A combination of electron microscopy and Auger depth profiling techniques was found useful in characterizing the interface zones of plated aluminum alloys. The pre-electroplating procedures examined were; zincate, Alcoa 661 Process, Alstan, and phosphoric acid anodizing. Good adhesion of electrodeposited nickel can be obtained on aluminum alloys. Failure of plated specimens in peel tests is by ductile fracture of the aluminum alloy substrate, except in the case of the anodic pretreatment where failure is principally through the oxide coating. To obtain best peel test results using the anodic pretreatment, the anodizing parameters must be tailored to the specific alloy that is to be plated.