Dye-sensitized rare earth upconversion material and preparation method thereof

A rare earth up-conversion and dye sensitization technology, applied in the field of rare-earth up-conversion materials and their preparation, can solve the problems of low luminous efficiency and the like

Active Publication Date: 2017-12-29
哈尔滨凯美斯科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the technical problem of low luminous efficiency of existing dye-sensitized u

Method used

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  • Dye-sensitized rare earth upconversion material and preparation method thereof
  • Dye-sensitized rare earth upconversion material and preparation method thereof
  • Dye-sensitized rare earth upconversion material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Example 1: Dye-sensitized Nd@Yb@Er / Yb@Yb@Nd doped NaYF in this example 4 The preparation of the hollow multilayer spherical shell is carried out in the following steps:

[0054] 1. SiO2 2 Preparation of nanosphere template: 4ml tetraethyl orthosilicate was quickly added to 65ml ethanol, 28ml deionized water and 7ml ammonia water and stirred for 2 hours. After washing three times with ethanol centrifugation, dry at 60°C for 12 hours to obtain SiO 2 . Prepared SiO 2 The TEM photo of figure 2 As shown, the product is a sphere with a diameter of about 100nm, and the size is relatively uniform;

[0055] 2. Preparation of luminescent layer:

[0056] (1) 30mg of SiO 2 The pellets were ultrasonically dispersed with 100 ml of deionized water at 40°C for 45 minutes, after which 0.25 mol of urea and a total of 0.5 mmol of YCl 3 , YbCl 3 , ErCl 3 Join (YCl 3 , YbCl 3 , ErCl 3 The molar ratio is 80:18:2) to continue ultrasonication, then transfer the mixture into a bea...

Embodiment 2

[0070] Embodiment 2: The difference between this embodiment and embodiment 1 is that the package of step 3 contains Yb 3+ The shell method and step 4 include Nd 3+ The thermal decomposition method of the shell is replaced by a hydrothermal method, and other steps and parameters are the same as in Example 1.

[0071] Wherein the inner transfer layer and the outer transfer layer of step 3 (i.e. the package contains Yb 3+ The specific method of preparation is: weigh the Yb(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O (the molar ratio of Yb to Y is 1:9), and 0.146g of EDTA were dissolved in 20ml of deionized water and stirred for 30 minutes. 0.2mmol of Er / Yb:NaYF 4 The spherical shell precursor and 0.262g of NaF were stirred and dispersed into 20ml of deionized water, and then slowly added to the rare earth nitrate solution and stirred for 30 minutes. After standing still for 2 hours, the supernatant was poured out, and the obtained white precipitate mixture was put into a re...

Embodiment 3

[0074] Example 3: In this example Nd@Yb@Er / Yb@Yb@Nd doped with LiYF 4 The preparation method of the hollow multi-layer spherical shell is different from Example 1 in that: the ErCl in Example 1 3 Replaced by the same molar number of TmCl 3 , NaOH in Example 1 is replaced by LiOH of the same molar number, and other steps and parameters are the same as in Example 1.

[0075] Figure 6 Given the dye-sensitized Nd@Yb@Tm / Yb@Yb@Nd doped LiLnF 4 The TEM image of the hollow multilayer spherical shell shows an obvious hollow structure; the corresponding up-conversion fluorescence comparison of the sample is as follows Figure 7 As shown, it can be seen that compared with conventional dye-sensitized up-conversion materials with the same concentration, the up-conversion efficiency of the bidirectional dye-sensitized product of the present invention is significantly improved under the same power density of 808nm laser irradiation.

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Abstract

The invention relates to rare earth upconversion materials and preparation methods thereof, in particular to a dye-sensitized rare earth upconversion material and a preparation method thereof and aims to solve the technical problem of low light emitting efficiency of existing dye-sensitized upconversion materials. The dye-sensitized rare earth upconversion material is in a five-layer hollow spherical shell structure which is composed of an inner layer, an inner transmitting layer, a light emitting layer, an outer transmitting layer and an outer layer sequentially from inside to outside, and infrared dye molecules are connected to surfaces of the inner layer and the outer layer of the hollow spherical shell structure. The preparation method includes: taking a silicon dioxide nanosphere as a template, coating the spherical surface of the template with an upconversion shell layer as the light emitting layer, etching the silicon dioxide to obtain a hollow upconversion spherical shell namely the light emitting layer, and simultaneously coating inner and outer surfaces of the hollow spherical shell with Yb<3+>-containing transmitting shell layers and Nd<3+>-containing surface shell layers to construct efficient bidirectional energy transmitting passages, and finally simultaneously connecting the dye molecules to the inner and outer surfaces of the spherical shell to serve as energy absorption antennas. The dye-sensitized rare earth upconversion material is applicable to the biological field of drug loading and controlled release.

Description

technical field [0001] The invention relates to a rare earth up-conversion material and a preparation method thereof, belonging to the field of optical materials. Background technique [0002] After rare earth ions absorb multiple incident near-infrared photons and jump to a higher energy level through excited state absorption or energy transfer process, the process of spontaneous emission to generate fluorescence is called upconversion fluorescence. The upconversion fluorescence phenomenon of rare earth ions has attracted great attention in recent years due to its unique advantages in the fields of biomarkers, solar cells, cancer phototherapy, and three-dimensional display. Especially Nd 3+ / Yb 3+ / Er 3+ The doped system has great prospects in biological applications because the system uses 808nm laser for pumping, avoiding the conventional Yb 3+ / Er 3+ The 980nm laser corresponding to the system has a strong thermal effect in the human body. [0003] However, the up-...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/85
CPCC09K11/02C09K11/7773
Inventor 刘禄闫东唐东阳卢开雷赵恩铭
Owner 哈尔滨凯美斯科技有限公司
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