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Preparation method of monodisperse silicon dioxide fluorescent microspheres

A technology of silica and fluorescent microspheres, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of reducing the surface activity of fluorescent microspheres, biocompatibility, and consuming silicon hydroxyl groups, so as to enhance luminescent performance and save energy. Effects of cost, broad application prospects

Inactive Publication Date: 2016-12-14
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the surface modification method will consume the silanol on the surface of the fluorescent microspheres, thereby reducing the surface activity and biocompatibility of the fluorescent microspheres.

Method used

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  • Preparation method of monodisperse silicon dioxide fluorescent microspheres
  • Preparation method of monodisperse silicon dioxide fluorescent microspheres

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Embodiment 1

[0019] Weigh 1mmolEu(NO 3 ) 3 Crystals were dissolved in 20mL95% absolute ethanol to prepare a solution, and another 3mmol DBM and 3mmol triethylamine were dissolved in 20mL 95% absolute ethanol to prepare b solution. The solution was dripped into solution b drop by drop. During the whole reaction process, the pH value of the whole reaction system was adjusted by triethylamine to maintain between 6.5-7.0. After stirring for 1 hour, it was suction filtered, washed and dried to obtain light yellow solid powder .

[0020]Measure 25mL of distilled water, 65mL of absolute ethanol, and 7mL of ammonia water in a beaker, and ultrasonically oscillate for 20 minutes to mix them evenly. In solution c, react for 30 minutes to obtain solution d; separately measure 18 mL of absolute ethanol, 8 mL of distilled water, and 2 mL of ammonia water in a beaker, and ultrasonically oscillate for 5 minutes to obtain solution e. Pour solution e into solution d at one time and react for 20 minutes to...

Embodiment 2

[0022] Weigh 1mmolEu(NO 3 ) 3 Crystals were dissolved in 20mL 95% absolute ethanol to prepare a solution, and another 3mmol TTFA and 3mmol triethylamine were dissolved in 20mL 95% absolute ethanol to prepare b solution. The solution was dripped into the b solution drop by drop. During the whole reaction process, the pH value of the whole reaction system was adjusted by triethylamine to maintain between 6.5-7.0. After stirring for 1 hour, it was suction filtered, washed and dried to obtain a white solid powder.

[0023] Measure 25mL of distilled water, 65mL of absolute ethanol, and 7mL of ammonia water in a beaker, and ultrasonically oscillate for 20 minutes to mix evenly. As a c solution, measure 4mL of tetraethyl orthosilicate (TEOS) and slowly add c solution, reacted for 30 minutes to obtain solution d; separately measure 18mL absolute ethanol, 8mL distilled water, and 2mL ammonia water in a beaker, ultrasonically oscillate for 5 minutes, as solution e, pour solution e into...

Embodiment 3

[0025] Weigh 1mmolEu(NO 3 ) 3 Crystals were dissolved in 20mL 95% absolute ethanol to prepare a solution, and another 3mmol TFA and 3mmol triethylamine were dissolved in 20mL 95% absolute ethanol to prepare b solution. The solution was dropped into solution b drop by drop. During the whole reaction process, the pH value of the whole reaction system was adjusted by triethylamine to maintain between 6.5-7.0. After stirring for 1 hour, the rare earth complex was obtained by suction filtration, washing and drying.

[0026] Measure 25mL of distilled water, 65mL of absolute ethanol, and 7mL of ammonia water in a beaker, and ultrasonically oscillate for 20 minutes to mix evenly. As a c solution, measure 4mL of tetraethyl orthosilicate (TEOS) and slowly add c solution, reacted for 30 minutes to obtain solution d; separately measure 18mL absolute ethanol, 8mL distilled water, and 2mL ammonia water in a beaker, ultrasonically oscillate for 5 minutes, as solution e, pour solution e into...

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Abstract

The invention discloses chemical composition and a preparation method of monodisperse silicon dioxide fluorescent microspheres. The general chemical formula of the fluorescent microspheres is SiO2@SiO2:Ln(L)3, wherein SiO2 represents silicon dioxide of the main part of the fluorescent microspheres, Ln represents a rare earth metal element serving as a luminescence center, and L represents an organic ligand serving as the enhanced fluorescence performance. The preparation method of the fluorescent microspheres is an organic ligand sensitization fluorescence enhancement-sol seed method, that is to say, silicon dioxide is taken as seed nucleuses, and a silicon dioxide-doped rare earth complex is taken as a surface coating substance. The preparation method is simple, and the obtained silicon dioxide fluorescent microspheres are good in sphericility, monodispersity, stability and luminescence property have a wide application prospect on photoelectric materials, fluorescent markers, drug targeting and the like.

Description

technical field [0001] The present invention uses organic ligand sensitized fluorescence enhancement-sol seed method to prepare monodisperse silica fluorescent microspheres, that is, silica is used as the core, and silica-doped rare earth complex is used as the surface coating The invention relates to the preparation of monodisperse silicon dioxide fluorescent microspheres, belonging to the field of fluorescent material preparation. Background technique [0002] Monodisperse silica microspheres are widely used in chromatographic column fillers, coatings, additives, etc. due to their high mechanical strength, good stability, and easy dispersion in solvents. At the same time, silica microspheres also have the advantages of non-toxicity, high biological activity, hydrophilicity, and easy functionalization of surface silicon hydroxyl groups, so they have great application value in the fields of catalysts, biology, and medicine. In order to realize the wider application of silic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/59C09K11/02
CPCC09K11/06C09K11/025C09K11/59C09K2211/182
Inventor 康明牟永仁刘敏孙蓉宋丽贤张平
Owner SOUTHWEAT UNIV OF SCI & TECH
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