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Method for quickly preparing NaYF:Yb/Er upconversion nano particles having different phases

A nanoparticle and phase technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve problems such as trouble, toxicity of reaction by-products, high reaction temperature, etc., and achieve simple and fast operation, simple post-processing of products, dispersion good sex effect

Inactive Publication Date: 2016-03-30
SUN YAT SEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic thermal decomposition method generally uses more expensive organometallic yttrium salts as reactants, and reacts in organic solvents and surfactants such as oleylamine and oleic acid. The reaction temperature is relatively high, and it needs to be carried out in an inert atmosphere. Solvent coating, post-treatment is more troublesome, and the reaction by-products are more toxic (J.Am.Chem.Soc., 2006, 128, 6426–6436)

Method used

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  • Method for quickly preparing NaYF:Yb/Er upconversion nano particles having different phases
  • Method for quickly preparing NaYF:Yb/Er upconversion nano particles having different phases
  • Method for quickly preparing NaYF:Yb/Er upconversion nano particles having different phases

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Experimental program
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Effect test

Embodiment 1

[0026] With 1.0mmol (the total amount of three substances) of Y (NO 3 ) 3 , Yb(NO 3 ) 3 and Er(NO 3 ) 3 Dissolve in 14mL ethanol solution according to stoichiometric ratio 78:20:2, add 3.0mmol NaF solution, stir for 10min, then add 0.342gNH 4 HF 2 , continue to stir for 30 minutes, transfer to a hydrothermal reaction kettle, react at 140°C for 48 hours, naturally cool to room temperature, centrifuge and wash with deionized water and absolute ethanol three times alternately, and obtain β‐NaYF after drying 4 : Yb / Er upconverting nanoparticles.

[0027] The XRD diffraction peaks of the product are as figure 1 As shown in the middle curve a, the shape is as figure 2 As shown, its up-conversion luminescence performance is as image 3 shown. From figure 1 It can be seen from the middle curve a that all diffraction peaks are consistent with β‐NaYF 4 Corresponding to the standard diffraction peak (JCPDS16‐0334).

[0028] From figure 2 It can be seen from the SEM photos...

Embodiment 2

[0031] 0.2mmol of Y (NO 3 ) 3 , Yb(NO 3 ) 3 and Er(NO 3 ) 3 Dissolve in 14mL propanol solution according to stoichiometric ratio 78:20:2, add 0.6mmol NaF solution, stir for 10min, then add 0.068gNH 4 HF 2 , continue to stir for 30 minutes, transfer to a hydrothermal reaction kettle, react at 180°C for 24 hours, naturally cool to room temperature, centrifuge and wash with deionized water and absolute ethanol three times alternately, and obtain β-NaYF after drying 4 : Yb / Er upconverting nanoparticles.

[0032] The XRD diffraction peaks of the product are as figure 1 Shown in curve b. From figure 1 It can be seen from the middle curve b that all the diffraction peaks are consistent with β‐NaYF 4 Corresponding to the standard diffraction peak (JCPDS16‐0334).

Embodiment 3

[0034] 0.5mmol of Y(NO 3 ) 3 , Yb(NO 3 ) 3 and Er(NO 3 ) 3 Dissolve in 14mL acetic acid solution according to the stoichiometric ratio of 78:20:2, add 1.5mmol of NaF solution, stir for 10min, then add 0.171gNH 4 HF2 , continue to stir for 30 minutes, transfer to a hydrothermal reactor, react at 180°C for 24 hours, cool to room temperature naturally, centrifuge and wash with deionized water and absolute ethanol three times alternately, and obtain α-NaYF after drying 4 : Yb / Er upconverting nanoparticles.

[0035] The XRD diffraction peaks of the product are as figure 1 As shown in the middle curve c, the shape is as Figure 4 shown. From figure 1 It can be seen from the middle curve c that all the diffraction peaks are consistent with α‐NaYF 4 Corresponding to the standard diffraction peak (JCPDS77‐2042). From Figure 4 It can be seen from the SEM photos in the figure that the product is nanoparticles with a size of about 100-150 nm.

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Abstract

The invention discloses a method for quickly preparing NaYF:Yb / Er upconversion nano particles having different phases. The method comprises the following steps: dissolving Y(NO3)3, Yb(NO3)3 and Er(NO3)3 in a solvent according to a stoichiometric ratio of 78:20:2 to form a Ln(NO3)3 solution; adding a NaF solution; stirring, adding NH4HF2 to enable the molar ratio of NH3HF2 to Ln(NO3)3 to be (3-6):1; keeping on stirring, and transferring into a hydrothermal reaction kettle, reacting for 3-48 hours at 140-220 DEG C, and naturally cooling to room temperature; and alternately washing the centrifugally separated product with deionized water and absolute ethyl alcohol, and drying to obtain the NaYF:Yb / Er upconversion nano particles, wherein the solvent is ethyl alcohol, propyl alcohol, acetic acid or propionic acid. The preparation is simple to open, easily available in raw materials and high in reaction speed, and the prepared particles have high purity and excellent upconversion luminescence performance.

Description

technical field [0001] The invention relates to the technical field of upconversion nanomaterials, in particular to a method for rapidly preparing NaYF in different phases 4 : A method for Yb / Er upconversion nanoparticles. Background technique [0002] Sodium yttrium fluoride (NaYF 4 ) is an important upconversion matrix material, NaYF 4 : Yb / Er is currently recognized as one of the materials with the highest upconversion luminous efficiency (Inorg.Chem., 2007, 46, 5404‐5410). Anti-counterfeiting, photovoltaic cells, and biomarkers highlight broad application prospects. [0003] Sodium yttrium fluoride has two crystal forms, cubic phase and hexagonal phase, and the performance of the hexagonal phase up-conversion material doped with rare earth ions is significantly better than that of the same doped cubic phase, such as the hexagonal phase NaYF 4 : Yb / Er upconversion intensity ratio cubic phase NaYF 4 : Yb / Er is one to two orders of magnitude higher (J.Mater.Chem., 2009...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85B82Y30/00B82Y40/00
Inventor 庄健乐吴明娒颜靖杨婧羚
Owner SUN YAT SEN UNIV
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