It is well known that WO(3) interacts efficiently with H(2) gas in the presence of noble metals (such as Pd, Pt and Au) at elevated temperatures, changing its optical behaviors; and that its crystallinity plays an important role in these interactions. For the first time, we investigated the in situ Raman spectra changes of WO(3) films of different crystal phases, while incorporating Pd catalysts, at elevated temperatures in the presence of H(2). The Pd/WO(3) films were prepared using RF sputtering and subsequently annealed at 300, 400 and 500 °C in air in order to alter the dominant crystal phase. The films were then characterized using SEM, XRD, XPS, and both UV-VIS and Raman spectroscopy. In order to fundamentally study the process, the measurements were conducted when films were interacting with 1% H(2) in synthetic air at elevated sample temperatures (20, 60, 100 and 140 °C). We suggest that the changes of Raman spectra under such conditions to be mainly a function of the crystal phase, transforming from monoclinic to a mix phase of monoclinic and orthorhombic achieved via increasing the annealing temperature. The as-deposited sample consistently shows similar Raman spectra responses at different operating conditions upon H(2) exposure. However, increasing the annealing temperature to 500 °C tunes the optimum H(2) response operating temperature to 60 °C.
Optical sensors based on surface plasmon resonance (SPR) are utilized for detecting toxic heavy metals in solutions. To improve the sensitivity of SPR sensors, nanostructured thin films with active layers can be synthesized. In this study, the response to Pb (II) was measured and compared for SPR sensors incorporating gold-chitosan-graphene oxide (Au/CS/GO) nanostructured thin films and Au/CS films. The characterization of Au/CS/GO using FESEM analysis revealed a film composed of nanosheets with wrinkled, rough surfaces. The results from XRD analysis confirmed the successful incorporation of GO in the prepared films. Additionally, AFM analysis determined that the Au/CS/GO films had a root mean square (rms) roughness of 28.38 nm and were considerably rougher than the Au/CS films. Upon exposure to a 5 ppm Pb (II) ion solution, the Au/CS/GO films exhibited higher SPR sensitivity, as much as 1.11200 ppm−1, than Au/CS films, 0.77600 ppm−1. This enhancement of the SPR response was attributed to strong covalent bonding between CS and GO in these films. These results indicated that the Au/CS/GO films show potential for the detection of heavy metal pollution in environmental applications.
We demonstrate the enhancement of surface plasmon resonance (SPR) technique by implementing a multi-metallic layers of Au-Ag-Au nanostructure in the chitosan-graphene oxide (CS-GO) SPR sensor for lead(II) ion detection. The performance of the sensor is analyzed via SPR measurements, from which the sensitivity, signal-to-noise ratio and repeatability are determined. The nanostructure layers are characterized using field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). We showed that the proposed structure has increased the shift in the SPR angle up to 3.5° within the range of 0.1-1 ppm due to the enhanced evanescent field at the sensing layer-analyte interface. This sensor also exhibits great repeatability which benefits from the stable multi-metallic nanostructure. The SNR value of 0.92 for 5 ppm lead(II) ion solution and reasonable linearity range up to that concentration shows that the tri-metallic CS-GO SPR sensor gives a good response towards the lead(II) ion solution. The CS-GO SPR sensor is also sensitive to at least a 10−5 change in the refractive index. The results prove that our proposed tri-metallic CS-GO SPR sensor demonstrates a strong performance and reliability for lead(II) ion detection in accordance with the standardized lead safety level for wastewater.
An etched tapered single mode optical fiber (SMF) coated with polyaniline (PANI) nanofibers is developed to detect ammonia (NH 3) in low concentrations. The SMF is etched with hydrofluoric acid and subsequently tapered using a glass processing workstation. The etched tapered SMF is coated with PANI via spray-coating deposition. This SMF modification significantly enhances the interaction of the evanescent field of the light propagating in the core with the PANI-sensing layer. The modified fiber sensor response is investigated by exposing the sensor to different concentrations of NH 3 over the C-band wavelengths of 1535-1565 nm. Integrating the modified optical fiber with the nanostructured PANI films produces highly sensitive optical sensor that operates at room temperature. The 50 µm etched tapered SMF coated with PANI produced response, recovery times, and sensitivity of 58 and 475 s, and 231.5%, respectively, in the C-band range. The limit of detection of the modified fiber sensor was 0.0025%, which is equal to 25 ppm. The developed sensor exhibits good repeatability, reversibility, and selectivity.
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