Production of meso- and giga-porous zirconia particles - An improved multi-step particle aggregation process

Macro- and giga-porous zirconia supports were prepared from a 20% colloidal sol of zirconia (ZrO₂) by a combination of a polymer-induced colloid aggregation (PICA) process and the oil emulsion (OE) method. The effect of the pH of the initial sol on the size of the PICA particles, and subsequently on the final product, made by oil-emulsion assisted aggregation of the PICA particles was thoroughly investigated. Both the PICA and the OE methods were further optimized for performance. Particle morphology and porosity of the resultant particles were characterized by scanning electron microscopy, mercury intrusion-extrusion porosimetry, and nitrogen adsorption-desorption sorptometry. The supports were comprised of stable aggregates of 50-250 μm in size. The pore and throat size distributions showed narrow bi-modal distributions over two distinct size scales: 10-100 nm and 600-3000 nm. In addition, different combinations of aggregation techniques and porous supports prepared in previous steps for use in a subsequent aggregation were evaluated. Optimal amounts of zirconia sol and 10-100 micron porous spherical particles produced by the OE method in an earlier step were combined in an additional OE process to yield stable giga-porous supports. Porous zirconia particles obtained after calcination and sintering had particle sizes of 0.15-3.5 mm and multimodal pore and throat distributions over a range of 50 nm-8 μm.