A series of MgAl-layered double hydroxides (MgAl-LDHs) were prepared by variable pH precipitation. The addition of the metal (M) containing solution to the base (B=NaOH) solution, either rapidly (r) or dropwise (d), led to the obtention of the MBr and MBd samples, respectively. In the other hand, by inverting the order of the added solution (pH increase methodology), BMr and BMd were obtained. The BMd sample was microwave aged at 80 °C, 150 °C and 220 °C for 45 min. The results of powder X-ray diffraction showed that rapid precipitation produces more crystalline LDHs than those obtained by dripping. The crystallinity of BMd was improved by microwave aging. All precipitation conditions produced nanoparticles with an average size of around 27.5 nm, which increased almost 5-fold with the microwave treatment. Precipitation by increasing pH gave LDHs with low pore volume, which increased during the heat treatment. Nevertheless, the specific surface area decreased significantly with aging temperature due to the increase in particle size.