We report on atomic force microscopy (AFM) studies of polyaniline (PANI) nanostructures formed during different stages of in situ film growth. Surface topography and single molecule force spectroscopy results indicate that early stage and late stage growth of PANI exhibit different morphologies and mechanical properties, while current–voltage response curves from conductive-AFM experiments indicate that late stage growth of PANI should be minimized to optimize conductive properties. Surface images of PANI films synthesized via short reaction times reveal the limited growth of black PANI precipitates, showing promise for the improved electrical behavior of polyaniline films.