An evaluation of NMR cryoporometry, density measurement and neutron scattering methods of pore characterisation

Sol-gel silicas with nominal pore diameters ranging from 25A to 500A were studied by NMR cryoporometry, and by neutron diffraction and small angle scattering from dry silicas over the Q range 8. 10(-4)A(-1) < or = Q < or = 17A(-1). Density and imbibation experiments were also performed. Geometric models of porous systems were constructed and were studied by both analytic techniques and Monte-Carlo integration. These models, combined with the information from the above measurements, enabled the calculation of the fully density corrected solid-solid density correlation functions G(r) for the sol-gel silicas, deduction of the (voidless) silica matrix density, measurement of the silica fraction in the grain and of the packing fraction of the silica grains and an estimation of the water equivalent residual hydrogen on the dried silica surface. In addition, the pore diameter D, pore diameter to lattice spacing ratio D/a, and pore and lattice variance sigma could also be measured. While the NMR cryoporometry pore diameter measurements for the sol-gel silicas show excellent co-linearity with the nominal pore diameters as measured by gas adsorption, and the calculated pore diameters from the measured neutron scattering show surprisingly good agreement with these measurements at large pore diameters, there is a divergence between the calibrations for pore diameters below about 100A.