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A single-doped-enriched core-shell structure up-conversion luminescent material and its preparation method

A technology of core-shell structure and luminescent materials, which is applied in the direction of luminescent materials, chemical instruments and methods, nanotechnology, etc., can solve the problems of no significant improvement, difficulty in meeting the harsh requirements of industrial production, instruments and equipment, etc., and achieve high-efficiency luminescence Effect

Active Publication Date: 2020-05-19
HUAZHONG UNIV OF SCI & TECH
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Problems solved by technology

In 2013, J.B. Zhao et al. used high power (~2.5×10 6 W / cm 2 ) excitation to achieve high-concentration doping and high-efficiency luminescence of luminescent center ions (Naturenanotech., 2013, 8, 729-734), however, such high radiation has strict requirements on instruments and equipment, and it is difficult to meet the needs of industrial production; 2014, Wang J . et al reported based on the monoclinic KYb 2 f 7 The multi-photon upconversion luminescence enhancement mechanism induced by the specific structure of the crystal Yb energy clusters (Nature Mater., 2014, 13, 157-162), however, despite the high Yb doping concentration of this system, its quantum yield is only 0.37%, which is different from the existing Know other NaYF 4 : There is no significant improvement compared to Yb and Er
Furthermore, in 2015, L.M.Wang et al. used high power (10 6 W / cm 2 ) radiation promotes the hexagonal NaYF 4 Phase Change to Highly Ionically Ordered Cubic NaYF 4 , the quantum yield is as high as 8.2% (Adv. Mater., 2015, 27, 5528-5533), but such high-power radiation limits the practical application and promotion of this method

Method used

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  • A single-doped-enriched core-shell structure up-conversion luminescent material and its preparation method
  • A single-doped-enriched core-shell structure up-conversion luminescent material and its preparation method
  • A single-doped-enriched core-shell structure up-conversion luminescent material and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0043] NaYF 4 :10%Er 3+ @NaYbF 4 @NaYF 4 preparation of

[0044] Step 1: NaYF 4 :10%Er 3+ Synthesis of C-nuclear nanomaterials: 0.9 mmol of Y-TFA and 0.1 mmol of Er-TFA in ethanol and 1 mmol of Na-TFA in ethanol were mixed, and ethanol was removed under argon flow at 120°C for 40 minutes to obtain trifluoroacetate Powder; add 8ml of oleic acid and 12ml of octadecene solvent under the Ar flow at room temperature, rise to 200°C for rapid dissolution, and cool down to room temperature; switch to Ar flow and remove water at 170°C for 40 minutes, then heat up to 270°C for 13 minutes, Incubate for 20 minutes, and after natural cooling, centrifuge twice with ethanol and place in 10ml cyclohexane.

[0045] Step 2: NaYF 4 :10%Er 3+ @NaYbF 4 Synthesis of C@S1-core-shell nanomaterials: Take 3ml of C-cyclohexane dispersion for core-shell structure synthesis. Take 1 mmol of Yb-TFA ethanol solution and 1 mmol of Na-TFA ethanol solution, remove ethanol for 30 minutes under argon fl...

Embodiment 2

[0050] NaYF 4 :50%Er 3+ @NaYbF 4 @NaYF 4 preparation of

[0051] Step 1: NaYF 4 :50%Er 3+ Synthesis of C-nuclear nanomaterials: 0.5mmol Er-TFA ethanol solution, 0.5mmol Y-TFA ethanol solution and 1mmol Na-TFA ethanol solution were mixed, and ethanol was removed under argon flow at 120°C for 30min to obtain trifluoro Acetate powder; add 8ml of oleic acid and 12ml of octadecene solvent under the Ar flow at room temperature, rise to 200°C for rapid dissolution, and then cool down to room temperature; switch to argon flow and remove water at 170°C for 30 minutes, then heat up to 270°C, keep warm for 16min, after natural cooling, centrifuge twice with ethanol, and place in 10ml cyclohexane.

[0052] Step 2: NaYF 4 :50%Er 3+ @NaYbF 4 Synthesis of C@S1-core-shell nanomaterials: Take 3ml of C-cyclohexane dispersion for core-shell structure synthesis. Take 1 mmol of Yb-TFA ethanol solution and 1.5 mmol of Na-TFA ethanol solution, remove ethanol at 120°C for 30 minutes under a...

Embodiment 3

[0056] NaGdF 4 :10%Er 3+ @NaYbF 4 @NaGdF 4 preparation of

[0057] Step 1: NaGdF 4 :10%Er 3+ C-Synthesis of nuclear nanomaterials: Mix 0.9 mmol of Gd-TFA and 0.1 mmol of Er-TFA in ethanol and 2 mmol of Na-TFA in ethanol, remove ethanol at 170°C for 20 minutes under argon flow to obtain trifluoroacetate powder; Add 4ml of oleic acid and 6ml of octadecene solvent under the Ar flow at room temperature, rise to 160°C for rapid dissolution, and then cool down to room temperature; switch to Argon flow and remove water at 120°C for 30 minutes, then raise the temperature to 320°C for 13 minutes, and keep warm for 16 minutes , after cooling naturally, centrifuge twice with ethanol and place in 10ml cyclohexane.

[0058] Step 2: NaGdF 4 :10%Er 3+ @NaYbF 4 Synthesis of C@S1-core-shell nanomaterials: Take 3ml of C-cyclohexane dispersion for core-shell structure synthesis. Take 1 mmol of Yb-TFA ethanol solution and 1.5 mmol of Na-TFA ethanol solution, remove ethanol at 120°C for ...

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Abstract

The invention discloses a mono-doped-enriched core-shell structure up-conversion luminescent material and a preparation method thereof. A chemical expression formula of the material is NaLnF4:A3+@NaYbF4@NaLnF4. The preparation method includes following steps: step 1, synthesizing a NaLnF4:A3+ core nanomaterial; step 2, epitaxially growing a NaYbF4 layer around the NaLnF4:A3+ core nanomaterial to obain a NaLnF4:A+@NaYbF4 core-shell nanomaterial; step 3, epitaxially growing a NaLnF4 layer around the NaLnF4:A3+@NaYbF4 core-shell nanomaterial to obtain NaLnF4:A3+@NaYbF4@NaLnF4. The NaLnF4:A3+@NaYbF4@NaLnF4 core-shell structure can effectively solve the problem of co-doping concentration limitation of intracell energy transfer, can effectively realize efficient light emitting of the up-conversion luminescent material, is found conducive to luminescence of three-photo transition emission especially under a Yb-enriched sensitized shell layer and realizes two-magnitude-order enhancement of 407nm wavelength.

Description

technical field [0001] The invention belongs to the field of preparation of up-conversion luminescent materials, and more specifically relates to a single doping-enrichment core-shell structure up-conversion luminescent material based on energy transfer and a preparation method thereof. Background technique [0002] In recent years, rare earth up-conversion luminescent materials have broad application prospects in various fields such as lighting, display, photoelectric conversion of solar cells, and bioluminescent imaging due to their excellent fluorescence properties. research hotspot. At present, the known high-efficiency upconversion luminescence processes can be roughly divided into three types: excited state absorption, energy transfer upconversion and photon avalanche. Among them, the energy transfer upconversion by combining sensitized ions and activated ions has been widely studied due to its high energy conversion efficiency and low power excitation performance. H...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85C09K11/02B82Y40/00
CPCB82Y40/00C09K11/02C09K11/7705
Inventor 马颖周斌唐冰阮霖霁翟天佑
Owner HUAZHONG UNIV OF SCI & TECH
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