This study presents a groundbreaking approach to heavy oil upgrading using water-soluble nickel acetate as a precatalyst, marking a shift from traditional oil-soluble catalysts. We demonstrate that nickel and copper acetates significantly enhance aquathermolysis, reducing the viscosity of heavy oil by almost 58% and the high-molecular-weight fractions from 38.3 to 23.5 wt % while increasing the lighter fractions from 61.7 to 76.5 wt %. The catalytic action of nickel and copper acetates facilitates the structural and compositional transformation of heavy oil, evidenced by the increased H/C atomic ratio and 30% reduction in the initial boiling point. Further, these catalysts yield an increase in light distillate production and promote the formation of stable free radicals, indicating a higher degree of hydrocarbon decomposition. Analytical techniques, including thermogravimetric analysis, kinetic analysis, X-ray diffraction, and scanning electron microscopy, confirm the effective decomposition of nickel and copper acetates into active nickel and copper species, predominantly nanoparticles smaller than 58 nm. The study underlines the potential of water-soluble catalysts such as nickel and copper acetates to enhance steam-based oil recovery and upgrading processes, offering a cost-effective and environmentally friendlier alternative to conventional methods. The ongoing research promises to solidify the role of catalysts in sustainable energy production.