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In the presented study, a novel approach for thermal atomic layer deposition (ALD) of Al₂O₃ thin films using plasma-activated water (PAW) as a co-reactant, replacing traditionally employed deionized (DI) water, is introduced. Utilizing ex situ PAW achieves up to a 16.4% increase in the growth per cycle (GPC) of Al₂O₃ films, consistent with results from plasma-enhanced atomic layer deposition (PEALD). Time-resolved mass spectrometry (TRMS) revealed disparities in CH₄ partial pressures between TMA reactions with DI water and PAW, with PAW demonstrating enhanced reactivity. Reactive oxygen species (ROS), namely H₂O₂ and O₃, are posited to activate Si(100) substrate sites, thereby improving GPC and film quality. Specifically, Al₂O₃ films grown with PAW pH = 3.1 displayed optimal stoichiometry, reduced carbon content, and an expanded bandgap. This study thus establishes “PAW-ALD” as a descriptor for this ALD variation and highlights the significance of comprehensive assessments of PAW in ALD processes.