooling to room temperature, centrifugal cleaning was performed to obtain the nuclear structure NaGd 0.64 Ce 0.15 f 4 :Yb 0.2 ,Ho 0.01 Upconverting nanoparticles. Among them, NH 4 F. The molar ratios of Na...

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Abstract

The invention discloses a luminous color variable upconversion nanometer luminescent material, which has a chemical expression of NaR0.8-x-yF4: Yb0.2, Hox, Tmy; in the chemical expression, R is at least one of Y, Gd and Ce, x is more than or equal to 0.0001 and less than or equal to 0.1, and y is more than or equal to 0.0005 and less than or equal to 0.1; the diameters of upconversion nanoparticles are 5-25nm. The material can be divided into two types according to the distribution mode of an activating agent: a single-core structure and a core-shell structure, wherein in the single-core structure, Tm and Ho are evenly distributed in nanoparticles, and in the core-shell structure, Tm and Ho are respectively distributed in a core and a shell. The invention also discloses a preparation method of the upconversion nanometer luminescent material. By using the surface effect of the upconversion nanometer luminescent material, the upconversion luminescence color of the material can change obviously along with the change of laser power density, temperature and radiation time under the condition of 980nm near infrared excitation, so that the material can be applied to the anti-counterfeit field.

Description

technical field [0001] The invention belongs to the technical field of up-conversion luminescent materials, and in particular relates to an up-conversion nano-luminescent material with variable luminous color, a preparation method and an application. Background technique [0002] Up-conversion luminescent materials can emit higher-energy visible light by absorbing lower-energy infrared light, and have broad application prospects in the fields of solid-state lasers, stereoscopic displays, biomedicine, and anti-counterfeiting. Up-conversion luminescent materials generally require activators (such as Tm 3+ and Ho 3+ ) and sensitizers (such as rare earth ions Yb 3+ ) directly involved, while matrix materials (such as NaYF 4 and NaGdF 4 ) indirectly plays an important role in the improvement of luminous efficiency. For example, in NaYF 4 :Yb,Ho,Tm, activator Tm 3+ and Ho 3+ from the adjacent sensitizer Yb 3+ It continuously receives 980nm infrared photons and emits three...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/02C09K9/00
CPCC09K11/7773C09K9/00C09K11/025
Inventor 邵起越欧阳立来张功托曽宇乔董岩蒋建清
Owner SOUTHEAST UNIV
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