Optically-detected magnetic resonance (ODMR) and positron annihilation spectroscopy (PAS) experiments have been employed to study magnesium-doped GaN layers grown by metal-organic vapor phase epitaxy. As the Mg doping level is changed, the combined experiments reveal a strong correlation between the vacancy concentrations and the intensity of the red photoluminescence band at 1.8 eV. The analysis provides strong evidence that the emission is due to recombination in which electrons both from effective mass donors and from deeper donors recombine with deep centers, the deep centers being vacancy-related defects.Deep defects play a key role in the performance limits and aging effects of GaN-based light-emitting devices. They also lead to photoluminescence (PL) at energies well below the band-gap. For example, PL and opticallydetected magnetic resonance (ODMR) studies [1,2,3,4] have suggested that deep defects are responsible for the red (1.8 eV) luminescence band which is often observed in Mg-doped GaN and that the band is due to recombination emission in which vacancy-dopant complexes are involved [1,2]. However, this proposal was mainly based on indirect evidence and on previous experience of II -VI compounds, and further experimental confirmation is therefore needed. The present study involved the use of both ODMR and positron annihilation spectroscopy (PAS) on the same set of samples covering a range of Mg doping levels and we have established a correlation between the ODMR spectra (obtained by monitoring the red PL) and the PAS results.ODMR is well established as a means of investigating centers involved in recombination processes in semiconductors [5,6]. For a detailed description of the technique and our ODMR system, see Ref. [7]. The ODMR was carried out at 14 GHz with the specimen at 2K. The PL was excited with a UV argon-ion laser (363.8/351.1 nm). The microwaves were chopped at 605 Hz and changes in the PL intensity caused by magnetic resonance were monitored at this frequency as the magnetic field was slowly swept. PAS with a slow positron beam is an effective tool for the investigation of open volume defects such as neutral or negatively charged vacancies in semiconductor films. When positrons annihilate electrons in semiconductors the resulting gamma ray energy spectrum, peaked at 511 keV, is Doppler-broadened (since the electrons have a range of momenta). The annihilation linewidth is characterized by quantities S (W ), defined as the central (wing) fraction of the line. The value of S (W ) is characteristic of the material under study, but * Electronic address: d.wolverson@bath.ac.uk is generally higher (lower) when vacancies are present [8]. Measurements of S (W ) can thus be used to monitor vacancy concentrations. In the present work, singledetector Doppler-broadening PAS was performed using a magnetic transport positron beam system [9]. Positrons were implanted into the layers at energies in the range 0.1 -30 keV, corresponding to mean depths up to 1.5 nm.Details of the growth of the GaN:Mg sampl...