Gold nanoparticles have been extensively studied for their applications in catalysis. For Au nanoparticles to be catalytically active, controlling the particle size is crucial. Here we present a low temperature (105 °C) thermal atomic layer deposition approach for depositing gold nanoparticles on TiO2 with controlled size and loading using trimethylphosphino-trimethylgold (III) and two co-reactants (ozone and water) in a fluidized bed reactor. We show that the exposure time of the precursors is a variable that can be used to decouple the Au particle size from the Au loading. Longer exposures of ozone narrow the particle size distribution while longer exposures of water broaden it. By studying the photocatalytic activity of Au/TiO2 nanocomposites we show how the ability to control particle size and loading independently can be used not only to enhance performance but also to investigate structure-property relationships. This study provides insights into the mechanism underlying formation and evolution of Au nanoparticles via a vapor phase technique which eliminates the shortcomings of conventional liquid-base processes.