Two sets of pillared clays (PILCs), chromia and tin-oxide-pillared montmorillonites and laponites, were successfully prepared at Aston University using both conventional and microwave-assisted methods and characterised by X-ray diffraction and thermogravimetric analysis. Microwave irradiation enabled the preparation of the PILCs in a fraction of time of the conventional methods. X-ray powder diffraction was not a suitable method for charactetizing laponite or pillared laponites due to the lack of first order reflections attributed to the small size of individual particles and the random rather than uniform face-to-face orientation of the clay platelets. Laponite appeared to be more thermally stable than montmorillonite. For pillared montmorillonites, dehydroxylation shifted to a lower temperature compared to the starting materials, whereas for tin-oxide-pillared laponites such a shift did not occur. On the other hand for chromia laponite dehydroxylation took place over a much wider temperature range compared to all other materials. The prepared PILCs were employed as catalysts in the hydrocracking of coal-derived liquids in a conventional microbomb reactor at Imperial College exhibiting high-quality performance and remaining active after 4 h utilization regardless of high coke deposition. They actually showed an increase in the total conversion when reused. (c) 2004 Elsevier B.V. All rights reserved.