Method for preparing silver sulfide nanocrystalline with near infrared fluorescence using one-step aqueous phase process

A near-infrared and nanocrystal technology, applied in the field of near-infrared fluorescent nanomaterials, can solve the problem that nanocrystals can only be dispersed in organic solvents, and achieve good optical properties and water solubility, good fluorescence emission, and good repeatability.

Active Publication Date: 2012-10-10
JILIN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the reported synthetic Ag 2 S nanomaterials mainly rely on the high-temperature pyrolysis precursor method (J.Am.Chem.Soc., 2010, 132, 1470-1471), which relies on high-temperature reactions and requires the use of long-chain stabilizers, resulting in nanocrystalline Can only be dispersed in organic solvents

Method used

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  • Method for preparing silver sulfide nanocrystalline with near infrared fluorescence using one-step aqueous phase process
  • Method for preparing silver sulfide nanocrystalline with near infrared fluorescence using one-step aqueous phase process
  • Method for preparing silver sulfide nanocrystalline with near infrared fluorescence using one-step aqueous phase process

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Experimental program
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Embodiment 1

[0016] AgNO at a concentration of 10mmol / L in 10ml 3 Add 10ml of the same equimolar concentration of glutathione compound containing thiol to the aqueous solution, and stir evenly. Then add 1ml, 0.6mol / L thiohydrazine complex (the product of solid sulfur powder reduced by hydrazine hydrate) as a sulfur source, stir at room temperature for 4 hours to obtain a reddish-brown solution; then add 60ml of ethanol as a precipitant, centrifuge after precipitation, and obtain The solid sample is Ag 2 S nanocrystals, redisperse it into 10ml water, its concentration is 10mmol / L, apply to aspects such as cell fluorescent labeling and fluorescence imaging, will 50 microliters above-mentioned Ag 2 The S nanocrystal solution was added to the MC3T3-E1 cell solution, incubated, and tested by laser confocal microscopy.

Embodiment 2

[0018] Ag with different fluorescence emission 2 Preparation of S nanocrystals, select glutathione, CH 3 COOAg and sulfurized amine were used as stabilizer, Ag source and sulfur source respectively. Add different proportions of reactants (50mmol glutathione, 10mmol CH 3 COOAg, 0.4ml 0.6mol / L amine sulfide; 25mmol glutathione, 10mmol CH 3 COOAg, 0.4ml 0.6mol / L amine sulfide; 10mmol glutathione, 10mmol CH 3 COOAg, 0.4ml 0.6mol / L amine sulfide; 10mmol glutathione, 10mmol CH 3 COOAg, 1.0ml 0.6mol / L sulfide amine) stirred at room temperature for 4h, respectively added 60ml ethanol as a precipitant, centrifuged after precipitation, the obtained solid sample was Ag 2 S nanocrystals, redisperse it in 10ml water to get Ag with tunable fluorescence 2 S nanocrystals (marked as S1, S2, S3, S4 respectively; S1 size 1.7nm, fluorescence emission peak position 627nm; S2 size 2.1nm, fluorescence emission peak position 652nm; S3 size 3.0nm, fluorescence emission peak position 688nm; S4 siz...

Embodiment 3

[0020] AgClO containing 5mmol / L in 10ml 4 In the aqueous solution, add 10ml, 25mmol / L mercapto-containing thioglycolic acid compound, and stir evenly. Then add 1ml of 0.5mol / L sodium sulfide as a sulfur source, and react at room temperature for 2 hours to obtain a reddish-brown solution; then add 50ml of ethanol as a precipitant, centrifuge after precipitation, and the resulting solid sample is Ag 2 S nanocrystals. It was redispersed into 10ml of water with a concentration of 5mmol / L, and it was applied to the aspects of cell fluorescence labeling and fluorescence imaging.

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Abstract

The invention belongs to the technical field of near infrared fluorescent nano materials, and particularly relates to a method for preparing Ag2S nanocrystalline with near infrared fluorescence using one-step aqueous phase process. The method includes: adding water-soluble sulfur source into silver ion solution, and using water-soluble sulfhydryl compound as stabilizer to prepare the water-soluble Ag2S nanocrystalline at one step under room temperature. The nanocrystalline prepared by the method has the advantages that size of the nanocrystalline can be controllably synthesized in a range of 0.5nm-10nm, particle size is uniform, controllable fluorescence emission of the nanocrystalline is fine, and emission peak positions can be controlled from a red region to a near infrared region (from 650nm to 900nm). Due to the fact that the water-soluble sulfhydryl compound is used as the stabilizer, environmental pollution is low, product purity is high, and fine optical property and water solubility are revealed. In addition, the method for preparing silver sulfide nanocrystalline with near infrared fluorescence is simple, mild in conditions, easy to operate, fine in repeatability and suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of near-infrared fluorescent nanomaterials, in particular to a one-step aqueous method for preparing Ag with near-infrared fluorescent properties. 2 S nanocrystal method. Background technique [0002] Near-infrared nano-fluorescent material refers to a new type of material whose emission area is between 650nm and 900nm. Light in this region has good permeability in organisms, so it has high application value in the field of live cell imaging. At present, although various near-infrared materials synthesized by many routes have been reported, such as PbS (Small., 2011, 7, 2250.), CdHgTe (Chem. Mater., 2008, 20, 6764-6769), Cd 3 P 2 (J.Am.Chem.Soc., 2010, 132, 5613-5615), but the disadvantage of these materials is that heavy metals are highly toxic and can only be dispersed in organic solvents. These conditions limit the use of these near-infrared materials on organisms. Applications. [0003] Ag 2 S nano...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G5/00C09K11/58
Inventor 林权王传洗徐琳马骋孙源卿杨柏崔占臣董凤霞
Owner JILIN UNIV
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