Kesterite (Cu2ZnSnS4, CZTS) powders were produced by reactive high-energy milling, starting from stoichiometric mixtures of the elemental components. CZTS forms fine crystals with a cubic structure, which evolves to the stable tetragonal form after thermal treatment. Tablets were produced by cold pressing of the ball milled powder, and sintered up to 660 °C. Seebeck coefficient, electrical resistivity, and thermal diffusivity were measured on the sintered tablets, pointing out the positive effect of CZTS nanostructure and of the rather large fraction of porosity: thermal conductivity is rather low (from ~0.8 W/(m K) at 20 °C to ~0.42 W/(m K) at 500 °C), while electrical conduction is not seriously hindered (electrical resistivity from ~8500 µΩ m at 40 °C to ~2000 µΩ m at 400 °C). Preliminary results of thermoelectric behavior are promising.

In this work, a poorly water-soluble drug (efavirenz) was mechanically activated by ball-milling. The effect of the mechanical activation on the dissolution behavior was investigated considering changes in the particle size and morphology. The powder diffraction was used to follow the comminution process, verifying phase compositions, and crystalline domain size. The interplay between domain and grain size was studied in relation to the solubility rate, through specific dissolution tests. Finally, the morphological characterization has allowed to complete the physical–chemical characterization of the milled powders. This study demonstrated that the mechanical activation of the drug leads the particle size reduction and, with a long milling time, morphological changes. The grain size reduction is not always sufficient to increase the solubility: morphology and agglomeration grade play an important role in the dissolution process.

Ball milling induced the formation of nanocrystalline and amorphization phase in Fe–25.68% Dy2O3 powder mixtures (mass fraction, %). The microstructure was investigated by using X-ray diffraction and transmission electron microscopy. The transformation of Dy2O3 from cubic to monoclinic crystal structure and then to the amorphization was observed during ball milling. A few Dy atoms were dissolved into Fe crystal structure, which was discussed using mechanical kinetics. After 48 h of ball milling, the homogenous mixtures of supersaturated nanocrystalline solid solution of Fe (Dy, O) and Dy2O3 amorphization were formed and the elements of Fe, Dy, and O were distributed uniformly in the ball-milled particles. During the whole ball mining process, a rapid decrease in Fe grain size was observed over the initial time period, while a constant value was presented in later stage, resulting in a final size of about 20 nm. The mechanism of the microstructural evolution of powder mixtures was analyzed and discussed.

Selected hydrides (TiH2, ZrH2), chlorides (VCl3, ScCl3) or oxides (V2O5) utilized as additives facilitating hydrogen release and uptake for magnesium hydride were investigated using mechano-chemical treatment and in-situ synchrotron radiation powder X-ray diffraction studies. The fastest hydrogen desorption and absorption kinetics for MgH2 was observed for a sample with 5 mol% V2O5 at 320 °C. Additional activation of the system (2 cycles, vacuum/p(H2) ~150 bar, 450 °C) leads to significant improvement of the kinetics even at lower temperatures, 270 °C. The observed prolific effect is achieved through the full reduction of vanadium oxides and formation of an efficient vanadium catalyst as nanoparticles and possibly interfacial effects in the MgO/Mg/MgH2/V system introduced during cycling hydrogen release and uptake in hydrogen/dynamic vacuum at 450 °C. Nanostructuring as well as hydrogen permeability via vanadium nanoparticles may improve kinetics and reduce the apparent activation energy for hydrogen release. Thus, the enhancement of hydrogen release/uptake in the MgH2 owe to “in situ” formation of vanadium nanoparticles by reduction of V2O5.

A powder obtained by ball milling a commercial FeMo alloy has been identified and investigated as possible reference material for powder diffraction line profile analysis. Ball milling yields micrometer-scale agglomerate particles made of rounded nanocrystalline domains with extensive lattice defects, so as to produce both size and strain contributions to the line profiles. The capability of a modern whole-powder pattern modeling to accurately quantify those aspects and the stability of the powder over a decade are shown and discussed.