Multiple small-angle neutron scattering characterization of the densification of ceramics: application to microporous silica

Multiple small-angle neutron scattering was used to characterize the microstructure evolution of porous silica as a function of thermal processing. This new technique offers a statistically significant determination of microstructure morphology in the 0.08–10 μm range, which was previously inaccessible without increasing the resolution of the currently available scattering spectroscopy beamlines. All of the scatterers, which in the present work are pores within ceramic bodies, are measured whether they are open or closed. Earlier mercury porosimetry and nitrogen desorption measurements of the microporous silica system indicated that there are two major populations of pores in this material, differing in pore size by approximately an order of magnitude. In this work, it was found that densification during the intermediate stages of sintering is accompanied by coarsening to radii > 0.22 μm within the population of large pores in microporous silica. In the late stages of sintering, there are no detectable pores with radii > 0.08 μm, and radii of gyration equal to 33 and 28 nm were measured. Finally, Monte Carlo simulations were carried out to complement the neutron-scattering measurements, to predict the influence on the results of the bimodal distribution, and to explore the sensitivity of the multiple-scattering method.