Synchrotron X-ray micro-computed tomography (X-ray mu CT) is employed to measure the volume variation of gas diffusion layer (GDL) of a polymer electrolyte fuel cell (PEFC). In the present study, 3D structures are reconstructed by merging orthogonal-plane images. Using the 3D reconstruction, the variation of structural parameters such as the porosity in GDL is investigated under freeze-thaw cycles. The freez-thaw cycles are established using cryo system and light source, respectively. As a result, a structural transformation is observed at the interface between GDL and micro porous layer (MPL). In addition, the porosity is critically changed with irreversible transition under freeze-thaw cycles. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.