RESUMO
A high-temperature, high-pressure, pulsed-gas sampling and detection system has been developed for testing new catalytic and photocatalytic materials for the production of solar fuels. The reactor is fitted with a sapphire window to allow the irradiation of photocatalytic samples from a lamp or solar simulator light source. The reactor has a volume of only 3.80 ml allowing for the investigation of very small quantities of a catalytic material, down to 1 mg. The stainless steel construction allows the cell to be heated to 350 °C and can withstand pressures up to 27 bar, limited only by the sapphire window. High-pressure sampling is made possible by a computer controlled pulsed valve that delivers precise gas flow, enabling catalytic reactions to be monitored across a wide range of pressures. A residual gas analyser mass spectrometer forms a part of the detection system, which is able to provide a rapid, real-time analysis of the gas composition within the photocatalytic reaction chamber. This apparatus is ideal for investigating a number of industrially relevant reactions including photocatalytic water splitting and CO2 reduction. Initial catalytic results using Pt-doped and Ru nanoparticle-doped TiO2 as benchmark experiments are presented.
RESUMO
Understanding the mechanism for growing TiO(2) nanotubes is important for controlling the nanostructures. The hydroxide nano-islands on the Ti surface play a significant role at the initial stage of anodization by forming the very first nano-pores at the interface between hydroxide islands and substrate and eliminating the H(2)O electrolysis. A quantitative time dependent SEM study has revealed a nanotube growth process with an initial linear increase of pore diameter, film thickness and number of pores. During the anodization of titanium, different current transient curves are observed for Ti samples with or without hydroxide on the surface. The transient current profile has been quantitatively analyzed by fitting several distinctive stages based on a growth mechanism supported by SEM observations. It is found that a saturated cubic dependent equation is appropriate to fit a short current upturn due to the increase of the surface area.