Calcination-induced catalytic activity of CO oxidation reaction (CO ? 1/2O 2 ? CO 2 ) for an intermetallic, AuZr 3 and a hydride, AuZr 3 H x (x = 4.8) has been studied. The catalytic activities for both samples were originated from the formation of nano-gold particles and nano-crystalline ZrO 2 , result by oxidation upon calcination. Oxidation of the AuZr 3 H x occurred at lower temperature than the AuZr 3 , gave rise to the formation of more homogenous distribution and smaller sizes of nano-gold particles (*5 nm) on ZrO 2 , which were responsible for relatively high catalytic performance. This study provides the possibility of hydrogen absorption treatment being a beneficial process for obtaining nano-composite from intermetallic compounds for catalysts.