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Dandelion-like Ag/WO3-x micro-nanostructured composite material-based SERS substrate, and preparation method and application thereof

A micro-nano structure, dandelion-like technology, applied in the field of cleaning SERS substrates, can solve the problem of easy re-contamination of the surface, and achieve the effects of high yield, mild reaction conditions, and highly sensitive SERS analysis and detection.

Active Publication Date: 2017-03-22
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Plasma bombardment or sputtering in a vacuum environment requires expensive vacuum equipment, and the cleaned surface is prone to recontamination, etc.

Method used

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  • Dandelion-like Ag/WO3-x micro-nanostructured composite material-based SERS substrate, and preparation method and application thereof
  • Dandelion-like Ag/WO3-x micro-nanostructured composite material-based SERS substrate, and preparation method and application thereof
  • Dandelion-like Ag/WO3-x micro-nanostructured composite material-based SERS substrate, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0034] The invention provides a SERS substrate based on a three-dimensional bionic micro-nano structure for pesticide residue detection and a construction method thereof. The SERS substrate has the advantages of clean surface and recyclability. First, the present invention proposes a method for preparing dandelion-like Ag / WO 3-x (0 2.72 Micro-nano structure (i.e. dandelion-like WO 2.72 Micro-nano prickles) hydrothermal reaction (see figure 1 ); (2), the WO 2.72 In-situ reduction of silver nanoparticles on the surface of micro-nano structures. Then the dandelion-like Ag / WO prepared by self-assembly on the surface of the solid substrate by spin coating method 3-x (0 3-x (0 <x <0.28) Composite SERS substrate.

[0035] Dandelion-shaped Ag / WO 3-x (0 <x <0.28) The preparation method of micro / nano structure is:

[0036] (1) Tungsten hexachloride (WCl 6 ) Is the precursor, which is fully dissolved in absolute ethanol and transferred to a hydrothermal reactor. After reacting at 180°C for 2...

Embodiment 2

[0050] 1) Put 1.6g of WCl 6 The solid powder was added to 100mL of absolute ethanol and fully stirred until it was completely dissolved (molar concentration is about 0.04M), and then quickly transferred to a 100mL hydrothermal reactor; the sealed hydrothermal reactor was placed in a vacuum oven, Increase the temperature from room temperature to 160°C at a rate of 10°C / min, then keep it warm for 12 hours, and cool to room temperature naturally after the completion of the heat preservation;

[0051] 2) Open the hydrothermal reactor, separate the obtained precipitate by vacuum filtration, and rinse the precipitate 3 times with deionized water and absolute ethanol, and then vacuum dry at 60°C for 4 hours. The resulting powder is Stoichiometric Dandelion-like WO 2.72 Micro-nano structure, spare;

[0052] 3) Combine 0.6g of prepared dandelion-like WO 2.72 The micro-nano structure was added to 120mL of deionized water to obtain a suspension. Then, at room temperature, a 0.1M silver nitrat...

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Abstract

The invention provides a dandelion-like Ag / WO3-x micro-nanostructured composite material-based SERS substrate, and a preparation method and an application thereof. The preparation method comprises the following steps: carrying out a hydrothermal reaction on WCl6 and anhydrous ethanol to prepare a dandelion-like WO2.72 acanthosphere structure, and loading high-density silver nanoparticles onto the surface of the dandelion-like WO2.72 acanthosphere by using the weak reductibility of WO2.72 and using silver nitrate as an oxidant in order to obtain a dandelion-like Ag / WO3-x micro-nanostructure; and spin-coating the Ag / WO3-x micro-nanostructure on the surface of a solid-phase substrate, and carrying out self assembling to obtain the SERS substrate. The preparation method has the advantages of simplicity, mild conditions, no large devices, and high yield, and is suitable for industrial production; and the prepared dandelion-like Ag / WO3-x micro-nanostructure has a unique three-dimensional structure, and allows the recyclable SERS substrate with clean surface to be obtained, so the SERS substrate has wide application prospect in the fields of SERS detection, catalysis and sensing.

Description

Technical field [0001] The invention relates to a recyclable clean SERS substrate, in particular to a dandelion-like Ag / WO 3-x (0 <x <0.28) SERS substrate of micro-nano structure composite material and its preparation method and its application in pesticide residue detection. Background technique [0002] The rapid development of agricultural industrialization has made the production of agricultural products increasingly dependent on foreign substances such as pesticides, antibiotics and hormones. However, the unreasonable use of various pesticides will inevitably cause pesticide residues in agricultural products to exceed the safe range and seriously affect food safety. At present, there are many kinds of rapid detection methods for pesticide residues. According to their principles, they are mainly divided into biochemical analysis methods, chromatographic detection methods, and spectral analysis methods. Among them, Surface-enhanced Raman Scattering (SERS) based on Raman...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 赵永席黄剑马大衍徐可为陈锋
Owner XI AN JIAOTONG UNIV
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