RESUMO
Zinc oxide (ZnO) nanorod thin films were prepared by CBD onto glass and FTO/glass substrates. Silver (Ag) nanoparticles were synthesized on the surface of the prepared ZnO nanorod thin films using electrochemical methods. The scanning electron microscopy images of the Ag/ZnO/glass core/shell nanostructure confirmed that the average particles size is 20 nm while it was 41 nm for Ag NPs that synthesized onto ZnO/FTO NRs. The photocatalytic activity of the prepared Ag/ZnO core/shell nanostructure was studied by analyzing the degradation of methylene blue (MB) dye under visible light. Various pH values (6 and 10) and exposure time (30-240) min were controlled to investigate the photocatalytic activity of as-prepared Ag/ZnO core/shell nanostructure and that annealed at 200 °C and 300 °C for 1 h. It was observed that when the pH was 6, the degradation rate increased with the annealing temperature and irradiation time reaching 51% at the annealing temperature of 300 °C and exposure time of 240 min. In other hands, when the pH was 10, and the sample was annealed at 200 °C, it showed a good degradation rate of 100% at the irradiation time of 90 min. By contrast, the sample annealed at 300 °C required 180 min to degrade the MB dye completely. The photoelectrochemical cell measurement based on photocurrent density revealed a slight response to light. Cycle voltammetry (CV) measurement was conducted, and the CV curves of the Ag/ZnO core/shell electrodes indicated nonfaradaic and pseudocapacitance behavior. The electrodes showed nearly rectangular CV curves, which indicated the dominance of the nonfaradaic capacitance behavior. The specific capacitance of the electrodes remained at approximately 99%. Mott-Schottky analysis revealed that the semiconductor was an n-type with dependence on flat band potential V FB deviation in the negative direction.
RESUMO
Scanning electron microscopy (SEM) of nanoscale objects in dry and fully hydrated conditions at different temperatures is of critical importance in revealing details of their interactions with an ambient environment. Currently available WETSEM capsules are equipped with thin electron-transparent membranes and allow imaging of samples at atmospheric pressure, but do not provide temperature control over the sample. Here, we developed and tested a thermoelectric cooling/heating setup for WETSEM capsules to allow ambient pressure in situ SEM studies with a temperature range between -15 and 100°C in gaseous, liquid, and frozen conditions. The design of the setup also allows for correlation of the SEM with optical microscopy and spectroscopy. As a demonstration of the possibilities of the developed approach, we performed real-time in situ microscopy studies of water condensation on a surface of Morpho sulkowskyi butterfly wing scales. We observed that initial water nucleation takes place on top of the scale ridges. These results confirmed earlier discovery of a preexisting polarity gradient of the ridges of Morpho butterflies. Our developed thermoelectric cooling/heating setup for environmental capsules meets the diverse needs for in situ nanocharacterization in material science, catalysis, microelectronics, chemistry, and biology.
