Multilayer films of metal-peptide dendrimers having a ferrocene core were constructed on gold surfaces functionalized with mercaptoundecanoic acid using a layer-by-layer approach for film construction. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to monitor the redox activity and stability of these films. The multilayer films showed good stability and exhibited direct electron transfer with the underlying electrode. The specific active surface concentration can be varied by the number of layers, the nature of the dendrimer, and the nature of metal ions used. (C) 2008 Wiley Periodicals, Inc. J Appl Polym Sci 111: 709-723, 2009