Quantitative atom‐probe field‐ion microscopy (APFIM), x‐ray photoelectron spectroscopy (XPS), and qualitative secondary ion mass spectrometry (SIMS) have been applied in a phenomenological study of the modification in surface composition of copper–nickel targets by low energy ion sputtering. In agreement with the bulk of previously reported studies, XPS and SIMS data suggest the preferential loss of copper. APFIM data have revealed that the immediate surface layers remain unchanged in composition while a nickel‐enriched layer is found immediately subsurface. This result is in accord with recent studies using ion scattering spectroscopy.

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