Nanopowders of pure nickel were directly synthesized for the first time by conventional solution combustion synthesis (SCS) method. In this article, a specific reaction pathway is suggested to describe the metallic phase formation during SCS. It is proposed that the exothermic reaction between NH3 and HNO3 species formed during the decomposition of glycine and nickel nitrate acts as the source of energy required to achieve the self-sustained reaction regime. A thermodynamic analysis of the combustion synthesis reaction indicates that increasing glycine concentration leads to establishing a hydrogen rich reducing environment in the combustion wave that in turn results in the formation of pure metals and metal alloys. TGA of reaction systems and XRD analysis of products in the quenched combustion wave show that the formation of oxide phases occurs in the reaction front, followed by gradual reduction of oxide to pure metallic phases in the postcombustion zone. A methodology for SCS of pure metals and metal alloys nanoparticles can be inferred from the results presented. (C) 2010 American Institute of Chemical Engineers AIChE J, 57: 2207-2214, 2011