Preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal

A paramagnetic, bifunctional technology, applied in the field of preparation of up-conversion fluorescent/paramagnetic bifunctional nanocrystals, can solve problems such as no public reports, and achieve huge industrial development prospects, high energy utilization, and improved efficiency. Effect

Inactive Publication Date: 2012-06-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, rare earth-doped upconversion nanocrystals have been synthesized rapidly (within a few minutes) by heating with microwave radiation in cheap and clean solvents such as water / ethanol, especially NaGdF 4 The literature and patents of monodisperse nanocrystals with both upconversion fluorescence and magnetism as a matrix have not yet been published.

Method used

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  • Preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal
  • Preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal
  • Preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (a) According to the molar ratio of 80% Gd, 18% Yb, 2% Er, accurately weigh 725mg (2mmol) Gd of rare earth oxide 2 o 3 , 177.35 mg (0.45 mmol) Yb 2 o 3 , 19.13 mg (0.05 mmol) Er 2 o 3 In a 50ml flask, add 5ml of pure water and 5ml of concentrated hydrochloric acid with a concentration of 37.5%, seal it tightly, heat it in a water bath at 80-85°C and stir it magnetically to dissolve it completely, then heat the solution slowly until it evaporates to dryness, and then make it to volume In a 25ml volumetric flask, get 0.2mol / L of LnCl 3 (Ln=80%Gd, 18%Yb, 2%Er) Solution A, sealed and stored for future use.

[0037] (b) Put 0.8g NaOH, 4ml H 2 O, 13ml oleic acid, and 7ml ethanol were mixed during stirring to obtain a homogeneous transparent solution B.

[0038] (c) During the stirring process, add 2ml 02mol / L solution A and 3ml 1mol / LNaF solution successively to solution B to obtain homogeneous translucent solution C.

[0039] (d) Take 7ml of the reactant solution fro...

Embodiment 2

[0044] (a) According to the molar ratio of 78% Gd, 20% Yb, 2% Er, accurately weigh 1.41g (3.9mmol) Gd of rare earth oxide 2 o 3 , 394.08 mg (1 mmol) Yb 2 o 3 , 38.25 mg (0.1 mmol) Er 2 o 3 Add 10ml of pure water and 10ml of 37.5% concentrated hydrochloric acid to the flask, seal it tightly, heat it in a water bath at 80-85°C and stir it magnetically to dissolve it completely, then heat the solution slowly until it evaporates to dryness, and then set the volume to 25ml volumetric flask, to obtain 0.4mol / L of LnCl 3 (Ln=78%Gd, 20%Yb, 2%Er) Solution A, sealed and stored for future use.

[0045] (b) Put 0.8g NaOH, 4ml H 2 O, 13ml oleic acid, and 7ml ethanol were mixed during stirring to obtain a homogeneous transparent solution B.

[0046] (c) During stirring, add 1ml of 0.4mol / L solution A and 3ml of 1mol / L NaF solution to solution B to obtain homogeneous translucent solution C

[0047] (d) Take 5ml of the reactant solution from C and add it to the 10mL quartz reactor of ...

Embodiment 3

[0050] (a) Accurately weigh 1078.44mg (2.975mmol) Gd of rare earth oxide according to the molar ratio of 59.5%Gd, 40%Yb, 0.5%Tm 2 o 3 , 788.16mg (2.0mmol) Yb 2 o 3 , 9.65mg (0.025mmol) Tm 2 o 3 Add 5ml of pure water and 3ml of 68% concentrated nitric acid to the flask, seal it tightly, heat it in a water bath at 80-85°C and stir it magnetically to dissolve it completely, then heat the solution slowly until it evaporates to dryness, and then set the volume to 25ml Volumetric flask, get 0.4mol / L LnNO 3 (Ln=59.5% Gd, 40% Yb, 0.5% Tm) Solution A, sealed and stored for future use.

[0051] (b) Put 0.8g NaOH, 4ml H 2 O, 13ml oleic acid, and 7ml ethanol were mixed during stirring to obtain a homogeneous transparent solution B.

[0052] (c) During the stirring process, add 2ml 0.4mol / L solution A and 6ml 1mol / L NaF solution to solution B successively to obtain homogeneous translucent solution C.

[0053] (d) Take 5ml of the reactant solution from C and add it to the 10mL quart...

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Abstract

The invention discloses a preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal, relating to a luminescent nanometer material. A quick and environment-friendly preparation method of up-conversion fluorescence/paramagnetic difunctional nanocrystal is provided, which comprises the following steps: dissolving rare-earth oxide in a determined molar ratio into hydrochloric acid or nitric acid solution to obtain chloride or nitrate solution mixed with various rare-earth elements; mixing sodium hydroxide, oleic acid, ethanol and water; fully stirring the mixture to obtain a homogeneous solution; adding rare-earth chloride or nitrate solution and sodium fluoride water solution, and fully mixing to obtain reaction precursor; and performing microwave synthesis of the reaction precursor solution, and after the reaction stops, centrifugating, washing and drying the product to obtain up-conversion fluorescence/paramagnetic difunctional nanocrystal. The preparation method well combines the ethanol/water solvent system and the microwave heating, is green and environment-friendly, has simple process, is easy to obtain cheap raw materials and has high efficiency; the product has regular shape, uniform size and good dispersity and has up-conversion fluorescence and paramagnetic properties.

Description

technical field [0001] The invention relates to a luminescent nanometer material, in particular to a method for preparing an upconversion fluorescent / paramagnetic double-functional nanocrystal. Background technique [0002] The up-conversion luminescence process involving multiphotons can convert long-wavelength excitation light into short-wavelength emission light. Due to its unique luminescent properties, up-conversion luminescent materials have important applications in many aspects such as solid-state lasers, fiber amplifiers, anti-counterfeiting technology, three-dimensional displays, and solar cells. In recent years, rare earth-doped upconversion luminescent nanomaterials have attracted extensive attention as bioluminescent probes in the fields of fluorescence detection and labeling of cells and tissues, biomolecular recognition, and disease diagnosis. Rare earth-doped upconversion luminescent nanomaterials can emit near-infrared, visible and even ultraviolet light un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 任磊王东
Owner XIAMEN UNIV
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