The synthesis and microstructural evolutions of the NiAl-15 wt% (Al2O3-13% TiO2) nanocomposite powders were studied. These nanocomposite powders are used as feedstock materials for thermal spray applications. These powders were prepared using high and low-energy mechanical milling of the Ni, Al powders and Al2O3-13% TiO2 nanoparticle mixtures. High and low-energy ball-milled nanocomposite powders were also sprayed by means of high-velocity oxy fuel (HVOF) and air plasma spraying (APS) techniques respectively. The results showed that the formation of the NiAl intermetallic phase was noticed after 8 h of high-energy ball milling with nanometric grain sizes but in a low-energy ball mill, the powder particles contained only alpha-Ni solid solution with no trace of the intermetallic phase after 25 h of milling. The crystallite sizes in HVOF coating were in the nanometric range and the coating and feedstock powders showed the same phases. However, under the APS conditions, the coating was composed of the NiAl intermetallic phase in the alpha-Ni solid solution matrix. In both of the nanocomposite coatings, reinforcing nanoparticles (Al2O3-13% TiO2) were located at the grain boundaries of the coatings and pinned the boundaries, therefore, the grain growth was prohibited during the thermal spraying processes. (C) 2014 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.