RESUMO
In this work, nanostructures comprising silver nanoparticles supported on a wrinkled chitosan matrix (Ag@Ch) were successfully synthesized by a simple aging process at room temperature for four days through self-assembly. Chitosan, a natural polysaccharide was used as a support as well as a reducing agent for the formation of Ag nanostructures and the creation of hotspots for SERS activity. The fabricated Ag@Ch nanostructures were characterized by several spectroscopic techniques and were used as a surface-enhanced Raman scattering (SERS) substrate. The effect of wet, dry, and liquid samples on the SERS enhancement has been studied and was found to be effective for sensing Methylene blue, Crystal Violet, and p-Nitrophenol with detection limits of 3.8, 8.1, and 8.2 ppb respectively. The SERS enhancement of the Ag@Ch was attributed to the combination of both electromagnetic (EM) and chemical effects (CE). Density functional theory (DFT) calculations were used to explain the observed surface enhancement. Good agreement was observed between the experimental and simulated spectra.
Assuntos
Quitosana , Nanopartículas Metálicas , Nanoestruturas , Análise Espectral Raman/métodos , Prata/química , Nanopartículas Metálicas/química , Teoria da Densidade Funcional , Nanoestruturas/químicaRESUMO
This work describes the preparation of palladium-based catalyst supported on magnetic chitosan (Pd@IO-Chitosan) for Suzuki Miyaura C-C coupling reaction. The Pd@IO-Chitosan catalyst was characterized using different spectroscopic and microscopic techniques such as Fourier transform infrared spectroscopy (FT-IR), transmission electron microscope (TEM), vibrating sample magnetometer (VSM), X-ray powder diffraction (XRD), X-ray Absorption Near Edge Structure (XANES) Spectroscopy and X-ray photoelectron spectroscopy (XPS). Pd@IO-Chitosan was further analysed by thermogravimetric analysis (TGA) in order to determine its thermal behavior. The catalyst comprised Pd, PdO species stabilised by chitosan that facilitated Suzuki coupling reactions. Palladium loading as low as 0.0055 mol% was found to be effective for aqueous Suzuki cross-couplings with excellent yields of over 99%. The catalyst could be recycled and reused at least 12 times with no significant decrease in its catalytic activity.