Controlled Synthesis of Alkali Metal Hydroxide Particles via Solvothermal Processing

This study presents a solvothermal approach starting from micron-sized hydroxide precursors, which combines features of top-down size reduction and bottom-up recrystallization, leading to nanoscale hydroxide particles. The method is based on autoclave treatment at a moderate temperature (180 °C) and a pressure of 8 bar, using different mixtures of water and isopropanol. The hydroxide precursors, used in micrometric form without surfactants or additives, were converted into nanoscale particles through a one-pot, one-step process. The nanomaterials obtained were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), optical microscopy (MO), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET) surface area analysis to assess their structural, morphological and textural characteristics. The results show that solvent composition and precursor concentration strongly influence the crystalline phase, particle morphology, dispersion stability and surface area. Well-defined acicular and fibrous morphologies were obtained for Ba(OH)2 and Sr(OH)2, while Mg(OH)2 formed spherical and hexagonal structures, respectively. Of all the conditions tested, the 75:25 water/isopropanol ratio produced the most stable systems. This work provides a method to produce alkaline earth hydroxide nanoparticles with tunable properties.