This paper describes the use of non-linear ultrasonic techniques for the characterization of material degradation in 99.98% pure copper due to high-temperature creep. Flat dog-bone-shaped specimens were subjected to constant load creep testing at different stress and temperature levels. Creep damage progression was monitored by conducting continuous and interrupted mode creep tests. In the case of continuous loading non-linear ultrasonic (NLU) measurements were conducted after fracture at different locations along the gage length of the sample. For interrupted tests the NLU measurements were conducted on different creep life fractions, through periodic interruption of the creep test. In all cases a through transmission NLU measurement technique was employed. Three different non-linear measurements, namely static displacement, second harmonic and third harmonic, were taken and their responses compared. The NLU measurements were found to be significantly sensitive to the extent of creep damage (∼200-2500% of base level), while the linear ultrasonic measurements, representing the change in longitudinal velocities, were only in the range 10-30% for a comparable creep damage level. NLU measurements carried out on fractured samples suggest that the NLU response was locally high at locations where the creep damage was concentrated, compared with other locations, even within the gage length of the specimen. This was confirmed using micrograph observations. Of the three non-linear measurements, the third harmonic data was most sensitive to creep damage. © 2009 Acta Materialia Inc.