Method for assembling precious metal nanocrystalline on surface of conical fiber

A noble metal nanocrystal, tapered optical fiber technology, applied in the field of optical fiber, can solve the problems of limiting the sensitivity of detection of pollutants, unable to control the morphology of nanostructures, etc.

Active Publication Date: 2015-05-13
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The structure of the noble metal sensitive layer prepared by this method is stable, but the morphology of the nanostructure cannot be ad

Method used

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  • Method for assembling precious metal nanocrystalline on surface of conical fiber
  • Method for assembling precious metal nanocrystalline on surface of conical fiber
  • Method for assembling precious metal nanocrystalline on surface of conical fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) First put 48 mg of silver nitrate and 48 mg of polyvinylpyrrolidone in 3 mL of pentylene glycol, the mass ratio of the three is about 1:1:60, and stir at room temperature until completely dissolved, then 0.8-1.2mg / mL sodium chloride ethylene glycol solution is mixed with it evenly, so that the mass ratio of silver nitrate and sodium chloride is 400:1, and the pentylene glycol solution of silver nitrate and PVP-k29 is obtained;

[0056] Put 5 ml of pentanediol as a reaction precursor in a 50 ml round-bottomed flask at 150 o C in methyl silicone oil for 1 hour, the bottle mouth of the round bottom flask was covered with a rubber stopper with a through hole, and the stirring rate was maintained at 500 RPM. Then, the pentanediol solution of silver nitrate and PVP-k29 was injected with The pump injected at a rate of 600 μL / min to 140 o In 5 mL of pentylene glycol solvent at C, react for 3 hours. After the reaction, maintain the stirring rate of the reaction solution un...

Embodiment 2

[0062] (1) First prepare 10 g / L sodium citrate aqueous solution and 5 g / L chloroauric acid aqueous solution, then inject 1000 μL sodium citrate aqueous solution into 90 o C into 50 mL of water, and 200 μL of chloroauric acid was added dropwise. The round-bottomed flask used for the reaction was placed in a water bath to maintain the temperature. The entire reaction time was maintained for 30 minutes, and finally a sodium citrate-protected sodium citrate with a diameter of about 13 nm was obtained. Suspensions of negatively charged gold nanospheres;

[0063] (2) Strip off the coating layer at the end of the multimode fiber with a blade, insert it into 40 wt% hydrofluoric acid, seal it with methyl silicone oil, and use a puller to slowly pull the fiber vertically at a rate of 19.4 μm / min,;

[0064] When the silicon oxide at the end of the optical fiber is corroded by hydrofluoric acid, the end forms a tapered structure with a cone angle of 3.6 o ; The core diameter of the mul...

Embodiment 3

[0068] (1) Dissolve 0.01 M in 0.25 mL HAuCl 4 and 0.6 mL of NaBH at 0.01 M 4 Add to 9.75 mLCTAB of 0.1 M in sequence, and then stir for two minutes at a speed of 700-900 rpm under a magnetic stirrer. o The constant temperature water tank of C was left standing for two hours as a seed solution;

[0069] Next, add 0.01 M of 0.25 mL HAuCl 4 , 0.01 M in 0.4 mL of AgNO 3 and 0.8 mL of 1.0 M HCl were added to 40 mL of 0.1 M CTAB in sequence. At this time, the solution was light yellow. After shaking evenly, 0.32 mL of 0.1 M ascorbic acid AA was added, and the solution became colorless after shaking slightly for 30 seconds. Then add 0.096 mL of pre-prepared seed solution, shake slightly for 30 seconds, and place at 28 o Stand still in the constant temperature water tank of C for 12 hours, finally form the suspension of positively charged gold nanorods protected by CTAB;

[0070] (2) Strip the cladding layer at the end of the multimode fiber with a blade, insert it into 40 wt% hy...

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Abstract

The invention discloses a method for assembling precious metal nanocrystalline on the surface of conical fiber. According to the method, electrified precious metal nano particles are modified on the surface of a conical fiber probe according to an electrostatic absorption principle, and organic pollutants are detected according to an SERS (surface enhancement Raman scattering) effect. First, the positively charged or negatively charged precious metal nano particles such as gold, silver and the like as well as the fiber probe with a conical tail end are prepared, siliane coupling agents with exposed negatively charged or positively charged functional groups are modified on the surface of the conical fiber probe, the nano particles which are charged oppositely to the surface of the fiber and dispersed in a solvent are absorbed on the surface of the fiber according to the electrostatic absorption principle, accordingly, the variety, the morphology and the density of the assembled nano particles are controlled, and the taper angle of the tail end of the fiber is optimized. The method provides a new assembly concept for coupling of the nano particles and the fiber, is effective for preparation and optimization of high-performance fiber SERS probes, and lays a foundation for convenient, quick and online SERS detection of environmental pollutants.

Description

technical field [0001] The invention belongs to the field of optical fibers, in particular to a method for assembling noble metal nanocrystals on the surface of tapered optical fibers. Background technique [0002] The development of portable fiber-optic Raman spectrometers has enabled the in-situ and rapid SERS detection of trace pollutants in field water. There are two key issues in this optical fiber Raman SERS detection technology: one is to prepare noble metal nanostructures with high SERS activity; the other is to stably assemble the nanostructures with high SERS activity on the surface of fiber optic probes. For a long time, people have been unremittingly studying the method of combining noble metal nanostructures with high SERS sensitivity and fiber optic probes, expecting to achieve high reproducibility and high sensitivity response to pollutant molecules. There are three commonly used methods for sensitizing fiber optic probes: [0003] The first method is the li...

Claims

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Application Information

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IPC IPC(8): G01N21/65B22F9/24B82Y30/00B82Y40/00
Inventor 黄竹林孟国文毛庆和雷星刘晔汪志伟
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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