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Water-soluble rare-earth terbium ion-doped cerium fluoride nanocrystallines and preparation method thereof

A technology of ion doping and nanocrystals, applied in chemical instruments and methods, nanotechnology, nano-optics, etc., can solve the problems of low fluorescence yield, single particle shape, poor monodispersity of solvent, etc., and achieve high product yield , simple process, uniform phase effect

Inactive Publication Date: 2013-05-22
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can solve the problems of low fluorescence yield, single particle shape, and poor monodispersity in solvents in the existing preparation methods.

Method used

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  • Water-soluble rare-earth terbium ion-doped cerium fluoride nanocrystallines and preparation method thereof
  • Water-soluble rare-earth terbium ion-doped cerium fluoride nanocrystallines and preparation method thereof
  • Water-soluble rare-earth terbium ion-doped cerium fluoride nanocrystallines and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Mix 1.8mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature until uniform, and obtain NH 4 F / EG mixed solution.

[0037] First weigh 0.15g of polyethyleneimine into another weighing bottle, and the amount is calculated according to the molar ratio of cerium nitrate hexahydrate to 1:6. Then add 0.6mmol cerium nitrate hexahydrate to the same weighing bottle, and inject 9mL of ethylene glycol.

[0038] When mixed to a uniform solution, add the prepared ethylene glycol solution of ammonium fluoride dropwise, stir until uniform, put the solution into a 20mL reaction kettle, put it in an oven at 200°C for 2h, and cool to room temperature.

[0039] The reaction product is directly centrifuged, and the precipitate is washed repeatedly three times with water and ethanol to remove the ethylene glycol in the reaction and the unreacted excess polyethyleneimine, and then dispersed in ethanol to prepare a well-dispersed water-soluble fluorina...

Embodiment 2

[0042] Mix 1.8mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir well at room temperature to obtain NH 4 F / EG mixed solution.

[0043] First weigh 0.15g of polyethyleneimine into another weighing bottle, and the amount is calculated according to the molar ratio of cerium nitrate hexahydrate to 1:6. Then add 0.6mmol cerium nitrate hexahydrate to the same weighing bottle, add terbium trichloride hexahydrate, the amount is calculated according to the ratio of 0.001 to 0.3:1 molar ratio with cerium nitrate hexahydrate. Inject 9 mL of ethylene glycol.

[0044] When mixed to a homogeneous solution, add the prepared NH dropwise 4 F / EG mixed solution, stirred until uniform, put the solution into a 20ml reaction kettle, put it in an oven at 200°C for 2 hours, and cooled to room temperature.

[0045] The reaction product is directly centrifuged, and the precipitate is repeatedly washed with water and ethanol three times to remove the EG in the reaction and the ...

Embodiment 3

[0048] Mix 1.8mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature until uniform, and obtain NH 4 F / EG mixed solution.

[0049] First weigh 0.15g of polyethyleneimine into another weighing bottle, and the amount is calculated according to the molar ratio of cerium nitrate hexahydrate to 1:6. Then add 0.6mmol cerium nitrate hexahydrate to the same weighing bottle, add terbium trichloride hexahydrate, the amount is calculated according to the ratio of 0.001 to 0.3:1 molar ratio with cerium nitrate hexahydrate. Inject 9 mL of ethylene glycol.

[0050] When mixed to a homogeneous solution, add the prepared NH dropwise 4 F / EG mixed solution, stirred until uniform, put the solution into a 20ml reaction kettle, put it in a 160°C oven for 2 hours, and cooled to room temperature.

[0051] The reaction product is directly centrifuged, and the precipitate is washed repeatedly three times with water and ethanol to remove the ethylene glycol in t...

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Abstract

The invention discloses water-soluble rare-earth terbium ion-doped cerium fluoride nanocrystallines and a preparation method thereof, and belongs to the technical field of fluorescent nano-crystalline materials and hydrothermal chemical method synthesis thereof. The rare-earth terbium ion-doped cerium fluoride nanocrystallines are rod-shaped or cube-like; and the polyethyleneimine is coated on the surfaces of the nanocrystallines. The preparation method comprises the following steps of: mixing cerium nitrate hexahydrate, terbium chloride hexahydrate, the polyethyleneimine and ethylene glycol in a certain ratio; reacting for 1 to 12 hours in a baking oven at the temperature of 160 to 240 DEG C; cooling a reaction product; washing the reaction product with water and ethanol; and drying in vacuum. The product has very high solubility, adjustable and controllable appearance, high particle stability and high fluorescence quantum yield, and also can be dispersed in different solvents. In the method, raw materials are cheap and easy to obtain; the process is simple; the cost is low; the process repeatability is high; and the nanocrystallines have a potential application value in the field of biomarkers.

Description

technical field [0001] The invention belongs to the technical field of fluorescent nanocrystal material and its hydrothermal chemical method synthesis, and in particular relates to a rare earth terbium ion-doped cerium fluoride fluorescent nanocrystal and a preparation method thereof. Background technique [0002] Cerium trifluoride (CeF 3 )[CN101172638, CN101172637] is a luminescent material with 100% activator, which has high ion conductivity and unique optical properties. Compared with the traditional oxide matrix, fluoride has lower vibrational energy, the smallest rare earth ion excited state quenching and less absorption in the visible-near infrared region, and fluoride-based nanomaterials are in the field of luminescent materials. Has a wide range of application potential. The energy level transition in the 4f electronic configuration rich in rare earth ions, and the 4f-4f transition of 4f electrons in the 4f electronic shell is parity forbidden, resulting in stable...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85B82Y20/00B82Y30/00
Inventor 施展李菲菲李春光冯守华
Owner JILIN UNIV
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