BaTi5O11 has been extensively studied because of their microwave dielectrics properties. Traditionally, it is difficult to achieve this material as single-phase. Here, we report an effective method to obtain BaTi5O11 powder with nanometer-scale crystals, by solid-state reaction at moderate temperatures and using as precursors nanostructured particles consisting of BaTiO3 and TiO2. The main advantage is the intimate contact between the BaTiO3 and TiO2 that ensure, when the solid-state reaction takes place, the formation of complex solid compounds from three or more constituents. The formation mechanism of BaTi5O11 has been studied as a function of both the thermal treatment and the time reaction. The reaction was monitored by Raman spectroscopy combined with Confocal microscopy, the aim of this characterization technique is strategy and design principles to obtain BaTi5O11 powder. Consequently, this work and structural study of complex inorganic nanoparticles. to provide the description of the general is a challenging task for the compositional and structural study of complex inorganic nanoparticles.