Time-resolved, in situ spectroscopy of electroless (EL) gold (Au) films combined with electron microscopy showed that the deposition rate increased up to two-fold on surfaces swept by the bulk flow of adjacent fluid at Reynolds numbers less than 1.0, compared to batch immersion. Deposition rates from 5.0 to 9.0 nm/min and thicknesses of the EL Au film from 20 to 100 nm, respectively, increased predictably with flow rate at conditions when the deposition was limited primarily by Fickian diffusion. Time-frames were identified for metal island nucleation, growth, and subsequent film development during EL Au deposition by real-time UV-visible spectroscopy of photoluminescence (PL) and surface plasmon features of nanoscale metal deposits. Film thicknesses measured by scanning electron microscopy and X-ray photoelectron spectroscopy paired with real-time optical spectroscopy of kinetic aspects of plasmon and PL optical features indicated that Au film deposition on surfaces swept by a steady flow of adjacent fluid can be primarily diffusion limited.