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In This Article

  • Summary
  • Abstract
  • Introduction
  • Protocol
  • Representative Results
  • Discussion
  • Acknowledgements
  • Materials
  • References
  • Reprints and Permissions

Summary

This protocol describes a fabrication method for a flexible substrate for surface-enhanced Raman scattering. This method has been used in the successful detection of low concentrations of R6G and Thiram.

Abstract

This article presents a fabrication method for a flexible substrate designed for Surface-Enhanced Raman Scattering (SERS). Silver nanoparticles (AgNPs) were synthesized through a complexation reaction involving silver nitrate (AgNO3) and ammonia, followed by reduction using glucose. The resulting AgNPs exhibited a uniform size distribution ranging from 20 nm to 50 nm. Subsequently, 3-aminopropyl triethoxysilane (APTES) was employed to modify a PDMS substrate that had been surface-treated with oxygen plasma. This process facilitated the self-assembly of AgNPs onto the substrate. A systematic evaluation of the impact of various experimental conditions on substrate performance led to the development of a SERS substrate with excellent performance and an Enhanced Factor (EF). Utilizing this substrate, impressive detection limits of 10-10 M for R6G (Rhodamine 6G) and 10-8 M for Thiram were achieved. The substrate was successfully employed for detecting pesticide residues on apples, yielding highly satisfactory results. The flexible SERS substrate demonstrates great potential for real-world applications, including detection in complex scenarios.

Introduction

Surface-Enhanced Raman Scattering (SERS), as a type of Raman scattering, offers the advantages of high sensitivity and gentle detection conditions, and can even achieve single molecule detection1,2,3,4. Metal nanostructures, such as gold and silver, are typically used as SERS substrates to enable substance detection5,6. Electromagnetic coupling enhancement on nanostructured surfaces plays a significant role in SERS applications. Metallic nanostructures with varying sizes, shapes, int....

Protocol

1. Synthesis of nanoparticles

  1. Preparation of Silver nitrate solution
    1. Using a precision weighing balance, measure 0.0017 g of AR-grade silver nitrate (AgNO3, see Table of Materials) and add it to 10 mL of deionized (DI) water. Stir the mixture to create a 10-3 mol/L AgNO3 solution.
  2. Preparation of the silver-ammonia complex
    1. Take 1 mL of AR-grade ammonia water (NH3.H2O, see

Representative Results

In this study, a flexible SERS substrate composed of synthetic AgNPs wrapped in glucose and self-assembled on PDMS using APTES was developed, achieving excellent detection performance for practical pesticide detection applications. The detection limits for R6G and Thiram were both reached at 10-10 M and 10-8 M, respectively, with an Enhancement Factor (EF) of 1 x 105. Furthermore, the substrate demonstrated uniformity.

The AgNPs wrapped in glucose were synthesi.......

Discussion

In this study, a flexible SERS substrate was introduced, which bonded AgNPs to PDMS through chemical modification and achieved excellent performance. During particle synthesis, specifically in the silver ammonia complex synthesis (step 1.2), the color of the solution plays a crucial role. Adding too much ammonia water dropwise can adversely affect AgNPs synthesis quality, potentially leading to unsuccessful detection results. Attention should be paid to substrate modification (step 2.2) during the synthesis process; othe.......

Acknowledgements

The research is supported by the National Natural Science Foundation of China (Grant No. 61974004 and 61931018), as well as the National Key R&D Program of China (Grant No. 2021YFB3200100). The study acknowledges the Electron Microscopy Laboratory of Peking University for providing access to electron microscopes. Additionally, the research extends thanks to Ying Cui and the School of Earth and Space Science of Peking University for their assistance in Raman measurements.

....

Materials

NameCompanyCatalog NumberComments
Ammonia (NH3.H2O, 25%)Beijing Chemical Works
APTES (98%)BeyotimeST1087
BD-20AC Laboratory Chrona TreaterElectro-Technic Products Inc.12051A
D-glucoseBeijing Chemical Works
Environmental Scanning electron microscope (ESEM)FEIQUANTA 250
Raman microscopeHoriba JYLabRAM HR Evolution
Rhodamine 6GBeijing Chemical Works
Silicone Elastomer Base and Silicone Elastomer Curing AgentDow Corning CorporationSYLGARD 184
Silver nitrateBeijing Chemical Works
Thiram (C6H12N2S2, 99.9%)Beijing Chemical Works

References

  1. Zheng, F., Ke, W., Shi, L., Liu, H., Zhao, Y. Plasmonic Au-Ag janus nanoparticle engineered ratiometric surface-enhanced Raman scattering aptasensor for ochratoxin A detection. Analytical Chemistry. 91 (18), 11812-11820 (2019).
  2. Zhou, L., et al.

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Polydimethylsiloxane PDMSSurface enhanced Raman Scattering SERSSilver Nanoparticles AgNPs3 aminopropyl Triethoxysilane APTESRhodamine 6G R6GThiramPesticide DetectionFlexible SubstrateEnhanced Factor EFSensitive Detection

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