The hybrid spray process that combines arc-spray with HVOF/plasma jet, has recently demonstrated its effectiveness in the deposition of functionally gradient coatings. This approach aims at exploiting the attributes of both the arc-spray technique combined with those of the HVOF/APS technique. This paper presents high speed visualization and plume characterization of an Arc/HVOF hybrid spray gun as well as a twin-wire arc spray gun. The physics of atomization in hybrid spray process is examined using high-speed camera. A DPV-2000 particle diagnostics sensor is used to measure particle velocity, temperature, size and distribution. The influence of feed material, arc-spray parameters, and the jet parameters on the particle characteristics is presented. The differences in the in-flight characteristics between the hybrid and the twin wire arc process have been discussed aided by the observed atomization phenomena with the high speed camera.