Atom-by-atom deposition of gold into polyaniline (PANI) through a repeated cyclic pathway has been reported previously by us. It was noticed that the efficiency of the preparation was complicated by concurrent oxidative degradation of PANI in the course of the gold deposition process, resulting in the loss of the deposited matrix. The primary objective of this research was to minimize the loss of the matrix by separating the PANI degradation and the atomic gold deposition parts of the cycle. The overoxidation of PANI was performed as a preconditioning step, prior to the gold deposition cycles. The FTIR spectra obtained after preconditioning on the stabilized PANI film show that the imine attachment sites for the chloroaurate anion are still available.. The presence of the deposited gold on the cyclic voltammograms of the PANI film could be easily observed. The work function of the prepared composite films increased linearly with the logarithm of number of gold deposition cycles. (C) 2011 The Electrochemical Society. [DOI: 10.1149/2.052112jes] All rights reserved.