A rare earth-doped up-conversion nanocrystalline luminescent material and its preparation method
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A technology of rare earth doping and luminescent materials, applied in luminescent materials, nano optics, nanotechnology, etc., can solve the problems of high temperature and low luminous efficiency, and achieve the effect of low crystallization temperature and good up-conversion luminescent performance
Active Publication Date: 2020-03-10
GUANGDONG UNIV OF TECH
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[0003] However, the current up-conversion luminescence efficiency of rare earth-doped up-conversion nanoparticles is low, and its preparation temperature is generally 260°C to 300°C, which is too high
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Embodiment 1
[0040] This embodiment provides a method for preparing rare earth-doped up-conversion nanocrystalline luminescent material, including:
[0041] (1) In a two-necked flask, add yttrium acetate (1.6mL, 0.2M), ytterbium acetate (0.4mL, 0.2M), thulium acetate (0.04mL, 0.02M), oleic acid (90%) and 1- Octadecene (90%), heated to 150°C in a heating mantle and kept for 1 hour to remove the water in the solution to obtain the first reaction liquid containing the rare earth-oleic acid complex precursor; among them, oleic acid and 1 -The volume ratio of octadecene is 3:7.
[0042] (2) Cool the first reaction solution to room temperature, evacuate and vent argon, and add NaOH (1mL, 1M) and NH through a single-channel syringe pump at a drip rate of 0.5mL / min under argon atmosphere 4 F (3.8mL, 0.4M), raise the temperature to 45℃, keep stirring under argon atmosphere for 1h; then, raise the temperature to 110℃ to remove methanol in the solution; then raise the temperature under argon atmosphere A...
Embodiment 2
[0045] The difference between this embodiment and Embodiment 1 is:
[0046] NH 4 The molar ratio of F to NaOH is 1.6:1;
[0047] The sample obtained is labeled Sample 2.
[0048] The other parts are basically the same as in Embodiment 1, and will not be repeated here.
Embodiment 3
[0050] The difference between this embodiment and Embodiment 1 is:
[0051] The crystallization temperature of step (2) is 280°C;
[0052] The sample obtained is labeled Sample 3.
[0053] The other parts are basically the same as in Embodiment 1, and will not be repeated here.
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Abstract
The invention belongs to the technical field of light-emitting materials and particularly relates to a rare-earth doped upconversion nanocrystalline light-emitting material and a preparation method thereof. The chemical formula of the rare-earth doped upconversion nanocrystalline light-emitting material is NaYF4:Yb/Tm(x/y mol%), wherein x=20, and y=0.2. The rare-earth doped upconversion nanocrystalline light-emitting material is in a pure hexagonal phase and of a snowflake shape and has large specific surface area. Test results show that the rare-earth doped upconversion nanocrystalline light-emitting material has good upconversion light-emitting performance under the excitation of 980-nanometer near infrared light and is high in conversion light-emitting efficiency. The preparation methodhas the advantages that the rare-earth doped upconversion nanocrystalline light-emitting material is prepared by co-doping sensitizer Yb<3+> and activator Tm<3+> in host material NaYF4 which is low in phonon energy and high in chemical stability, the rare-earth doped upconversion nanocrystalline light-emitting material is obtained by the co-precipitation of yttrium acetate, ytterbium acetate, thulium acetate, NH4F and NaOH in solvent oleic acid (OA) and 1-octadecane (ODE), low crystallization temperature is achieved, crystal growth can be achieved at 220 DEG C, and efficiency and safety are achieved.
Description
Technical field [0001] The invention belongs to the technical field of luminescent material preparation, and specifically relates to a rare earth doped up-conversion nanocrystalline luminescent material and a preparation method thereof. Background technique [0002] Rare earth-doped up-conversion nanoparticles (UCNPs) are a class of promising and widely used new fluorescent materials, which can convert low-energy near-infrared light excitation light into high-energy shortwave emission. Because UCNPs have narrow emission bands, long fluorescence lifetime, high chemical stability, and low potential biological toxicity, and because near-infrared lasers are used as excitation light sources, they have a deep tissue penetration depth and no interference and scattering from autofluorescence of biological samples Significant advantages such as light interference and almost no damage to biological tissues, have important application prospects in the fields of fluorescent biological detect...
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