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We report the thermal stability of spherically shaped cobalt-promoted molybdenum disulfide (Co/MoS₂) nano-catalysts from in-situ heating under electron irradiation in the scanning transmission electron microscope (STEM) from room temperature to 550 °C ± 50 °C with aid of Fusion^® holder (Protochip©, Inc.). The catalytic nanoparticles were synthesized via a hydrothermal method using sodium molybdate (Na₂MoO₄·2H₂O) with thioacetamide (CH₃CSNH₂) and cobalt chloride (CoCl₂) as promoter agent. The results indicate that the layered molybdenum disulfide structure with interplanar distance of ~0.62 nm remains stable even at temperatures of 550 °C, as observed in STEM mode. Subsequently, the samples were subjected to catalytic tests in a Robinson Mahoney Reactor using 30 g of Heavy Crude Oil (AGT-72) from the golden lane (Mexico’s east coast) at 50 atm using (ultrahigh purity) UHP hydrogen under 1000 rpm stirring at 350 °C for 8 h. It was found that there is no damage on the laminar stacking of Co/MoS₂ with temperature, with interlayer spacing remaining at 0.62 nm; these sulfided catalytic materials led to aromatics rise of 22.65% and diminution of asphaltenes and resins by 15.87 and 3.53%, respectively.