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Porous silicon dioxide-stabilized noble metal cluster fluorescent material and method for preparing same

A technology of porous silica and fluorescent materials, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of artificial motor protein-protein interaction changes, dyeing, ligand dissociation, etc., and achieve the effect of wide application prospects

Inactive Publication Date: 2012-09-19
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Due to the small particle size and large specific surface area of ​​noble metals, they have extremely high surface energy, and are easy to agglomerate to form larger noble metal nanoparticles, which lose their fluorescence ability
Organic ligands can stabilize noble metal clusters to a certain extent, but in the process of functionalization and aging in biological media, the noble metal clusters stabilized by organic ligands still have the problem of ligand dissociation and instability. Stability is limited; when biomacromolecules are used to stabilize gold and silver clusters, these stable ligands have a certain affinity for biological tissues, which will cause unnecessary staining. In addition, these macromolecules will also disturb the labeled biomolecules, resulting in Artificial movement and alteration of protein-protein interactions in cells

Method used

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  • Porous silicon dioxide-stabilized noble metal cluster fluorescent material and method for preparing same
  • Porous silicon dioxide-stabilized noble metal cluster fluorescent material and method for preparing same
  • Porous silicon dioxide-stabilized noble metal cluster fluorescent material and method for preparing same

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Embodiment 1

[0032] Dissolve 10 g of Brij?58 in 50 mL of cyclohexane (toluene), stir and heat to 50°C, after complete dissolution, mix 0.45 mL of hydroxyethylethylenediamine with 1.5 mL of 0.5 chloroauric acid solution to form a Blood red, then add the solution to the microemulsion system, stir for 1 h, then add 0.2 g of NaBH 4 Restore the gold complex, stir and react for 50 minutes, the system turns black, then add 0.4 mL mercaptoethanol to complete the corrosion and stabilize the gold clusters, stir for 1 hour until the color of the system becomes colorless, adjust the pH of the reaction solution to 10.5 with ammonia water -12, drop 10 g of ethyl orthosilicate, and stir for 2 h. After centrifugation, washing, drying, roasting, electron microscope observation, such as figure 1 As shown, the gold clusters are uniformly dispersed in the spherical shell of silica, and the XPS analysis results of the material are as follows: figure 2 , indicating that gold is zero-valent, the excitation an...

Embodiment 2

[0035]Dissolve 10 g of Brij?58 in 50 mL of cyclohexane (dodecane), stir and heat to 50°C. After complete dissolution, mix 0.45 mL of ethanolamine with 1.5 mL of 0.5 silver nitrate solution, and the solution changes from cloudy to cloudy again. It is colorless and transparent, then add the solution into the microemulsion system, stir for 1 h, then add 0.2 g of NaBH 4 Restore the silver complex, stir for 50 minutes, the system turns black, then add 0.4 mL of thiodiglycol to complete the corrosion, and stabilize the silver clusters, stir for 1 hour, after the color of the system turns light brown, adjust the reaction with methylamine The pH value of the solution was 10.5-11, 10 g of ethyl orthosilicate was added dropwise, and the reaction was stirred for 2 h. After centrifugation, washing, drying, roasting, electron microscope observation, such as Figure 4 As shown, the silver clusters are uniformly dispersed in the spherical shell of silica, XPS analyzes the material, the resu...

Embodiment 3

[0038] Dissolve 10 g of Brij?58 in 50 mL of cyclohexane (octane), stir and heat to 50°C, after complete dissolution, mix 0.45 mL of ethanolamine with 1.5 mL of 0.3 mol / L chloroplatinic acid solution, and then The solution was added to the microemulsion system, stirred for 1 h, and then 0.2 g of NaBH 4 Restore the platinum complex, stir for 50 minutes and the system turns gray, then add 0.4 mL of mercaptoethanol (trihydroxyethylphosphine, trihydroxypropylphosphine) to complete the corrosion and stabilize the platinum clusters, stir for 1 hour, and when the color of the system is uniform, The pH value of the reaction solution was adjusted to 10.5-11 with ammonia water, 10 g of tetraethyl orthosilicate was added dropwise, and the reaction was stirred for 2 h. After centrifugation, washing, drying, roasting, electron microscope observation, such as Figure 7 As shown, platinum clusters are uniformly dispersed in spherical shells of silica.

[0039]

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Abstract

The invention provides a porous silicon dioxide-stabilized noble metal cluster fluorescent material and a method for preparing the same, and belongs to the technical field of preparing nano compound materials. The method for preparing the fluorescent material comprises the following steps of: corroding noble metal nano particles into noble metal clusters by a corrosion method, and stabilizing the noble metal clusters by a noble metal cluster stabilizer; performing the in situ stabilization of the noble metal clusters in a porous silicon dioxide structure by the hydrolysis of organic silicate ester, removing organic matters, performing hydrogen reduction to obtain the silicon dioxide-stabilized noble metal clusters, and conveniently preparing the porous silicon dioxide-stabilized noble metal cluster fluorescent material of Au, Ag, Pt, Pd and combination of double noble metals by adjusting the ligand, stabilizer and reaction conditions. Because the silicon dioxide is chemically and electrically inactive, the noble metal clusters show intrinsic fluorescence characteristics. The fluorescent material prepared by the method has stable fluorescence, chemical inertness and biocompatibility and is widely applied to fluorescence imaging and sensing.

Description

technical field [0001] The invention relates to a porous silicon dioxide-stabilized noble metal cluster fluorescent material and a preparation method thereof, belonging to the technical field of preparation of nanocomposite materials. Background technique [0002] Fluorescence sensing and imaging are widely used in scientific research, environmental monitoring and medical diagnosis due to their simple operation, intuitive information and high detection sensitivity. However, commonly used organic fluorescent dyes have the problem of photobleaching, which reduces the detection sensitivity and shortens the observation time; at the same time, large fluorescent markers will disturb the labeled biomolecules, causing artificial movement in cells and changes in protein-protein interactions . Although semiconductor quantum dots have improved photophysical properties such as minimal photobleaching, quantum dots are usually synthesized under harsh conditions, use toxic raw materials, ...

Claims

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Application Information

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IPC IPC(8): C09K11/58C09K11/87
Inventor 吕荣文邹伟
Owner DALIAN UNIV OF TECH
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