Ruthenium dioxide (RuO2) shows excellent activity toward the acidic oxygen evolution reaction (OER); however, its practical application is limited by poor long-term stability. Herein, a single-phase Mo0.5Ru0.5O2 nanoparticle catalyst is reported with a high Mo content, synthesized via high-temperature thermal shock treatment under an oxygen atmosphere (HTSO), exhibiting high activity and stability in OER. The HTSO technique involves rapidly heating the precursor to ≈1200 °C for ≈0.05 s in oxygen, followed by immediate quenching at a rate of ≈104 °C s-1. The resulting nanoparticles exhibit a uniform size of ≈10 nm and homogeneous elemental mixing, overcoming the thermodynamic barriers that typically lead to phase separation in conventional synthesis methods. The Mo0.5Ru0.5O2 catalyst achieves an overpotential of 210 mV at 10 mA cm-2 and maintains stable performance over 300 h at 50 mA cm-2 in OER, significantly surpassing the stability of RuO2 and other reported high-metal-content doped RuO2 catalysts. High-valence Mo, with its multiple accessible oxidation states and compatible ionic radius, serves as an ideal dopant for RuO2, enabling stable lattice substitution, effective electron donation, and ultimately suppressing Ru over-oxidation while enhancing stability. This approach enhances catalyst stability and Ru utilization, providing a versatile platform for synthesizing other metal-doped RuO2 systems toward cost-effective and stable OER catalysts.