Ordered mesoporous silicon-dioxide-substrate fluorescence nanometer material and preparing method thereof

A technology of fluorescent nanomaterials and mesoporous silica, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of uneven dispersion of fluorescent groups, susceptibility to environmental erosion, low fluorescence quantum yield, etc., and achieve synthesis Simple and easy process, good fluorescence stability, high fluorescence quantum yield effect

Inactive Publication Date: 2009-09-09
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages are: (1) complex process; (2) low post-grafting efficiency; (3) uneven dispersion of fluorescent groups; (4) low fluorescence quantum yield and poor fluore

Method used

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  • Ordered mesoporous silicon-dioxide-substrate fluorescence nanometer material and preparing method thereof
  • Ordered mesoporous silicon-dioxide-substrate fluorescence nanometer material and preparing method thereof
  • Ordered mesoporous silicon-dioxide-substrate fluorescence nanometer material and preparing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] First, with Rhodamine B (RhB) and aminopropyltriethoxysilane (APTES) as raw materials, dry N, N-dimethylformamide (DMF) as solvent, 1-ethyl-(3 -Dimethylaminopropyl) carbodiimide hydrochloride (EDC·HCl) as catalyst and dehydrating agent, stirred in anhydrous and light-proof environment for 24 hours, prepared silane coupling agent with RhB fluorescent functional group (RhB-APTES).

[0034] 1.2gP123 and 0.4gZrOCl 2 ·8H 2Add O together to 100mL 2mol / L hydrochloric acid solution, stir at 35°C to dissolve completely, and then add 0.02gRhB-APTES to the system. Add 2.1g TEOS after 30 minutes, continue stirring for 24 hours, then centrifuge and wash. Finally, it was refluxed for 6 hours in 250 mL of ethanol solution of hydrochloric acid (0.5% by volume), centrifuged and dried. The obtained ordered mesoporous silica-based fluorescent nanomaterial has an average particle diameter of 400nm, an average pore diameter of 4.8nm, and a pore volume of 0.7cm 3 g -1 , BET specific su...

Embodiment 2

[0036] Firstly, RhB and APTES were used as raw materials, dry DMF was used as solvent, EDC·HCl was used as catalyst and dehydrating agent, and the silane coupling agent RhB- APTES.

[0037] 1.2gP123 and 0.8gZrOCl 2 ·8H 2 Add O together into 100mL 2mol / L hydrochloric acid solution, stir at 35°C to dissolve completely, and then add 0.4gRhB-APTES to the system. After 30 minutes, add 2 g of methyl orthosilicate, continue to stir for 24 hours, then centrifuge and wash. Finally, it was refluxed for 6 hours in 250 mL of ethanol solution of hydrochloric acid (0.5% by volume), centrifuged and dried. The obtained ordered mesoporous silica-based fluorescent nanomaterial has an average particle size of 200 nm, an average pore size of 4.8 nm, and a pore volume of 0.7 cm 3 g -1 , BET specific surface area is 700m 2 g -1 . The grafting rate of the obtained ordered mesoporous silica-based fluorescent nanomaterial is 0.13 RhB functional groups / nm -2 , the fluorescence quantum yield is...

Embodiment 3

[0039] Firstly, using fluorescein isothiocyanate (FITC) and aminopropyltrimethoxysilane (APTMS) as raw materials, using absolute ethanol as solvent, stirring in anhydrous and light-proof environment for 24 hours, prepared the fluorescent functional group with FITC Silane coupling agent (FITC-APTMS).

[0040] 1gF127 and 1gZnCl 2 Add together 100mL 2mol / L hydrochloric acid solution, stir at 38°C to dissolve completely, then add 0.5g FITC-APTMS to the system. Add 2.1g TEOS after 30 minutes, continue stirring for 24 hours, then centrifuge and wash. Finally, it was refluxed for 6 hours in 250 mL of ethanol solution of hydrochloric acid (0.5% by volume), centrifuged and dried. The obtained ordered mesoporous silica-based fluorescent nanomaterials have an average particle diameter of 350 nm, an average pore diameter of 5 nm, and a pore volume of 0.8 cm 3 g -1 , BET specific surface area is 680m 2 g -1 . The obtained ordered mesoporous silica-based fluorescent nanomaterials hav...

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Abstract

The invention relates to an ordered mesoporous silicon-dioxide-substrate fluorescence nanometer material and a preparing method thereof, which belong to the technical field of fluorescence nanometer materials of mesoporous molecular sieves. The ordered mesoporous silicon-dioxide-substrate fluorescence nanometer material is characterized by having the aperture size of 3 to 30 nm, the hole capacitance of higher than 0.5cm<3>/g<-1> and the specific area of larger than 500 m<2>/g<-1>, and the organic fluorescence molecules are grafted on the internal wall of the hole passage of the ordered mesoporous silicon-dioxide substrate in a mono-disperse and covalent way. The fluorescence material of the invention prepared by grafting the organic fluorescence functional groups on the ordered mesoporoussilicon-dioxide substrate in a mono-disperse and covalent way has high grafting rate (can be as high as 0.2 fluorescence functional group/nm<-2>), high fluorescence quantum rate (higher than 80 percent) and excellent optical stability.

Description

technical field [0001] The invention relates to an ordered mesoporous silica-based fluorescent nanomaterial and a preparation method thereof, belonging to the technical field of mesoporous molecular sieve fluorescent nanomaterials. Background technique [0002] Since Mobil Corporation synthesized mesoporous molecular sieves for the first time in 1992, mesoporous materials have attracted great attention in the fields of drug loading, catalysis, microreactors, adsorption, separation, chromatography, and optics. Using CTAB plasma surfactant as a structure-directing agent, the technology of synthesizing ordered mesoporous silica nanomaterials with controlled morphology has been very mature. Although the pore size is easily controlled by using pore expanders and nonionic surfactants, the controlled synthesis of ordered mesoporous silica nanomaterials with large pore sizes (greater than 3 nm) is difficult. Nanoscale ordered mesoporous silica particles with large pore sizes are pa...

Claims

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Application Information

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IPC IPC(8): C09K11/06C09K11/59
Inventor 何前军施剑林陈雨崔方明
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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