The study addresses layer-by-layer formation processes and properties of gold nanoparticle films deposited from reverse micellar solutions of Brij 30 surfactant on rigid glass and flexible polymer (PET) substrates. The films are of interest for transparent electronics and optical sensorics. The spectrophotometric studies of film formation revealed linear relationships between the extinction of growing film at definite wavelengths and the number of nanoparticle deposition cycles, and their parameters were determined. The effects of concentrations of gold and 1,2-ethanedithiol as an interlayer linker in the initial solutions on the film growth were elucidated. Data on the composition, morphology, optical spectra, and surface resistance of gold nanoparticle films, and changes of these characteristics during heat treatment in air and in boiling ethanol were gained using X-ray diffractometry, scanning electron and atomic force microscopy, UV-Vis spectroscopy, and electrical resistance measurements.