In Situ Observation of ZnO Nanoparticle Formation by a Combination of Time-Resolved X-ray Absorption Spectroscopy and X-ray Diffraction.

The formation of ZnO nanomaterials from different Zn acetylacetonate precursor solutions was studied in situ by employing simultaneous, time-resolved X-ray diffraction (XRD) and X-ray absorption spectroscopy (EXAFS) at the Zn K-edge. The precursor solutions were heated from room temperature to the desired reaction temperatures in a hermetically sealed cell dedicated to X-ray experiments. In general, the first indications for the formation of hexagonal ZnO were found for elevated temperatures of about 80 °C both by XRD and EXAFS, and the contributions increase with temperature and time.

High-temperature treatments of niobium under high vacuum, dilute air- and nitrogen-atmospheres as investigated by in situ X-ray absorption spectroscopy.

Niobium metal foils were heat-treated at 900°C under different conditions and in situ investigated with time-resolved X-ray absorption fine-structure (EXAFS and XANES) measurements. The present study aims to mimic the conditions usually applied for heat treatments of Nb materials used for superconducting radiofrequency cavities, in order to better understand the evolving processes during vacuum annealing as well as for heat treatments in controlled dilute gases. Annealing in vacuum in a commercially available cell showed a substantial amount of oxidation, so that a designated new cell was designed and realized, allowing treatments under clean high-vacuum conditions as well as under well controllable gas atmospheres.