Catalysts of Ni-Rh/SiO2, Rh/SiO2, and Ni/SiO2 were prepared by the incipient wetness method and characterized with techniques of thermomagnetometry and H-2 NMR spectroscopy. The Ni/SiO2 showed a Curie temperature around 635 K. On the contrary, no Curie transition temperature was observed for all the Rh-Ni/SiO2 catalysts. Observed chemical shifts of deuterium adsorbed on Ni/SiO2 and Rh/SiO2 catalysts were -38 and -60 ppm, respectively, under 300 Torr D-2, while the bimetallic Ni-Rh/SiO2 catalysts showed a more downfield shift. Further, the observed chemical shift for the bimetallic catalysts also showed a Ni/Rh ratio dependent and shifted toward upfield with Ni/Rh ratio; the chemical shift finally approached that of Ni/SiO2 ( - 38 ppm) as the Ni/Rh ratio was higher than five. These occurrences were attributed to the formation of bimetallic Ni-Rh alloy.