RESUMO
We present the concept for a sample holder designed for mounting and heating of plate-like samples that is based on a clamping mechanism for easy handling. The clamping mechanism consists of a U-shaped bracket encompassing the sample support plate from the rear. Two spring wires are fixed in the walls of the bracket spanning the sample to secure it with only two point contacts. This enables the sample to freely expand or contract during heating and cooling. To accommodate for a large variety in sample size, shape, and quality, we introduce two designs differing in the generation of the clamping force: One pressing the sample against the spring wires, the other one pulling the spring wires onto the sample. Both designs yield an automatically even alignment of the sample during the mounting process to achieve an even load distribution and reliable fixation specifically for brittle samples. For high temperature treatment, the sample holders are enhanced by a resistive heating plate. As only the sample and a small fraction of the sample holder are heated, temperatures of 1300 °C are reached with only 8 W heating power. The sample support and heating components are mounted on a 11 mm × 13 mm base plate with a handle that can be transferred between the sample entry stage, the preparation stage, and surface science experiments in the ultra-high vacuum system.
RESUMO
The surface morphology of CeO(2)(111) single crystals and silicon supported ceria films is investigated by non-contact atomic force microscopy (NC-AFM) and Kelvin probe force microscopy (KPFM) for various annealing conditions. Annealing bulk samples at 1100 K results in small terraces with rounded ledges and steps with predominantly one O-Ce-O triple layer height while annealing at 1200 K produces well-ordered straight step edges in a hexagonal motif and step bunching. The morphology and topographic details of films are similar, however, films are destroyed upon heating them above 1100 K. KPFM images exhibit uniform terraces on a single crystal surface when the crystal is slowly cooled down, whereas rapid cooling results in a significant inhomogeneity of the surface potential. For films exhibiting large terraces, significant inhomogeneity in the KPFM signal is found even for best possible preparation conditions. Applying X-ray photoelectron spectroscopy (XPS), we find a significant contamination of the bulk ceria sample with fluorine while a possible fluorine contamination of the ceria film is below the XPS detection threshold. Time-of-flight secondary ion mass spectroscopy (TOF-SIMS) reveals an accumulation of fluorine within the first 5 nm below the surface of the bulk sample and a small concentration throughout the crystal.
RESUMO
We present a versatile system for the preparation of oxide crystal surfaces in the ultra-high vacuum (UHV) at temperatures up to 1300 K. Thermal treatment is accomplished by direct current heating of a tantalum foil in contact with the oxide sample. The sample temperature is measured by a thermocouple at a position close to the crystal and its reading is calibrated against the surface temperature determined by a second thermocouple temporarily attached to the surface. The design of the sample holder is based on a transferable plate originally developed for a commercial UHV scanning probe microscope. The system is, however, also suitable for the use with electron spectroscopy or electron diffraction based surface analytical techniques. We present results for the high-temperature preparation of CeO(2)(111) surfaces with atomically flat terraces exhibiting perfect atomic order and cleanliness as revealed by non-contact atomic force microscopy (NC-AFM) imaging. NC-AFM imaging is, furthermore, used to demonstrate the temperature-controlled aggregation of gold atoms on the CeO(2)(111) surface and their evaporation at high temperatures.
