High-resolution tomography techniques have facilitated an improved understanding of solid oxide fuel cell (SOFC) electrode microstructures.The use of X-ray nano computerised tomography (nano-CT) imposes some geometrical constraints on the sample under investigation; in this paper, we present the development of an advanced preparation technique to optimise sample geometries for X-ray nano-CT, utilizing a focused ion beam (FIB) system to shape the sample according to the X-ray field of view at the required magnification.The technique has been successfully applied to a Ni-YSZ electrode material: X-ray nano-CT has been conducted at varying length scales and is shown to provide good agreement; comparison of results from X-ray and more conventional FIB tomography is also demonstrated to be favourable.Tomographic reconstructions of SOFC electrodes with volumes spanning two orders of magnitude are presented. (C) 2010 Elsevier Ltd. All rights reserved.