Neutron diffraction data is used to reveal details of the effect of ad
ding titania to a silica-based sol-gel, including a first direct obser
vation of the Ti-O correlation, At low Ti contents the data are consis
tent with the 4-fold oxygen coordination derived from NMR. Even at the
se concentrations the silica network is shown to have been affected si
gnificantly, with bond-length distributions being narrowed, and with a
high level of network-OH indicating a qualitative change in the mesos
copic structure associated with interfacial surfaces, Data on a phase
separated sample supports the conclusion that the network-OH is associ
ated with the phase separation process.