A fundamental goal of ultrasonic nondestructive evaluation is to characterize material defects before failure. During material fatigue, dislocations tend to nucleate, becoming sources of stress concentration. Eventually, cracks start to form and lead to material failure. Recent research has indicated that nonlinear harmonic generation can be used to distinguish between materials of high and low dislocation densities. This research reports nonlinear harmonic generation measurements to distinguish between those areas of high and low dislocation densities in copper bars. The copper bars were subjected to flexural fatigue. Periodic scans were taken in order to track dislocation development during the fatigue life of the material. We show that this technique provides improved early detection for critical components of failure.