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Method for preparing upcoversion nanocrystalline on rare-earth adulterating fluoride

A rare earth doping and fluoride technology, which is applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve the problems that it is difficult to obtain dispersed up-conversion luminescent particles

Inactive Publication Date: 2009-10-07
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

Although high-temperature hot solvent synthesis and combustion methods can obtain particles with a size of about 10-20nm, they are not water-soluble; complex precipitation methods, microemulsion methods, sol-gel methods and hydrothermal synthesis are difficult to obtain dispersibility Good up-converting luminescent particles with a size of about 10nm

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Immerse 0.3 g of SBA-15 into 10 ml of 0.2mol / l Ln(NO 3 ) 3 (Ln=Y, Yb, Er, molar ratio Y / Yb / Er=70:25:5) In the aqueous solution, ultrasonic treatment is performed for 30 seconds, and the mixed solution at room temperature is continuously stirred for 24 hours, taken out, filtered, washed with water, and dried. Then add it to 10ml of 0.8mol / l NaF aqueous solution, continue to stir for 24h, then transfer it to a 20ml polytetrafluoroethylene lined reactor, and conduct hydrothermal treatment at 140℃ for 48h, then take out the product and filter. Wash with water, then add it to 10ml of 5% hydrofluoric acid solution, stir for 2 days, centrifuge, wash with water, and dry under vacuum at 80℃ to obtain Yb 3+ , Er 3+ Doped NaYF 4 Nanocrystalline.

Embodiment 2

[0018] Dip 0.1 g of SBA-15 into 10 ml of 0.1 mol / l Ln(NO 3 ) 3 (Ln=La, Yb, Tm, molar ratio La / Yb / Tm=95:1:4) In an aqueous solution, irradiate ultrasonic waves for 5 minutes, and the mixed solution is continuously stirred for 24 hours, taken out, filtered, washed with water, and dried. Then add it to 10ml 0.4mol / l NH 4 In the F aqueous solution, stir for 2h, then transfer it to a 20ml polytetrafluoroethylene lined reactor, hydrothermally heat at 160℃ for 24h, take it out and filter, after washing with water, add it to 10ml of 4% hydrofluoric acid In the solution, stir for 3 days, centrifuge, wash with water, and dry under vacuum at 60℃ to obtain Yb 3+ , Tm 3+ Doped LaF 3 Nanocrystalline.

Embodiment 3

[0020] Dip 0.2g of FSM-16 into 10ml of 0.1mol / l LnCl 3 (Ln=Y, Yb, Er, molar ratio Y / Yb / Er=70:20:10) In an aqueous solution, ultrasonically irradiate for 30 seconds, and the mixed solution at room temperature is continuously stirred for 24 hours, taken out, filtered, washed with water, and dried. Then add it to 10ml 0.4mol / l NH 4 Stir in F water solution for 2h, then transfer it to a 20ml polytetrafluoroethylene lined reactor, hydrothermally heat at 100℃ for 48h, take it out and filter, wash with water, add it to 10ml of 2% hydrofluoric acid In the solution, stir for 3 days, centrifuge, wash with water, and dry under vacuum at 40℃ to obtain Yb 3+ , Er 3+ Doped YF 3 Nanocrystalline.

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Abstract

The present invention relates to an improved method for preparing an upcoversion nanocrystalline on a rare-earth adulterating fluoride which includes steps as follows: weighing rare-earth nitrates Ln(NO3)3 or rare-earth chlorides LnCl3, adding de-ionized water for confecting combined stock solution with 0.05-0.2 mol / l concentration; adding mesoporous molecular screen powder into the solution, ultrasonic treatment, mixing continuously, filtering, deposition bathing, drying; adding the obtained solid powder into fluor oligosol or ammonium fluoride water solution, stirring for reacting thoroughly; moving the reaction mixer into a reactor, water heat treating 8-48 hours under temperature 100-180 deg c; placing the product into a fluohydric acid solution to soak for removing molecular screen forwork, bathing and vacuum drying for obtaining upcoversion irradiancy nanocrystalline of rare-earth adulterating fluoride with less than 10 nm size. The upcoversion irradiancy nanocrystalline does not agglomeration and can obtain globular shape particle with uniform decentralized.

Description

Technical field [0001] The invention relates to an improved method for preparing rare earth-doped fluoride upconversion nanocrystals. Background technique [0002] Upconversion luminescence refers to the use of low-energy light excitation to obtain high-energy light. It is widely used in near infrared light detection, imaging and lasers. In recent years, because of its high detection sensitivity, up-conversion fluorescent materials, as a new type of fluorescent markers, have broad application prospects in drug screening, biomolecular recognition, immunoassays and clinical diagnosis. As a fluorescent labeling material for biomolecules, especially when used for in vivo labeling, due to the needs of metabolism, the material itself is required to be small in size, uniform in distribution, good in dispersibility, and soluble in water. At present, the commonly used methods for synthesizing rare earth upconversion luminescent nanocrystals include high-temperature thermal solvent synthes...

Claims

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Application Information

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