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.
The solution synthesis route as a scalable bottom-up synthetic method possesses significant advantages for synthesizing nanostructured bulk thermoelectric (TE) materials with improved performance. Tuning the composition of the materials directly in the solution, without needing any further processing, is important for adjusting the dominant carrier type. Here, we report a very rapid (2 min) and high yield (>8 g/batch) synthetic method using microwave-assisted heating, for the controlled growth of Bi2–xSbxTe3 (x: 0–2) nanoplatelets. Resultant materials exhibit a high crystallinity and phase purity, as characterized by XRD, and platelet morphology, as revealed by SEM. Surface chemistry of as-made materials showed a mixture of metallic and oxide phases, as evidenced by XPS. Zeta-potential analysis exhibited a systematic change of isoelectric point as a function of the material composition. As-made materials were directly sintered into pellets by using spark plasma sintering process. TE performance of Bi2−xSbxTe3 pellets were studied, where the highest ZT values of 1.04 (at 440 K) for Bi2Te3 and 1.37 (at 523 K) for Sb2Te3 were obtained, as n- and p-type TE materials. The presented microwave-assisted synthesis method is energy effective, a truly scalable and reproducible method, paving the way for large scale production and implementation of towards large-area TE applications.
Scalable synthetic strategies for high-quality and reproducible thermoelectric (TE) materials is an essential step for advancing the TE technology. We present here very rapid and effective methods for the synthesis of nanostructured bismuth telluride materials with promising TE performance. The methodology is based on an effective volume heating using microwaves, leading to highly crystalline nanostructured powders, in a reaction duration of two minutes. As the solvents, we demonstrate that water with a high dielectric constant is as good a solvent as ethylene glycol (EG) for the synthetic process, providing a greener reaction media. Crystal structure, crystallinity, morphology, microstructure and surface chemistry of these materials were evaluated using XRD, SEM/TEM, XPS and zeta potential characterization techniques. Nanostructured particles with hexagonal platelet morphology were observed in both systems. Surfaces show various degrees of oxidation, and signatures of the precursors used. Thermoelectric transport properties were evaluated using electrical conductivity, Seebeck coefficient and thermal conductivity measurements to estimate the TE figure-of-merit, ZT. Low thermal conductivity values were obtained, mainly due to the increased density of boundaries via materials nanostructuring. The estimated ZT values of 0.8–0.9 was reached in the 300–375 K temperature range for the hydrothermally synthesized sample, while 0.9–1 was reached in the 425–525 K temperature range for the polyol (EG) sample. Considering the energy and time efficiency of the synthetic processes developed in this work, these are rather promising ZT values paving the way for a wider impact of these strategic materials with a minimum environmental impact.
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