This investigation analyzed the effect of reactant particle size on the stress development characteristics of NiAl synthesized through self-propagating high temperature synthesis. Four sample combinations of NiAl were synthesized based on initial particle diameters of the reactants: (i) 10 μm Al and 10 μm Ni (S1), (ii) 10 μm Al and 100 nm Ni (S2), (iii) 50 nm Al and 10 μm Ni (S3), and (iv) 50 nm Al and 100 nm Ni (S4). Characterization of NiAl was performed by parallel comparison of the distribution of residual stresses of the samples prior to and after the reaction. Residual stresses were quantified using x-ray diffraction. Upon characterization it was found that combinations S1, S2, and S3 exhibited tensile residual stresses, while combination S4 exhibited compressive residual stresses. Statistical analysis confirmed that self-propagating high temperature synthesis products derived from nanoparticle reactant sizes exhibited compressive residual stresses offering improved fatigue resistance in composite production.