The microstructural evolution of spray formed materials depends on the thermal and dynamic behavior of the atomized droplets during their trajectory in direction of the substrate, which are governed by process parameters. In the present work, the influence of process parameters on the microstructural behavior of Fe-6.5%Si deposits was studied. The studied parameters were: gas/metal mass flow rate (GMR), the atomization nozzle-to-substrate distance and the substrate material. It was noticed that with the increase of nozzle-to-substrate distance or of the GMR, the porosity volumetric percentage increased, while grain size was reduced. Use of ceramic substrate resulted in porosity decrease and grain size increase when compared to results obtained with the use of water-cooled metallic substrate.