A highly dispersed supported Rh catalyst was successfully prepared by an arc-plasma process for the first time and was characterized by means of TEM, XPS and EXAFS. Repeated generation of pulsed arc-plasma using a Rh rod as a cathode was found to deposit crystallized uniform metallic Rh particles with the size of 2.4 +/- 1.1 nm onto the surface of AlPO(4) powders. The metal-support interaction via Rh-O-P bonding in the catalyst prepared using arc-plasma was found to be weaker than in the catalyst prepared by conventional wet impregnation. The arc-plasma catalyst preparation achieved a higher CO oxidation activity because of highly dispersed metallic Rh nanoparticles. (C) 2011 Elsevier B.V. All rights reserved.