The mechanism of the mechanically assisted mineral carbonation of commercial olivine under the flow of a carbon dioxide (CO₂)/nitrogen (N₂) mixture has been elucidated by ex situ powder X-ray diffraction and Fourier-transform infrared spectroscopy. The overall CO₂ conversion depends on the rotational frequency of the mill’s engine, and it reaches 85% within 90 min of mechanical treatment at a flow rate of 2.5 L min⁻¹. By tuning the frequency of rotation, the kinetics of CO₂ conversion unveil a complex reaction pathway involving subsequent steps. Structural analyses suggest that clinochlore, a magnesium (Mg-)- and iron (Fe-)-containing aluminosilicate gathered among the components of olivine, is formed and consumed in different stages, thus promoting the CO₂ sequestration that eventually results in the formation of hydrated and anhydrous Mg-based carbonates.

Several new compounds, with desirable properties of ion mobility and working voltage, have been recently proposed using a density functional theory (DFT) computational approach as potential electrode materials for beyond-lithium battery systems. After evaluation of the ‘energy above hull’, thiospinel MgCr₂S₄ has been suggested as interesting multivalent battery cathode candidate, even though the synthesis of its exact stoichiometry poses serious challenges. In this work, MgCr₂S₄ is prepared using an innovative mechanochemical route starting from magnesium or magnesium hydride, chromium, and sulfur powders. The progress of such mechanically induced reaction as a function of processing time is carefully monitored by XRD with Rietveld refinement, evidencing the occurrence of a mechanically induced self-propagating reaction (MSR). The effect of parameters associated with the milling apparatus (impact energy) on the products composition are also investigated. To our knowledge, this work represents the first report of the scalable and simple mechanical alloying synthesis of thiospinel MgCr₂S₄ (space group Fd-3 m, a = 10.09 Å) and opens up interesting possibilities for the exploitation of such material in next-generation post-lithium batteries.

In situ synchrotron and conventional XRD patterns were solved for the phase developed at 700 °C with the Amm 2 orthorhombic space group, lattice parameters a = 21.187 Å; b = 3.827 Å; c = 19.377 Å; β = 119.83° and chemical composition V ₄ Nb ₂₀ O ₆₀ (ρ = 4.09 g cm ⁻³ ).

A 3D-printable, ARDUINO-based multipurpose X-ray stage of compact dimensions enabling in situ electric field and temperature-dependent measurements is put into practice and tested here. It can be routinely applied in combination with a technique of structural characterization of materials. Using high-performance X-ray laboratory equipment, two investigations were conducted to illustrate the device’s performance. The lattice characteristics and microstructure evolution of piezoelectric ceramics of barium titanate, BaTiO₃ (BT), and barium calcium zirconate titanate, with compositions of (Ba_0.92Ca_0.08) (Ti_0.95Zr_0.05)O₃ (BC8TZ5), were studied as a function of the applied electric field and temperature. The X-ray stage is amenable as an off-the-shelf device for a diffraction line in a synchrotron. It provides valuable information for poling piezoceramics and subsequent optimization of their performance.

A single (Ba_0.85Ca_0.15)(Zr_0.10Ti_0.90)O₃ phase material with a tetragonal structure is processed and synthesized with a modified Pechini method using ethylenediaminetetraacetic acid and glycerol as chelating and esterifying agents, respectively. The complete chemical transformation to the desired phase is achieved at 900 °C, which is 300 °C lower than conventional synthesis methods. Its consolidation, reaching up to 91% relative density, is carried out at 1400 °C. It is clearly demonstrated that the use of ethylenediaminetetraacetic acid and glycerol reagents is particularly beneficial for inducing a homogeneous grain size distribution (10 μm), which leads to very promising electromechanical properties (d₃₃ = 451 pC/N; d₃₁ = 160 pC/N; kp = 0.40; $\epsilon {\prime }_{33}^T$ = 4790 and Q_m = 358) of the densified system.

The rapid rise of publications claiming the synthesis of free-standing borophene via top-down approaches has generated intense excitement, but also deep ambiguity, around the true nature of the resulting materials. Here we demonstrate that, under representative bath-sonication and mechanical milling conditions, no known borophene polymorph is formed. We have compared sonication of boron powder in water, hydrogen peroxide, organic solvents, and ball-milling in controlled gas atmospheres treatments. Multimodal characterization reveals that, under the selected processing routes investigated here, no evidence of borophene or other 2D boron polymorphs is observed. Instead, they yield fragmented β-boron grains coated by boron oxide and boric-acid-derived surface layers, whose defect-rich structure entirely governs the observed optical properties. Sonication promotes hydrolysis and oxidation, while ball milling induces mechanical amorphization followed by formation of an ultrathin BxOy layer. The intense photoluminescence reported in the literature arises from defect states in oxidized boron networks rather than from quantum confinement in putative “borophene nanosheets.” Furthermore, processing in dimethylformamide results in solvent carbonization, raising the possibility of misassigning carbon dots as boron-based luminescent materials. These results challenge widespread interpretations of top-down borophene synthesis and establish rigorous, experimentally grounded criteria for validating past and future claims of free-standing borophene.