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The tin-free electroless metallization process developed in our laboratory consists in attaching the Pd(+ 2)-based catalyst on surfaces which were previously grafted with nitrogen-bearing groups. The so-functionalized surfaces lead to the formation of true covalent bonds between palladium and nitrogen-based species. In this work, the different steps of the process are studied, namely: (i) the grafting of nitrogen-bearing groups on an insulating surface by various processes already used in our laboratory, (ii) the seeding of the surface with Pd(+ 2) species, (iii) the reduction of Pd(+ 2) to Pd(0) by different routes (this step is needed due to the use of industrial plating baths which contain strong stabilizers that prevent or delay plating), (iv) the Ni metallization using low- and high-phosphorus plating baths. Phosphorus which originates from the plating bath reducer is partly incorporated in the Ni films and creates some stresses. Adhesion of the resulting films is evaluated by the Scotch® tape test. The main parameters responsible for adhesion and governing the characteristics of the Ni film/substrate interface are: the nature of the substrate, the Pd(+ 2) reduction route and the phosphorus content of the Ni plating bath. All these parameters influence the amount of stresses generated both at the metal/substrate interface and within the film.