A range of high quality Ga 1−x Mn x N layers have been grown by molecular beam epitaxy with manganese concentration 0.2 x 10%, having the x value tuned by changing the growth temperature (T g ) between 700 and 590 °C, respectively. We present a systematic structural and microstructure characterization by atomic force microscopy, secondary ion mass spectrometry, transmission electron microscopy, powder-like and high resolution X-ray diffraction, which do not reveal any crystallographic phase separation, clusters or nanocrystals, even at the lowest T g . Our synchrotron based X-ray absorption near-edge spectroscopy supported by density functional theory modelling and superconducting quantum interference device magnetometry results point to the predominantly +3 configuration of Mn in GaN and thus the ferromagnetic phase has been observed in layers with x > 5% at 3 < T < 10 K. The main detrimental effect of T g reduced to 590 o C is formation of flat hillocks, which increase the surface root-mean-square roughness, but only to mere 3.3 nm. Fine substrates' surface temperature mapping has shown that the magnitudes of both x and Curie temperature (T C ) correlate with local T g . It has been found that a typical 10 o C variation of T g across 1 inch substrate can lead to 40% dispersion of T C . The established here strong sensitivity of T C on T g turns magnetic measurements into a very efficient tool providing additional information on local T g , an indispensable piece of information for growth mastering of ternary compounds in which metal species differ in almost every aspect of their growth related parameters determining the kinetics of the growth. We also show that the precise determination of T C by two different methods, each sensitive to different moments of T C distribution, may serve as a tool for quantification of spin homogeneity within the material.
Flame spray pyrolysis (FSP) is a novel technique for the fabrication of nanostructured catalysts with farreaching options to control structure and composition even in cases where complex composites need to be prepared. In this study, we took advantage of this technique to synthesize highly dispersed pure and Pddoped iron oxide nanoparticles and investigated them as Fischer-Tropsch (FT) catalysts. By systematically varying the Pd content over a large range from 0.1 to 10 wt %, we were able to directly analyze the influence of the Pd content on activity and selectivity. In addition to catalytic measurements, the structure and composition of the particles were characterized before and after these measurements, using transmission electron microscopy, adsorption measurements, X-ray diffraction, and EXAFS. The comparison revealed on the one hand that small Pd clusters (diameter: 1-2 nm) evolve from initially homogeneously distributed Pd and on the other hand that the iron oxide transforms into iron carbides depending on the Pd content. The presence of Pd influences the particle size in the pristine samples (8-11 nm) resulting in specific surface areas that increase as the Pd content increases. However, after activation and reaction the specific surface areas become similar due to partial agglomeration and sintering. In a fixed bed FT reaction test, enhanced FT activity was observed with increasing Pd content while the selectivity shifts to longer chain hydrocarbons, mainly paraffins. Mechanistic implications regarding the role of Pd for the performance of the catalysts are discussed.
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