We present a straightforward and fast positron annihilation spectroscopy (P
AS) technique for measuring the 2 to 3 photon annihilation ratio of Ps (ele
ctron-positron) atoms (3 gamma PAS), utilized here for the nondestructive c
haracterization of mesoporous (pore size >1 nm) dielectric films. Examples
are given for similar to1-mum-thick foamed methyl-silsesquioxane (MSSQ) fil
ms, produced by mixing MSSQ (0-90 wt % fraction) with a sacrificial foaming
agent (porogen). Probing these films as a function of depth allows one to
monitor Ps escape from interconnected pores and to determine the threshold
for pore interconnectivity to the film surface. A classical treatment of Ps
diffusion is used to calculate the open and closed porosity fractions as a
function of the initial porogen load. (C) 2001 American Institute of Physi
cs.