The activation kinetics of acceptors was investigated for heteroepitaxial layers of GaN, doped with Mg. After growth, the samples were exposed to isochronal rapid thermal anneals in the temperature range from 500 to 775 °C. The samples were studied by variable temperature Hall effect measurements and photoluminescence (PL) spectroscopy in the as‐grown condition and after each temperature step. The thermal treatment reduced the resistivity by six orders of magnitude and thep‐type conductivity was found to be dominated by an acceptor with an activation energy of ∼170 meV. This acceptor is attributed to Mg atoms substituting for Ga in the GaN lattice and the activation process is consistent with dissociation of electrically inactive Mg–H complexes. It is shown that the appearance of a blue emission band in the PL spectrum of Mg‐doped GaN does not directly correlate with the increase inp‐type conductivity. ©1996 American Institute of Physics.