Preparation method of rare earth-doped sodium gadolinium tetrafluoride nanomaterial

A technology of sodium gadolinium tetrafluoride and nanomaterials, which is applied in the fields of chemical instruments and methods, luminescent materials, etc., and can solve the problems of the preparation and subsequent application of rare earth fluoride up-conversion luminescent nanomaterials, the large size of rare earth fluoride nanoparticles, three To solve the problems of high toxicity of fluoroacetate and achieve the effect of easy promotion, simple and novel process, and uniform size

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

AI Technical Summary

Problems solved by technology

Generally, the small-sized rare earth fluoride nanoparticles produced by hydrothermal solvothermal system are mainly a-crystal form, but the luminescence efficiency of a-crystal form is low
The thermal cracking method can well control the crystal shape and size, and can generate rare earth fluoride up-conversion luminescent nanocrystals with small size (< 50nm) and b crystal form, but the thermal cracking method also has defects, such as trifluoroacetic acid commonly used in this system Salt is highly toxic, and the reaction process needs to be carried out under the conditions of anhydrous, anaerobic and inert gas protection
However, compared with the traditional method, the rare earth fluoride nanoparticles synthesized by the ionic liquid method generally have larger size, wider particle size distribution and poor dispersion.
[0005] Although the above existing methods have successfully synthesized rare earth fluoride upconversion nanomaterials, these existing technologies have their own defects, which largely limit the preparation and subsequent application of rare earth fluoride upconversion luminescent nanomaterials.

Method used

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  • Preparation method of rare earth-doped sodium gadolinium tetrafluoride nanomaterial
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  • Preparation method of rare earth-doped sodium gadolinium tetrafluoride nanomaterial

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Experimental program
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Effect test

Embodiment 1

[0031] (a) 20mmol of solid RECl 3 ·6H 2 O (RE=Gd, Yb, Er) and 60mmol of sodium oleate were dissolved in 30mL of distilled water, 40mL of absolute ethanol and 70mL of n-hexane and refluxed for 4 hours, then poured into a pear-shaped separatory funnel for separation, leaving The upper organic phase was washed with 35 mL of distilled water, repeated three times, and vacuum-dried to prepare a rare earth oleic acid complex;

[0032] (b) Take 1 mmol of rare earth oleic acid complex and 1 mmol of sodium oleate, add 3 mL of oleic acid, and raise the temperature to about 140 ° C under the protection of nitrogen to dissolve all of them to prepare a rare earth oleic acid precursor solution;

[0033] (c) Take out the rare earth oleic acid precursor solution prepared in the second step, add it into the polytetrafluoroethylene liner of the hydrothermal reaction kettle, and then add 15mL of butylmethylimidazolium tetrafluoroborate ionic liquid (BmimBF 4 );

[0034] (d) Put the hydrotherma...

Embodiment 2

[0036] (a) 10mmol of solid GdCl 3 ·6H 2 O and 30mmol of sodium oleate were dissolved in 15mL of distilled water, 20mL of absolute ethanol and 35mL of normal hexane and were refluxed for 4 hours, then poured into a pear-shaped separating funnel for liquid separation, leaving the upper organic phase, adding 15mL of distilled water for washing, Repeat three times, carry out vacuum drying, make rare earth oleic acid complex;

[0037] (b) Take 0.5 mmol of rare earth oleic acid complex and 0.5 mmol of sodium oleate, add 3 mL of oleic acid, and heat up to about 140 °C under the protection of nitrogen to dissolve all of them to prepare a rare earth oleic acid precursor solution;

[0038] (c) Take out the rare earth oleic acid precursor solution prepared in the second step, add it to the polytetrafluoroethylene liner of the hydrothermal reaction kettle, and then add 5 mL of butylmethylimidazolium tetrafluoroborate ionic liquid (BmimBF 4 ), finally add 20mL of methanol solution;

[0...

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Abstract

The invention discloses a method of preparing a rare earth-doped sodium gadolinium tetrafluoride nanomaterial. The method comprises the following steps of: (1) dissolving solid rare earth chloride and sodium oleate in a solvent and performing reflux treatment, separating and collecting the supernatant organic phase, washing with water, and vacuum drying to obtain a rare earth-oleic acid complex compound; (2) adding the rare earth-oleic acid complex compound and sodium oleate into oleic acid and completely dissolving to obtain a rare earth-oleic acid precursor solution; (3) taking out the rare earth-oleic acid precursor solution obtained in the step (2), transferring to the polytetrafluoroethylene inner container of a hydrothermal reaction kettle, and adding butylmethylimidazol tetrafluoroborate to the reaction kettle; and (4) putting the hydrothermal reaction kettle into a muffle furnace, allowing reactions to take place, centrifuging, washing the resulting white solid with distilled water and ethanol in order, and vacuum-drying or freeze-drying, to obtain the rare earth-doped sodium gadolinium tetrafluoride nanomaterial. The method has the advantages of simple process, small number of equipment, low energy consumption and environmental friendliness; and ensures uniform size of the nanomaterial product.

Description

technical field [0001] The invention relates to a preparation method in the technical field of upconversion rare earth fluoride nanomaterials, in particular to a rare earth doped sodium gadolinium tetrafluoride (NaGdF 4 : Yb, Er) nanomaterials preparation method. Background technique [0002] NaGdF 4 :Yb, Er nanomaterials, as a new class of upconversion luminescent materials, have become one of the hotspots of research at home and abroad. NaGdF 4 : Yb, Er nanomaterials have special properties, it can have two emission peaks at 550 nm and 650 nm under the excitation of 980 nm near-infrared excitation light source, and b-NaGdF 4 : Yb, Er up-conversion luminous efficiency is better than a-NaGdF 4 : Yb, Er are at least an order of magnitude higher. And the wavelength and intensity of the generated light can be adjusted by different rare earth doping elements, so it can be applied to up-conversion fluorescence imaging. In addition, due to the existence of Gd element, it can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 何蒙崔大祥
Owner SHANGHAI JIAO TONG UNIV
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