We report, for the first time, our result on characterisation of Al-pi
llared clay using positron annihilation spectroscopy (PAS) along with
XRD and BET techniques. Positron life-time spectra for Al-pillared mon
tmorillonite, as received and calcined at different temperature (100-5
00 degrees C), along with the parent natural clay are measured. The an
nihilation rate of ortho-positronium (o-Ps) increases monotonically wi
th calcination temperature up to 300 degrees C and falls subsequently.
Similar behaviour is seen for the fraction of o-Ps formed. We interpr
et the initial rise in annihilation rate of o-Ps to be due to the incr
ease in Bronsted acidity with dehydroxylation of pillars. The reductio
n in annihilation rate on calcination at higher temperatures could be
due to loss of acidity and/or due to mesopore formation following dela
mination of clay structure.