Abstract. The radiation damage of polycrystalline Ni3Al thin foils of stoichiometric composition by a nanoscale stationary 200 keV FEG electron probe in an FEI Tecnai F20 (S)TEM has been investigated. Nanometre holes are produced in these TEM thin films and EDX spectra from the irradiated volume have been collected with the incident electron beam at both  and , From the EDX results, preferential surface sputtering of aluminium from Ni3Al has been demonstrated. The sputtering rate at the electron-exit surface of a Ni)Al thin foil has been measured. The film sputtering and hole formation processes have been simulated successfully, All the experimental results agree well with theoretical results from Molecular Dynamics (MD) and Monte Carlo (MC) computer simulations (W. S. Lai & D. J. Bacon, University of Liverpool).