The study of influence of Fe and Ti alloying elements in the Ni3Al intermetallic alloy on diffusion feature in Ni/Ni3Al-Me (Me = Fe or Ti) joints was performed using the diffusion couple technique. Four sets of diffusion couples of diverse compositions prepared by means of resistance welding or electron beam welding in vacuum were used. The concentrations profiles and diffusivities of welded Ni/Ni3Al-Fe and Ni/Ni3Al-Ti joints were determined after annealing at 1050°C for 100 hours. The concentration profiles were smoothed using suitable types of polynomials. The Kirkendall voids in the area between the Matano plane and the new interface created after annealing were observed. Metallographic study and qualitative evaluation of voids by means of AFM method revealed different feature of Kirkendall regions in Ni/Ni3Al-Fe couples unlike Ni/Ni3Al-Ti joints.