A focused ion beam (FIB) instrument has been used to mill surfaces in singlecrystal Si and single-crystal Cu for subsequent electron backscattering diffraction (EBSD) analysis. The FIB cuts were performed using a 30 keV and a 5 keV Ga ϩ ion beam at a stage tilt of 20°to provide a readily obtainable 70°surface for direct EBSD investigation in a scanning electron microscope (SEM). The quality of the patterns is related to the amount of FIB damage induced in the Cu and Si. These or similar methods should be directly transferable to a FIB/SEM dual beam instrument equipped with an EBSD detector.