In this paper, we present an experimental study on the structural evolution of B2 type FeAl multilayers submitted to thermal annealing. Multilayer samples have been obtained by evaporating 15 couples of 10 nm Fe and 14 nm Al layers on (100)-oriented Si wafers in an UHV chamber. After deposition, the samples have been heat treated at temperatures ranging from 375 to 775 K. Some samples were also annealed in air to promote the formation of a surface oxide layer. Different analytical techniques were used in order to achieve a complete characterisation of the deposited layers. (C) 2003 Elsevier Science B.V. All rights reserved.