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A kind of preparation method of porous rare earth doped up-conversion nanomaterial

A rare earth doping, nanomaterial technology, applied in nanotechnology, luminescent materials, nanotechnology, etc., can solve the problems of limited application, complexity, low yield, etc., and achieve the effect of inhibiting continuous growth

Active Publication Date: 2016-09-28
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the co-precipitation method requires subsequent high-temperature heat treatment higher than 600 ° C. High energy consumption and high temperature will cause a large amount of agglomeration and fusion of nanomaterials; the hydrothermal method that directly uses water as the reaction medium can prepare the required materials through a one-step reaction. However, most of the prepared materials are micron-scale rods / spheres, which limits their further application in the field of bioimaging; the precursor materials and by-products used in the pyrolysis method have high toxicity, and Li Yadong The material prepared by the solvothermal method represented by the professor is hydrophobic and requires subsequent modification
[0005] Nowadays, most of the up-conversion nanomaterials that can be used for drug loading are coated mesoporous silicon. The preparation process is cumbersome and complicated, requiring a large number of subsequent processing steps, so the yield is extremely low and the production cost is high.

Method used

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  • A kind of preparation method of porous rare earth doped up-conversion nanomaterial
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  • A kind of preparation method of porous rare earth doped up-conversion nanomaterial

Examples

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Embodiment 1

[0039] Preparation of Porous Rare Earth Doped Upconversion NaLuF 4 :Yb 3+ , Er 3+ Nanomaterials, the specific steps are as follows:

[0040] (1) the rare earth oxide LuO 3 Add to dilute hydrochloric acid solution, stir until the rare earth oxide LuO 3 Completely dissolve, rotary evaporate, remove excess hydrochloric acid, prepare the rare earth chloride LuCl 3 Storage solution, the rare earth chloride LuCl in the storage solution 3 The molar concentration is 0.4mol / L;

[0041] (2) According to LuCl 3 (20%YbCl 3 +2%ErCl 3 / TmCl 3 / HoCl3 ) : DDBAC: GA is 2: 1: 6, adds DDBAC and GA mixed solution in the rare earth chloride stock solution that step (1) makes, the total molar concentration of both DDBAC and GA is 0.4mol / L in this mixed solution , and fully stirred for 40min;

[0042] (3) According to LuCl 3 (20%YbCl 3 +2%ErCl 3 / TmCl 3 / HoCl 3 ): NaF is 1: 6 to the mixed solution of the additive prepared in step (2) and the rare earth chloride stock solution, slowl...

Embodiment 2

[0047] Preparation of Porous Rare Earth Doped Upconversion NaGdF 4 :Yb 3+ , Er 3+ Nanomaterials, the specific steps are as follows:

[0048] (1) the rare earth oxide GdO 3 Add to dilute hydrochloric acid solution, stir until the rare earth oxide GdO 3 Completely dissolve, rotary evaporate, remove excess hydrochloric acid, prepare rare earth chloride GdCl 3 Stock solution, the rare earth chloride GdCl in the stock solution 3 The molar concentration is 0.1mol / L;

[0049] (2) According to GdCl 3 (20%YbCl 3 +2%ErCl 3 / TmCl 3 / HoCl 3 ): DDBAC: GA is 1: 1: 8, adds DDBAC and GA mixed solution in the rare earth chloride stock solution that step (1) makes, the total molar concentration of both DDBAC and GA in this mixed solution is 0.2mol / L, and fully stirred for 20min;

[0050] Up-conversion materials require a host material that emits light by exciting rare earth ions doped in the host material with near-infrared laser light. For 'GdCl 3 (20%YbCl 3 +2%ErCl 3 / TmCl 3...

Embodiment 3

[0056] Preparation of Porous Rare Earth Doped Upconversion NaGdF 4 :Yb 3+ , Er 3+ For nanomaterials, materials are added according to the ratio of Ln: CTAB: GA: NaF = 1: 1: 8: 12, and the rest are the same as in Example 2. 'Ln' is an abbreviation for lanthanides, referred to here: GdCl 3 (20%YbCl 3 +2%ErCl 3 / TmCl 3 / HoCl 3 )

[0057] Such as Figure 7 In (1) and (2), the prepared NaGdF 4 :Yb 3+ , Er 3+ The nanomaterial is a short porous rod-like structure with a length of about 600nm and a pore diameter of about 300nm.

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Abstract

The invention relates to a preparation method of porous rare earth doped up-conversion nanomaterials, which adopts a one-step hydrothermal method for synthesis. First, a certain concentration of rare earth chloride storage solution is prepared, a surfactant and a foaming agent are added, and then fluorine is slowly added dropwise. A sodium chloride solution is used to prepare a precursor of a rare earth up-conversion nanomaterial, and then the precursor is subjected to a hydrothermal reaction to prepare a porous rare earth-doped upconversion nanomaterial. Compared with the prior art, the invention adopts a one-step hydrothermally induced "explosion" process, which is simple, convenient to operate, easy to popularize and apply on a large scale, and provides a new way and idea for preparing porous nanomaterials, and has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorescent nanometer materials, and relates to a preparation method of nanomaterials, in particular to a preparation method of porous rare earth doped up-conversion nanomaterials. Background technique [0002] The World Health Organization recently released the "2014 World Cancer Report". The number of cancer patients worldwide is increasing at an alarming rate. In 2012, there were 14 million new cases of cancer worldwide and 8.2 million deaths. It is estimated that within 20 years, cancer will With 22 million new cases and 13 million deaths, developing countries are particularly hard hit. Due to changes in lifestyle and aging population, the task of cancer prevention and treatment in China is very arduous. In 2012, there were 3.06 million new cancer cases in my country (accounting for 20% of the world), and 2.2 million cancer deaths (accounting for 25% of the world). The highest incidenc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/77B82Y30/00
Inventor 高国邱培宇孙容瑾崔大祥
Owner SHANGHAI JIAOTONG UNIV
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