Characterisation of metakaolin-based geopolymers using beam-based and conventional PALS

Abstract

The nano-porosity of metakaolin-based geopolymers and the effect of heat-treatment on porosity have been studied with conventional and beam-based positron annihilation lifetime spectroscopy (PALS). Conventional PALS found significant nano-porosity in the geopolymers, as indicated by the presence in the PALS spectrum of two long lifetime components, τ3 = 1.58 ns and τ4 = 47 ns, associated with pore diameters of approximately 0.5 and 3 nm respectively. The lifetime of the shorter component was found to decrease monotonically with successive heat treatments of 300°C and 600°C. Beam-based PALS, conducted at 5 keV, also indicated two long lifetime components, τ3 = 4.84 ns and τ4 = 54.6 ns. These are significantly longer than those observed by conventional PALS and the monotonic decrease of τ3 with successive heat treatments was not observed. As the beam-based PALS probed only the near-surface region, with an average implantation depth of about 350 nm, these results suggest that the near-surface structure may vary significantly from that of the bulk. This could be an inherent property of the samples or an artefact caused by surface effects or sample outgassing.