In this work we report on the lattice site location of rare earths in single-crystalline ZnO by means of the emission channeling (EC) technique. Following low dose (3×1013at/cm2) 60 keV ion implantation of the precursor isotope 169Yb, a position-sensitive electron detector was used to monitor the angular distribution of the conversion electrons emitted from 169Tm* as a function of the annealing temperature up to 600°C in vacuum. An additional annealing at 800°C in flowing O2 was performed. The EC measurements revealed that around 95–100% of the rare earth atoms occupy substitutional Zn sites up to an annealing temperature of 600°C/vacuum. After the 800°C/O2 annealing, the emission channeling effects decreased considerably.