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

Abstract

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-Mo₂C, 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_xC, 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.