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Preparation and application of Raman enhancement substrates based on multi-layer composite structures

A multi-layer composite and Raman technology, applied in Raman scattering, measuring devices, instruments, etc., can solve the problems of slow growth rate, stability and uniformity of few-layer nanomaterials, poor uniformity and stability, etc. problems, to achieve the effect of simple and fast preparation method, excellent stability, and improved detection limit

Active Publication Date: 2019-11-05
GUANGDONG FOOD & DRUG VOCATIONAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Raman-enhanced scattering is a means of trace molecular detection, while gold and silver nanometer Raman-enhanced substrates are used in traditional processes, the process is complicated, the materials are expensive, and the uniformity and stability are not good.
Metal oxides can achieve sensitive Raman-enhanced detection through regulation, but because the traditional regulation method achieves enhancement by introducing material defects, its stability and uniformity cannot be guaranteed.
Recently developed two-dimensional nanomaterials have good uniformity, but their large-area preparation process is complicated, and many two-dimensional materials with high Raman enhancement effects, such as compounds such as sulfur, tellurium and selenium, are toxic and are not suitable for promotion
On the other hand, its enhancement effect is strongly related to the thickness, and its effect weakens rapidly with the increase of thickness, which brings great uncertainty to the actual application.
In addition, the growth rate of few-layer nanomaterials is slow, and there is currently no relevant method for large-scale production. Therefore, how to achieve simple and efficient preparation of sensitive and stable Raman-enhanced substrates is a key issue for practical applications.

Method used

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  • Preparation and application of Raman enhancement substrates based on multi-layer composite structures
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  • Preparation and application of Raman enhancement substrates based on multi-layer composite structures

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A method for preparing a Raman-enhanced substrate based on a multilayer composite structure, comprising the steps of:

[0046] A. On the quartz substrate 1, place several 2 substrates 2, a spacer 3 is placed on the upper surface of each substrate 2, and a spacer 3 with a cross-sectional area of ​​1×1 cm is placed on the upper surface of each spacer 3 2 The molybdenum sheet 4 obtained several composite laminates 5;

[0047] B. Preparation of molybdenum oxide substrate: Put the quartz substrate 1 with several composite laminates 5 into the heating equipment that has been preheated at 600°C for heat treatment, and react at a temperature of 600°C for 5 minutes; take out the quartz substrate 1, cooling, removing the spacer 3, and making a molybdenum oxide substrate;

[0048] C. Deploy SnCl 2 Solution: prepare SnCl with a concentration of 10nmol / L in a glass container 2 solution, and then to the SnCl 2 Dilute hydrochloric acid was added dropwise to the solution to adjust...

Embodiment 2

[0056] A method for applying a Raman-enhanced substrate based on a multilayer composite structure, comprising the steps of:

[0057] Step (1): Take the R6G molecule, dissolve it in deionized water, and prepare a concentration of 4×10 -6 M's R6G molecular solution;

[0058] Step (2): Place the Raman-enhanced substrate based on the multilayer composite structure prepared in Example 2 on step (1) 4×10 -6 In the R6G molecular solution of M, place it for 20 minutes, then take it out, dry the surface, and obtain the sample to be tested;

[0059] Step (3): Using a micro-Raman spectrometer with an excitation light wavelength range of 514nm, a 50x eyepiece, an excitation light intensity of 0.625mW, and an integration time of 10s, measure the R6G molecule at 1100cm -1 -1700cm -1 The characteristic vibration; and with the same thickness (100nm) of pure molybdenum oxide for 4×10 -6 Raman enhancement effect of the R6G molecular solution of M.

Embodiment 3

[0063] A method for applying a Raman-enhanced substrate based on a multilayer composite structure, comprising the steps of:

[0064] Step (1): Take MB molecules, dissolve them in deionized water, and prepare the concentration to be 4×10 -3 M, 4×10 -4 M, 4×10 -5 M, 4×10 -6 M, 4×10 -7 M, 1×10 -7 M, 6×10 -8 M, 2×10 -8 MB molecular solution of M;

[0065] Step (2): The Raman-enhanced substrates based on the multi-layer composite structure prepared in Example 2 were respectively placed in step (1) with a concentration of 4×10 -3 M, 4×10 -4 M, 4×10 -5 M, 4×10 -6 M, 4×10 -7 M, 1×10 -7 M, 6×10 -8 M, 2×10 -8 In the MB molecular solution of M, place it for 20 minutes, then take it out, dry the surface, and obtain the sample to be tested;

[0066] Step (3): Using a micro-Raman spectrometer with an excitation light wavelength range of 633nm, a 50x eyepiece, an excitation light intensity of 0.945mW, and an integration time of 10s, measure the MB molecule at 1100cm -1 -1700c...

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Abstract

The invention relates to the technical field of trace molecule detection, in particular to preparation and application of Raman enhancement substrates based on multi-layer composite structures. The preparation method comprises the following steps that multiple substrates are placed on a quartz baseplate, an insulation part and a molybdenum sheet are placed on the upper surface of each substrate insequence, and the substrates are placed in pre-heated heating equipment for a thermal reaction; the substrates are taken out and cooled, the insulation parts are removed, and molybdenum oxide substrates are prepared; a SnCl2 solution with the concentration of 10 nmol / L is prepared, and the pH value of the SnCl2 solution is adjusted to 5-6; the prepared molybdenum oxide substrates are placed in the SnCl2 solution, placed in a pre-heated heating table for Sn ion interlayer intercalation, taken out and blow-dried through a nitrogen gun, and the Raman enhancement substrates based on the multi-layer composite structures are prepared. The preparation method is easy and quick to implement, an intralayer structure of molybdenum oxide is not changed, by introducing interlayer ions, doping is achieved, and the prepared substrates are stable in quality and high in sensitivity.

Description

technical field [0001] The invention relates to the technical field of trace molecule detection, in particular to the preparation and application of a Raman enhanced substrate based on a multilayer composite structure. Background technique [0002] Raman-enhanced scattering is a means of detecting trace molecules, while gold and silver nanometer Raman-enhanced substrates are used in traditional processes, the process is complicated, the materials are expensive, and the uniformity and stability are not good. Metal oxides can achieve sensitive Raman-enhanced detection through regulation, but because traditional regulation methods achieve enhancement by introducing material defects, their stability and uniformity cannot be guaranteed. Recently developed two-dimensional nanomaterials have good uniformity, but their large-area preparation process is complicated. At the same time, many two-dimensional materials with high Raman enhancement effects, such as compounds such as sulfur,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 陈秋兰陈建刘虔铖金浩宇
Owner GUANGDONG FOOD & DRUG VOCATIONAL COLLEGE
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