Controlled Morphology Synthesis of Nanostructured β-AlF_3–<i>x</i>(OH)<i>_x</i> with Tunable Specific Surface Area

In this work, the synthesis of β-AlF3–x(OH)x nanoparticles with very high specific surface area (SSA) using a microwave-assisted solvothermal process is reported. The influence parameters on morphology and SSA was investigated, nature solvent shown to have greatest impact. Five samples prepared different mixtures were deeply characterized by thermogravimetric analysis (TGA), N2 sorption, powder X-ray diffraction, transmission electron microscopy (TEM), 19F 27Al high-field solid-state NMR. Their SSAs range from 25 345 m2·g–1 an associated OH content slightly increasing ≈16% (AlF2.52(OH)0.48) ≈19% (AlF2.42(OH)0.58), as estimated TGA Compared previous reference work [Dambournet, D., Chem. Mater. 2008, 204 1459−1469], up 4 times larger obtained. TEM revealed formation hollow nanostructures except when exceeds 300 m2·g–1, in which case isolated are observed. sample highest also displaying appealing cumulative pore volume 0.060 cm3·g–1, its hydrogen adsorption capability evaluated show that potential interest for storage applications.