Nanocrystalline powders with an average particle size of 50 nm has been synthesized in two materials systems under hydrothermal conditions below 100°C. Processing variables, such as temperature, concentration and molar ratio of reactants and reaction time were optimized to obtain particles of reduced size and stoichiometric compositions. Hydrothermal reaction takes place between Ba(OH)2 solution and titanium/iron precursors in sealed polyethylene bottles in the BaTiO3 and BaFe12O19 systems, respectively. While crystalline BaTiO3 forms relatively fast within a few hours, formation of fully crystalline and stoichiometric BaFei20i9 require considerably longer reaction times up to several weeks and strongly dependent on the Ba:Fe ratio of the precursors. The structural and compositional evaluation of the nanophase powders were studied by XRD and TEM techniques.