Spinodal Decomposition by a Two-Step Procedure for Nano Porous Silica.

The phase separation of the NaO-BO-SiO system was explored both theoretically and experimentally in order to attain a spinodal structure having a narrowed periodic distance (<70 nm) with the porosity being kept at ∼60%. The phase separation was dealt with by two stages: an initial thermodynamic process of spinodal decomposition and a latter growth of the spinodal structure. The initial structural development was related to the interfacial energy and the change in free energy caused by phase separation. For the latter growth, a mathematical model was proposed to explain the kinetics by incorporating the effect of the inverse-square law in the diffusion of SiO, and a basic relation of (: average periodic distance; : time) was successfully derived. The phase separation was carried out accordingly by two steps: first for the phase separation forming durable silica skeletons at lower temperatures and second for the new equilibrium at the elevated temperature and the subsequent growth of the phase-separated structure. It was proven that the addition of AlO in the glasses decreased the interfacial energy, leading to small periodic distances and the rapid establishment of the durable silica skeletons. In the two-step process, the fraction of borate-rich phase increased, and the structure grew depending on a modified period of time.