Si
lica-based MCM-41-
like mesoporous materia
ls with high coba
lt content (
Si/Co
23) have been synthesized through a one-pot surfactant-assisted procedure from aqueousso
lution using a cationic surfactant (CTMABr = cety
ltrimethy
lammonium bromide) asstructura
l directing agent, and starting from mo
lecu
lar atrane comp
lexes of Co and Si asinorganic hydro
lytic precursors. This preparative technique a
llows optimizing the dispersionof the Co guest species in the si
lica wa
lls. The mesoporous nature of the fina
l materia
ls isconfirmed by XRD, TEM, and N
2 adsorption-desorption isotherms. They disp
lay unimoda
land re
lative
ly narrow pore size distributions, whereas their pore array evo
lves from orderedhexagona
l (H
0) to wormho
le-
like (W) as the Co content increases. A carefu
l spectroscopic(UV-visib
le and NMR) and magnetic study of these materia
ls shows that, regard
less of theSi/Co ratio, Co atoms are organized in we
ll-dispersed, uniform CoO nanodomains (ca. 3 nm)partia
lly
embedded within the si
lica wa
lls. These materia
ls, which show superparamagneticbehavior, can be referred to as mesoporous CoO-MCM-41 nanocomposites.