Scanning Electron Microscopy of an 8 μm Thick ZrO2 Film
This abstract reports the occurrence of 'breakaway oxidation' for unalloyed zirconium in 300°C oxygen. An excellent review of zirconium and zirconium alloy oxidation can be found elsewhere (1).Approximately one dozen crystal bar zirconium coupons were placed in a resistance wound furnace held at 300°C and through which oxygen (initially passed through a silica gel dessicant) was passed. Over a period of three years, the samples accumulated over 700 days of oxidation time. The kinetics followed a rate law between cubic and parabolic until achieving an oxide thickness approximately 350 nm at which point 'breakaway' occurred. For instance, in one year the film increased in thickness from 0.35 to more than 8 μm. These thick, post-transition oxides were examined in the SEM.The samples were characterized by regions approximately 40 μm in diameter which spalled with a density of about 45 per cm2.