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Method for preparing fluorescent nano material converted on NaYF4

A technology of fluorescent nanomaterials and rare earth ions, applied in the field of preparation of NaYF4 up-conversion luminescent nanomaterials, can solve problems such as troublesome operation and difficult control

Inactive Publication Date: 2009-09-09
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently used to prepare NaYF 4 None of the particle methods can achieve both shape and size control and water solubility, and further organic functionalization is required to achieve water solubility or connection with biomolecules, which is troublesome to operate and difficult to control

Method used

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  • Method for preparing fluorescent nano material converted on NaYF4
  • Method for preparing fluorescent nano material converted on NaYF4
  • Method for preparing fluorescent nano material converted on NaYF4

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 0.8041 g of Y (NO 3 ) 3 ·6H 2 O, 0.3504 g Yb (NO 3 ) 3 ·6H 2 O and 0.0692 g Er(NO 3 ) 3 ·6H 2 O (Y / Yb / Er molar ratio 70:25:5) was dissolved in 10ml of deionized water, the concentration of the mixed solution was 0.3mol / l, and then 1.2 grams of sodium polyacrylate (molecular weight was 5100) was added to make it in the mixed solution The percentage concentration is 10%, stir to make it fully dissolved. Adjust the pH value to 4 with dilute nitric acid, and keep stirring for 1h to generate a stable white complex. Then add 0.4445 grams of ammonium fluoride (the ratio of fluoride ion to rare earth ion is the stoichiometric ratio of the structural formula), and stir until the solution forms a nearly transparent colloid. It was then transferred to a 20 ml autoclave lined with polytetrafluoroethylene, and the autoclave was placed in an oven at 180° C. for 4 h. After natural cooling, centrifuge, wash, and vacuum-dry at 30°C to obtain spherical nanocrystalline gra...

Embodiment 2

[0025] Weigh 1.0913 grams of Y (NO 3 ) 3 ·6H 2 O, 0.0140 g Yb (NO 3 ) 3 ·6H 2 O and 0.0552 g Er(NO 3 ) 3 ·6H 2 O (Y / Yb / Er molar ratio 95: 1: 4) is dissolved in 10ml deionized water, and the concentration of the mixed solution is 0.3mol / l, then adding 5ml concentration is 5% maleic acid acrylic acid copolymer sodium salt (molecular weight is 50000, the percentage concentration is 1.5%), adjust the pH value to 3.5 with 0.5mol / l dilute nitric acid, stir to make it react fully, and keep stirring for 1h. Then add 25ml of sodium fluoride solution with a concentration of 0.96mol / l, stir for 4 hours, transfer to a 60ml autoclave, and place in an oven at 140°C for 48 hours. After natural cooling, centrifuge, wash, and vacuum-dry at 80°C to obtain spherical particle-like Yb with an average size of 400nm 3+ , Er 3+ Doped with NaYF 4 Upconverting fluorescent nanomaterials. see figure 2 Field emission scanning microscope topography photographs are shown.

Embodiment 3

[0027] Weigh 0.2427 g of YCl 3 ·6H 2 O, 0.0388 g YbCl 3 ·6H 2 O and 0.0383 g TmCl 3 ·6H 2 O (Y / Yb / Tm molar ratio 80: 10: 10) is dissolved in 10ml deionized water, and the concentration of the mixed solution is 0.1mol / l, then adding 10ml concentration is 3% maleic acid acrylic acid copolymer sodium salt (molecular weight is 50000, the percentage concentration is 1.5%), stir to make it fully react. Adjust the pH value to 6 with dilute hydrochloric acid, and keep stirring for 1h. Then add 20ml of ammonium fluoride solution with a concentration of 0.6mol / l, stir until almost transparent, then transfer to a 60ml autoclave, and place in an oven at 180°C for 24h. After natural cooling, centrifuge, wash, and dry at 60°C to obtain hexagonal flaky crystal Yb with a size of 1 μm 3+ , Tm 3+ Doped with NaYF 4 Upconverting fluorescent nanomaterials. see image 3 Field emission scanning microscope topography photographs are shown.

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Abstract

The invention relates to a method for preparing fluorescent nano material converted on NaYF4, comprising the steps: yttrium nitrate, ytterbium nitrate and erbium nitrate or yttrium chloride, ytterbium chloride, erbium chloride and thulium chloride are dissolved in de-ionized water according to the mixture radio that the mol ratio of rare earth ions which are yttrium ion, ytterbium ion and erbium ion is equal to (70-95): (1-25): (0.5-10), so that the mixed solution is prepared; water soluble polymer having the ligand radical with the rare earth ions is added into the mixed solution for stirring reaction to form complex compound; the pH value of the mixed solution is adjusted to be 2-6; sodium fluoride, ammonium fluoride or hydrofluoric acid can be added into the mixed solution and stirred until colloid solution that is approximately transparent is obtained; then, the colloid solution is put into a high pressure closed reactor and heated at the temperature of 140-200 DEG C; after that the obtained product is cooled to be the room temperature, centrifugated, separated, washed and dried, finally, the fluorescent nano material converted on NaYF4 is obtained. The method can be used for preparing the converted material at lower temperature, the particle size and the appearance can be controlled, and the water-solubility is good.

Description

technical field [0001] The present invention relates to NaYF 4 Preparation method of up-conversion luminescent nanomaterials, especially a NaYF with controllable particle size and morphology 4 Preparation method of upconversion fluorescent nanomaterial. Background technique [0002] An upconversion luminescent material is a material that can emit visible light when excited by near-infrared light. Due to its special properties, up-conversion materials can be used in many aspects such as three-dimensional display, infrared detection, solid-state laser, anti-counterfeiting, and high-sensitivity biomolecular fluorescent labeling materials. In recent years, the use of up-conversion fluorescent materials as biomolecular fluorescent labeling materials has attracted widespread attention due to their high detection sensitivity. As a fluorescent labeling material for biomolecules, the size and shape of the material itself need to be controllable, the size distribution is uniform, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C30B7/10C30B29/12
Inventor 孙雅娟孔祥贵刘晓敏曾庆辉张友林于沂
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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