Claude R. Henry

The best current way to prepare Au/TiO2 catalysts is the method of deposition−precipitation with NaOH (DP NaOH) developed by Haruta and co-workers. With this method, it is possible to obtain small gold metal particles (2−3 nm), but the corresponding gold loading remains rather low (∼3 wt %). The main goal of this work is to investigate other methods of preparation of Au/TiO2 catalysts to obtain small gold metal particles (2−3 nm) and a higher Au loading. It is shown that anion adsorption with AuCl4- (AA) does not produce Au loading higher than 1.5 wt % and the average particle size is not very small (∼4 nm). Cation adsorption with Au(en)23+ (CA) leads to small particles (2 nm) when the solution/support contact time is moderate (1 h), but the Au loading does not exceed 2 wt %. The most promising method of preparation appears to be deposition−precipitation with urea (DP urea). Indeed, samples with gold particles as small as those obtained with DP NaOH (∼2 nm) can be prepared, and all gold in solution is deposited on TiO2 in contrast to DP NaOH. The DP urea samples reported in this paper can reach a Au loading as high as 8 wt % using a TiO2 support with a surface area of 45 m2 g-1. The possible mechanisms of deposition of gold on the TiO2 support by the different methods of preparation are discussed.

One challenge in the production of nanometer-sized objects with given properties is to control their growth at a macroscopic scale in situ and in real time. A dedicated ultrahigh-vacuum grazing-incidence small-angle x-ray scattering setup has been developed, yielding high sensitivity and dynamics. Its capabilities to derive the average particle shape and size and the film growth mode and ordering and to probe both surfaces and buried interfaces are illustrated for two prototypical cases: the model catalyst Pd/MgO(100) and the self-organized Co/Au(111) system. A wide range of technologically important systems can potentially be investigated in various gaseous environments.

The current status and future prospects of non-contact atomic force microscopy (nc-AFM) and Kelvin probe force microscopy (KPFM) for studying insulating surfaces and thin insulating films in high resolution are discussed. The rapid development of these techniques and their use in combination with other scanning probe microscopy methods over the last few years has made them increasingly relevant for studying, controlling, and functionalizing the surfaces of many key materials. After introducing the instruments and the basic terminology associated with them, state-of-the-art experimental and theoretical studies of insulating surfaces and thin films are discussed, with specific focus on defects, atomic and molecular adsorbates, doping, and metallic nanoclusters. The latest achievements in atomic site-specific force spectroscopy and the identification of defects by crystal doping, work function, and surface charge imaging are reviewed and recent progress being made in high-resolution imaging in air and liquids is detailed. Finally, some of the key challenges for the future development of the considered fields are identified.