GaN:Mg layers with different concentration of Mg dopant were grown by metalorganic vapour phase epitaxy. The incorporation of Mg was verified by secondary ion mass spectroscopy. In order to dissociate Mg-related complexes and thus electrically activate the acceptor dopant, the as-grown layers were annealed in pure N 2 at ~800 °C for 30 minutes. The influence of the post-growth annealing on the layer properties was studied by photoluminescence (PL) and impedance spectroscopy. Impedance spectroscopy measurement showed that the annealed samples reveal higher charge concentrations and lower sheet resistance. Moreover, the relaxation time of hole traps decreased in annealed samples by one order of magnitude compared to as-grown samples. The changes in the electrical properties have been correlated with the changes in the PL spectra.