Rapid synthesis of high-purity molybdenum carbide with controlled crystal phases

The synthesis of phase-pure carbide nanomaterials is crucial for understanding their structure-performance relationships, and for advancing their application in catalysis. Molybdenum carbides, in particular, have garnered increasing interest due to their Pt-like surface electronic properties and high catalytic activity. Traditional methods for synthesizing molybdenum carbide are often lengthy and energy-intensive, leading to an uncontrolled phase, low purity, and excessive carbon coverage, which hinder their catalytic performance improvement. This work introduces a novel pulsed Joule heating (PJH) technique that overcomes these limitations, enabling the controlled synthesis of high-purity molybdenum carbides (β-Mo 2 C, η-MoC 1− x , and α-MoC 1− x ) within seconds by using MoO x /4-Cl- o -phenylenediamine as the hybrid precursor. The PJH method allows precise control over the diffusion of carbon species in the Mo-C system, resulting in a significantly improved phase purity of up to 96.89 wt%. Moreover, the electronic structure of platinum catalysts on molybdenum carbide was modulated through electron metal-support interaction (EMSI) between Pt and Mo x C, and contributed to enhanced catalytic performance compared to carbon-supported Pt catalysts during the hydrogen evolution reaction. Overall, this work paves the way for efficient production of high-quality molybdenum carbide nanomaterials, and thus is expected to accelerate their industrial deployments in practical catalytic reactions. A kinetic controllable method for the preparation of phase-pure molybdenum carbide phase, α-MoC 1− x , η-MoC 1− x , and β-Mo 2 C was determined by adjusting the continuous pulsed Joule heating.