We report the synthesis of ion-exchangeable molybdenum sulfide chalcogel through an
oxidative coupling process, using (NH4) 2MoS4 and iodine. After supercritical drying, the
MoS x amorphous aerogel shows a large surface area up to 370 m2/g with a broad range of
pore sizes. X-ray photoelectron spectroscopic and pair distribution function analyses reveal
that Mo6+ species undergo reduction during network assembly to produce Mo4+-containing
species where the chalcogel network consists of [Mo3S13] building blocks comprising …