Method for preparing three-primary-color up-conversion luminescent material with orthogonal excitation-emission response

A technology of luminescent materials and three primary colors, applied in the direction of luminescent materials, nanotechnology for materials and surface science, chemical instruments and methods, etc., can solve the problems of not preparing three primary colors up-conversion luminescent materials, harmful energy transfer, light excitation Crosstalk and other issues

Active Publication Date: 2020-10-23
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in lanthanide-doped single-core nanocrystals and core-shell nanomaterials with common structures, the co-doping of multiple luminescent ions will cause photoexcitation crosstalk, harmful energy migration and cross-relaxation between energy levels, and fluorescence reactivation. Absorption, fluorescence quenching between different ions, etc., making it difficult for UCNPs with simple structures to achieve controllable three-color luminescence
For example, due to the above reasons, in the true three-dimensional color display technology based on up-conversion luminescence, researchers have not solved the problems of excitation light crosstalk, harmful energy transfer and fluorescence reabsorption for many years, so they have not prepared Three-wavelength near-infrared light excitation-orthogonal response three-primary-color upconversion luminescent material

Method used

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  • Method for preparing three-primary-color up-conversion luminescent material with orthogonal excitation-emission response
  • Method for preparing three-primary-color up-conversion luminescent material with orthogonal excitation-emission response
  • Method for preparing three-primary-color up-conversion luminescent material with orthogonal excitation-emission response

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1: NaYF 4 : Preparation of Yb / Tm (30 / 0.5mol%) core nanocrystals.

[0054] NaYF was first prepared by using a fully automatic nanomaterial synthesizer 4 : Yb / Tm (30 / 0.5mol%) core nanocrystals.

[0055] Specific preparation process: Y(CH 3 COO) 3 (0.278mmol), Yb(CH 3 COO) 3 (0.120mmol) and Tm(CH 3 COO) 3 (0.002mmol) aqueous solution was added to a mixed solvent of 3mL oleic acid and 7mL octadecene at room temperature, stirred and heated to 150°C and reacted for 60 minutes to form the oleic acid complex Y, Yb, Tm-OA core precursor. After the resulting mixed solution was naturally cooled to room temperature, 4 mL of NH 4 F (0.4moL / L) and 2mL NaOH (0.5moL / L) in methanol solution, heated to 50°C and stirred continuously for 30 minutes, then stirred and heated to 100°C, reacted under vacuum for 10 minutes to remove methanol, and finally in an argon atmosphere Lower the temperature to 290°C for 90 minutes. After the reaction was completed, it was cooled to roo...

Embodiment 2

[0056] Example 2: NaYF 4 :Yb / Tm@NaYF 4 Preparation of core-shell nanocrystals.

[0057] The core prepared in Example 1 was used as a seed crystal, and added to the reaction system of the Y-OA shell precursor to induce epitaxial growth of NaYF 4 Shell.

[0058] The specific preparation process is to Y(CH 3 COO) 3 (0.4mmol) aqueous solution is added in the mixed solvent of 3mL oleic acid and 7mL octadecene, the gained mixture is stirred and heated to 150 ℃ and reacted for 60 minutes to form the oleic acid complex Y-OA shell layer precursor, treat that the mixed solution of gained is naturally cooled to After room temperature, the cyclohexane solution (~0.4 mmol) of the core nanocrystals prepared above and 4 mL of NH 4 F (0.4moL / L) and 2mL NaOH (0.5moL / L) methanol solution, continue to stir for 30 minutes under the reaction conditions of 50 ℃, then stir and heat to 100 ℃ for 20 minutes under vacuum to remove cyclohexane and Methanol, finally heated up to 290°C for 90 minute...

Embodiment 3

[0059] Example 3: NaYF 4 :Yb / Tm@NaYF 4 @NaYF 4 : Preparation of Er / Ho (5 / 5mol%) bilayer core-shell structure nanocrystals.

[0060] A fully automatic nanomaterial synthesizer was used to prepare double-layer core-shell structure nanocrystals by layer-by-layer wrapping.

[0061] The specific preparation process is that the preparation of the double-layer core-shell structure nanocrystal is similar to the above-mentioned preparation method of the core-shell structure nanocrystal. It is only necessary to replace the Y-OA shell precursor prepared above with the Y, Er, Ho-OA shell precursor, and use the core-shell structure nanocrystal prepared in Example 2 as a seed crystal to induce epitaxial growth of NaYF 4 : Er / Ho shell. The prepared product was dispersed into cyclohexane for characterization and preparation of three-layer core-shell structure nanocrystals in the next step.

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Abstract

The invention provides a method for preparing a three-primary-color up-conversion luminescent material with orthogonal excitation-emission response, and belongs to the technical field of true three-dimensional color display, up-conversion luminescence and nano core-shell material preparation crossing. Specifically, a one-core five-shell structure nanocrystal is prepared through firstly preparing ablue light-emitting core through a full-automatic nano synthesizer, and sequentially inducing epitaxial growth of a first inert isolation layer, a second red light-emitting layer, a third inert isolation layer, a fourth green light-emitting layer and a fifth 808nm exciting light energy absorption layer by using a layer-by-layer wrapping method. Under the excitation of near-infrared light with three different wavelengths of 1560 nm, 808 nm or 980 nm, the five-shell core-shell structure nanocrystal can respond to orthogonal up-conversion luminescence of three primary colors of red, green and blue. The method provides technical support for panchromatic luminescence adjustment, multi-color display, multi-color coding, anti-counterfeiting and the like.

Description

technical field [0001] The invention belongs to the interdisciplinary technical fields of true three-dimensional color display, up-conversion luminescence and preparation of nano-core-shell materials, and in particular relates to a method for preparing an orthogonal excitation-emission response three-primary-color up-conversion luminescent material. Background technique [0002] The core of the true three-dimensional display technology based on up-conversion luminescence is an up-conversion luminescent material with three primary colors of red, green and blue with orthogonal excitation-response. This technology requires that in the displayed three-dimensional space, each point has the performance of vertical excitation and orthogonal emission. That is to say, when excited with one kind of near-infrared light, red, green or blue fluorescence can be obtained; when excited with two different near-infrared lights, two colors of red, green and blue fluorescence can be obtained; ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/85B82Y20/00B82Y30/00B82Y40/00
CPCC09K11/02C09K11/7773B82Y20/00B82Y30/00B82Y40/00
Inventor 秦伟平贾恒董妍惠张丹秦冠仕赵丹尹升燕狄卫华贾志旭
Owner JILIN UNIV
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