“…Some groups have applied such analysis techniques as SEM (scanning electron microscopy) and even optical microscopy to detect the first signs of degradation of barrier integrity by appearance of defects on the surface of the barrier layer or the copper film, or appearance of etch pits after chemical removal of the barrier layer and selective etching of silicon (see, e.g., [5,15,18,20,82,99,100,103]). Plan view and cross-sectional TEM analyses (see, e.g., [11,14,19,21,71,93,96,98,101,104]) were used to detect interaction at the interfaces, degradation of the interface sharpness, and formation of spikes of Cu-silicide at the interface, or to measure Cu or Al concentration at different depths of the barrier layers using EDX (energy-dispersive X-ray spectroscopy) [90,99,105].…”