In the present study, ultrafined Zr-V-Fe based alloy powder prepared by a plasma arc discharge process with changing process parameters. The chemical composition of synthesized powder was strongly influenced by the process parameters, especially the hydrogen volume fraction in the powder synthesis atmosphere. The synthesized powder had an average particle size of 50 nm. The synthesized Zr-V-Fe based particles had a shell-core structure composed of metal in the core and oxidse in the shell.