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Three perovskite-type materials with a different amount of B-site Ni doping have been tested for their catalytic performance during me-thane dry reforming (MDR) followed by characterization with X-ray dif-fraction (XRD) and scanning electron microscopy (SEM). They could be activated via a reductive treatment (either during a pre-reduction step or di-rectly in reducing reaction atmosphere), the main activating mechanism be-ing the formation of Ni nanoparticles on the surface by exsolution. The catalytic activity increased with the particle size and density. The particle distribution properties could be improved by increasing the amount of Ni doping from 3 % to 10 %, by using an A-site sub-stoichiometric perovskite and by choosing a higher annealing temperature during material prepara-tion. A deactivation over time was observed, due to segregation of CaCO3 on the surface, but no coking or particle sintering occurred