Alumina/silicas have been prepared by three methods: complexing-agent-
assisted sol-gel, coprecipitation and hydrogel kneading. The propertie
s of these alumina/silicas were investigated by solid-state magic-angl
e-spinning nuclear magnetic resonance (MAS NMR), ammonia temperature-p
rogrammed desorption (TPD) and nitrogen adsorption. Al-O-Si bond forma
tion is more effectively performed in the sol-gel alumina/silicas than
in the conventional ones. This was deduced from the shift profile in
the Si-29 NMR spectra of the sol-gel alumina/silicas with the change i
n the Al/Si ratio, which is comparable to that of zeolites. Because of
the effective Al - O - Si bond formation by the sol-gel method, the s
ol-gel alumina/silicas show much higher acid amounts than the correspo
nding conventional ones. As certain complexing agents can level the hy
drolysis rates of silicon and aluminium alkoxides and bind both metal
atoms, the use of a complexing agent is effective for the formation of
Al-O-Si bonds and the preparation of alumina/silicas with high miscib
ility and controlled properties.