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Preparation method of multifunctional surface enhanced raman scattering (SERS) substrate

A surface-enhanced Raman and multi-functional technology, applied in the field of analysis and detection, can solve the problems of complex preparation process, waste of energy and resources, and inability to reuse, etc., and achieve the effect of small sample volume, real-time on-site detection, and convenient sampling

Inactive Publication Date: 2012-10-03
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Since the discovery of the SERS effect, various SERS substrates with Raman enhancement effects have been continuously prepared. SERS substrates with super Raman enhancement effects and easy access have always been a research hotspot. In recent years, various SERS substrates with different Topographically structured SERS substrates have been continuously produced by researchers, although the detection limit reaches 10 -12 -10 -14 M's SERS substrates have been reported by researchers, but the preparation process of these SERS substrates is complicated, the required equipment is expensive, and they cannot be reused, which will cause a waste of energy resources, and there is still a certain gap from practicality. exists in

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  • Preparation method of multifunctional surface enhanced raman scattering (SERS) substrate
  • Preparation method of multifunctional surface enhanced raman scattering (SERS) substrate
  • Preparation method of multifunctional surface enhanced raman scattering (SERS) substrate

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preparation example Construction

[0022] Such as figure 1 As shown, the multifunctional capillary surface-enhanced Raman substrate preparation method includes the following steps: A: A layer of ZnO seeds is generated on the inner wall of the capillary by thermal decomposition, and then the capillary is exposed to Zn(NO 3 ) 2 and HMT solutions to grow ZnO arrays; B: Transform ZnO arrays into TiO 2 array; C: on TiO 2 Nanotubes are decorated with silver particles.

[0023] figure 2 Conversion of ZnO arrays to TiO 2 Scanning electron microscope image of the array. It consists of four parts: A, B, C, and D. Among them, A: SEM images of zinc oxide nanorod arrays grown in a large area; B: SEM images of titanium dioxide nanotube arrays in a large area; C: A partial view of Figure A In the enlarged picture, we can see the array of zinc oxide nanorods neatly arranged; D: the partial enlarged picture of Figure B, we can see that the array of titanium dioxide nanotubes grows neatly on the inner wall of the capilla...

Embodiment 1

[0027] Building TiO on the inner wall of the capillary 2 Nanotube array:

[0028] First, let the ethanol solution of zinc acetate enter the inside of the capillary, dry it in an oven at 60 degrees Celsius, and then anneal it at 350 degrees Celsius for 20 minutes, so that a layer of zinc oxide seeds can be produced on the inner wall. Then, place the capillary in Zn(NO 3 ) 2 React with HMT solution at 90 degrees for 90 minutes to grow a layer of ZnO array on the inner wall. ZnO array in (NH 4 ) 2 TiF 6 and H 3 BO 3 Reacting in medium for 90 minutes, the titanium oxide nanotube array can be obtained. figure 2 A and C are SEM photos of zinc oxide arrays under different magnifications, respectively, and zinc oxide arrays distributed in a wide range can be seen; figure 2 B and D are SEM pictures of replacing zinc oxide with titanium oxide.

Embodiment 2

[0030] Silver particles modified on TiO 2 surface:

[0031] Immerse the capillary with the titanium oxide nanotube array in 0.05g / 20mL tin dichloride aqueous solution first, and rinse it with secondary water several times after one hour, so that a layer of divalent tin ions will be adsorbed on the surface of the titanium oxide. Then put it in the silver ammonia solution of 1mmol / L, take it out after 30 minutes and wash it, you can get the titanium oxide nanotube array modified by silver particles, as image 3 shown.

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Abstract

The invention provides a preparation method of a multifunctional surface enhanced raman scattering (SERS) substrate. The preparation method comprises the following steps of: firstly, paving a layer of ZnO seeds on the inner wall of a capillary, developing a ZnO nanorod array in Zn(NO3)2 and hexamethylenetetramine (HMT) solution, and soaking and reacting the capillary in solution of (NH4)2TiF6 and H3BO3, thus obtaining a TiO2 nanotube array; and soaking a nanotube in which TiO2 is grown into SnCl2 to ensure that a layer of bivalent tin ions are adsorbed on the surface layer of the nanotube, soaking the nanotube into Ag(NH3)2+ and reducing the nanotube to silver particles, thus obtaining the multifunctional SERS substrate. Compared with the conventional SERS substrate, the multifunctional SERS substrate based on the capillary has functions of raman enhancement and repeated use, is convenient to carry and sample, and can realize real-time field detection.

Description

technical field [0001] The invention relates to an analysis and detection technology, in particular to a surface-enhanced Raman spectrum detection method. Background technique [0002] Raman scattering was discovered by Indian scientist C.V. Raman in experiments in 1928, so this phenomenon is called Raman scattering, in short: when light passes through a transparent medium and is scattered by molecules, the frequency changes . Raman spectroscopy, like infrared spectroscopy, reflects the information of molecular vibration-rotational energy levels, but the signal of Raman scattering is very weak, and its intensity is only one millionth of the incident light intensity. Periods are not widely appreciated by the scientific community. Until 1974, after roughening the surface of a smooth silver electrode, Fleishmann et al. first obtained a high-quality Raman spectrum of a monolayer of pyridine molecules adsorbed on the surface of a silver electrode. Compared with the Raman scatt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 杨良保陈晋马永梅刘锦淮
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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