The steady and stoichiometric delivery of metal-organic precursor mixtures is essential for the production of complex, functional nanomaterials in the gas phase. Chemical vapor synthesis (CVS) is a corresponding process which enables the production of complex oxide nanoparticles such as perovskites. While there exist a vast number of compositions that form perovskite structures, many technically relevant materials consist of transition metals and lanthanides. Their corresponding metal organic precursors often deviate significantly in their thermal behavior, resulting in a challenging delivery of precursors to the reactor. One suitable method for precursor delivery is flash evaporation by an infrared laser, where a mixture of solid precursors is instantly sublimed. Using flash evaporation, the stoichiometry of the generated vapor corresponds to the composition of precursors in the solid mixture. In this study, we present an alternative flash evaporation system based on a marking laser which rapidly scans a focused infrared beam across a precursor powder bed. By focusing the beam, higher energy densities are reached, compared to existing systems while a large area powder bed is repeatedly scanned and sublimed. Fourier-transform infrared spectroscopy (FTIR) measurements confirm the decomposition-free sublimation of precursor mixtures. Furthermore, we confirm the successful precursor delivery by the synthesis of LaFeO3 nanoparticles with an average crystallite size of 5.3 nm. The structure of the ensemble of nanoparticles is examined using X-ray diffraction (XRD) and Rietveld refinement, transmission electron microscopy (TEM), selected area diffraction (SAED), and extended X-ray absorption fine structure (EXAFS) at the Fe-K edge analyzed by reverse Monte Carlo (RMC) analysis.

The identification of structure−activity relationships is challenging for complex oxides like lanthanum-based perovskite nanoparticles. The purpose of this study is to examine the structure of LaCo 1−x Fe x O 3 nanoparticles and develop a detailed structural model to identify subtle changes of the structure after catalysis. Therefore, small nanoparticles with a significant fraction of surface atoms and varying iron content (x = 0, 0.5, 1) are synthesized in the gas phase by chemical vapor synthesis and tested in cyclohexene oxidation in the liquid phase. The crystal structure is examined by X-ray and selected area electron diffraction. Additionally, the local structure of the cations is probed by Xray absorption spectroscopy at the Co, Fe, La K, and La L 3 -edges. For a quantitative analysis of the local structure before and after catalysis, an atomistic model is refined by the available extended X-ray absorption fine structure spectra using Reverse Monte Carlo methods. The produced nanoparticles are small with a coherent diffraction domain size between 5 and 10 nm, highly crystalline, and consist mainly of the perovskite phase with a secondary spinel phase. In cyclohexene oxidation, the cobalt-containing samples exhibit significant catalytic activities. The active samples show structural changes after catalysis accompanied by reconstruction of the local structure surrounding the cations in the perovskite phase, which resembles edge-sharing cobalt octahedra.