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The development of efficient and cost-effective catalysts for hydrogen evolution reaction (HER) is crucial for the advancement of electrochemical water splitting technology. Here, we report a novel synthetic method for the preparation of single-crystalline NiCoP nanorods with tunable aspect ratios using a CO-assisted, trioctylphosphine (TOP)-mediated approach. The introduction of CO gas at different temperatures allows for the control of the nanorod growth, resulting in various aspect ratios while maintaining a hexagonal crystal structure and a composition of 1:1 Ni/Co as NiCoP. Our results demonstrate that the NiCoP nanorods with higher aspect ratios exhibit improved HER activity and stability, with the highest aspect ratio nanorods showing the lowest overpotential and Tafel slope in both acidic and alkaline media. This study highlights the importance of controlling the size and morphology of bimetallic phosphide nanoparticles to optimize their catalytic activity for HER, providing new insights into the design and optimization of nanostructured catalysts for electrochemical water splitting applications.