We have investigated the structural and defect characteristics of GaAs and Al x Ga 1Ϫx As grown at low substrate temperature ͑250°C͒ by molecular beam epitaxy. Using x-ray diffraction we have observed an increase in lattice parameter for all as-grown layers, with the Al x Ga 1Ϫx As layers showing a smaller expansion than the GaAs layer. However, infrared absorbtion measurements revealed that the concentration of neutral arsenic antisite defect, ͓As Ga ͔ 0 , was not significantly affected by aluminum content (x), with only a small reduction for xϭ0.36. Positron beam studies showed that the low temperature layers had a higher concentration of vacancy-related defects ͑ϳ10 17 cm Ϫ3 ͒ than the semi-insulating substrate, with the Al x Ga 1Ϫx As layers having the highest values. After annealing ͑600°C, 15 min͒ the lattice constants relaxed to those of conventionally grown material and ͓As Ga ͔ 0 was reduced in all cases, with the smallest reduction occurring for the xϭ0.36 layer, indicating that the Al atoms strengthen the lattice against excess arsenic incorporation and hold the arsenic antisite atoms more strongly in position. X-ray photoelectron spectroscopy showed that arsenic diffused out of the surface region and was replaced by oxygen, possibly due to an insufficient overpressure of forming gas during the anneal. This oxygen penetration was greater for the GaAs layer than for the Al x Ga 1Ϫx As layers. Extra Raman peaks at 200 and 257 cm Ϫ1 confirmed that the surface was very disordered. There was, nevertheless, a large increase ͑4%͒ in the positron S parameter in the bulk of the annealed layers, suggesting the formation of vacancy clusters, whereas in the surface region we find evidence that As Ga diffusion proceeded at a faster rate in the xϭ0.36 than the xϭ0.2, in agreement with the vacancy-enhanced As Ga diffusion model.