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Preparation method of rare earth doped fluoride nano dispersion liquid

A nano-dispersion, rare earth doping technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low concentration dispersion, low fluorescence efficiency, etc., and achieve the effects of improving uniformity, improving luminous efficiency, and low temperature

Inactive Publication Date: 2014-01-29
XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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Problems solved by technology

[0005] In order to solve the problems of low-concentration dispersion and low fluorescence efficiency of rare earth-doped fluoride nanomaterials in organic liquids, the invention provides a preparation method of rare earth-doped fluoride nano-dispersion liquid

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  • Preparation method of rare earth doped fluoride nano dispersion liquid
  • Preparation method of rare earth doped fluoride nano dispersion liquid
  • Preparation method of rare earth doped fluoride nano dispersion liquid

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preparation example Construction

[0023] A preparation method of a rare earth-doped fluoride nano-dispersion liquid, specifically comprising the following steps:

[0024] 1) Preparation of rare earth doped fluoride nanopowder:

[0025] Add ethanol or methanol to the mixed solution of 0.2mol / L nitrate solution of rare earth ions and 0.2mol / L nitrate solution of matrix ions, the doping concentration range of rare earth ions is 0.5~20mol%, under the condition of ultrasonic oscillation, Continue to drop 1mol / L of F - Ionic solution, use dilute nitric acid or sodium hydroxide solution to adjust the pH value of the reaction system to 2-4, and react for 10 minutes; then, transfer the reaction mixture into a reaction kettle, and react at 120-200°C for 8-20 hours; Centrifuge at a speed of 8000-10000rpm / min for 10min to obtain the precipitate; wash the precipitate with secondary water and absolute ethanol in sequence, repeat each washing step 3-5 times, and then dry the washed precipitate under vacuum at 65°C for 2 day...

Embodiment 1

[0031] Measure 9.5mL0.2mol / L La(NO 3 ) 3 and 0.5mL0.2mol / L Nd(NO 3 ) 3 , add 20mL ethanol, Nd 3+ The doping concentration of ions was 5 mol%. Under ultrasonic vibration, add 6.0mL1mol / L NaF solution dropwise to the above mixed solution, use sodium hydroxide solution to adjust the pH value of the reaction system to 3, continue the reaction for 10min, transfer the reacted mixed solution into the reaction kettle, React at 150°C for 8h. Centrifuge the product at a speed of 10,000rpm / min for 10min to obtain a precipitate, wash the precipitate with secondary water and absolute ethanol in turn, repeat each washing step 3 times, and then dry the washed precipitate at 65°C under vacuum for 2 days . Finally, grind the dried precipitate to obtain nanopowder, weigh 652 mg of the nanopowder in 1 mL of a mixed solvent of tetrabromoethane and dimethyl sulfoxide, the volume ratio of the two solvents is 1.5:1, and ultrasonically After dispersing for 10min, LaF with a dispersion concentr...

Embodiment 2

[0034] Measure 8.0mL0.2mol / L Y(NO 3 ) 3 and 2.0mL0.2mol / L Nd(NO 3 ) 3 , add 20mL ethanol, Nd 3+ The doping concentration of ions was 20 mol%. Under ultrasonic vibration, add dropwise 6.0mL1mol / L NH 4 For solution F, use sodium hydroxide solution to adjust the pH of the reaction system to 4, continue the reaction for 10 minutes, transfer the reacted mixed solution into a reaction kettle, and react at 170° C. for 12 hours. Centrifuge the product at a speed of 10,000rpm / min for 10min to obtain a precipitate, wash the precipitate with secondary water and absolute ethanol in turn, repeat each washing step 3 times, and then dry the washed precipitate at 65°C under vacuum for 2 days . Finally, grind the dried precipitate into nanopowder, weigh 350 mg of the nanopowder in 1 mL of a mixed solvent of dibromoethane and carbon tetrachloride, the volume ratio of the two solvents is 3:1, and ultrasonically disperse for 10 minutes After obtaining the YF with a dispersion concentration...

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Abstract

The invention provides a preparation method of a rare earth doped fluoride nano dispersion liquid, and solves the technical problems of the existing rare earth doped nano dispersing process that the dispersing concentration is low and the luminous property of the nano dispersion liquid is inhibited by a surface modifier. The method comprises the following steps of using nitrate containing reaction ions as a reaction precursor, adjusting the pH (potential of hydrogen) value of a reaction system, synthesizing a rare earth doped fluoride nano powder by a hydrothermal method, and dispersing the rare earth doped fluoride nano powder into an inorganic solvent by an ultrasonic technique according to solvent polarity, solvent density, nano particle surface charges and the like to obtain a transparent rare earth doped fluoride nano dispersion liquid. The nano dispersion liquid prepared by the preparation method has the advantages of high dispersing concentration, high transparency, high purity and difficulty in aggregation. The preparation method has the advantages that the required temperature is lower, the technology is simple, the operation is easy, and the luminous rate of the rare earth luminous material in the solvent is greatly improved.

Description

technical field [0001] The invention belongs to the field of preparation of rare earth-doped nano-luminescent materials, and in particular relates to a preparation method of rare earth-doped fluoride nano-dispersion liquid with high dispersion concentration, high optical transmittance and high fluorescence intensity. Background technique [0002] Rare earth-doped nano-luminescent materials are important luminescent materials, which have been widely used in optical waveguides, lighting displays, biology and other fields. The luminescent properties of rare earth ions have a great relationship with the host material, which not only requires the host material to have high chemical stability and mechanical strength, but also requires the host material to have low lattice vibration energy. Fluorides are used as host materials for rare earth doping because of their low phonon energy and good stability. So far, research on rare earth ion-doped fluoride nanomaterials has mainly focu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85C09K11/61
Inventor 韦玮彭波崔晓霞王中跃
Owner XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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