Microwave-Assisted Solid-State Synthesis of Catalytically Relevant Potassium Intercalated Molybdenum Chalcogenides

The demand for large scale sustainable energy solutions for a posthaste evolving energy landscape calls for the development of transformative materials with the ability to mediate sustainable renewable energy conversion. Molybdenum chalcogenides like molybdenum dichalcogenides and Chevrel phases (CPs), M_yMo₆X₈ (M = alkali, alkaline, transition, post-transition, and lanthanide metals; X = S, Se, Te) have shown promise as electrocatalysts for the hydrogen evolution reaction (HER), carbon dioxide reduction (CO₂R) and the oxygen reduction reaction (ORR). However, efficient, and selective electrochemical conversion is hindered by achieving controlled bonding affinity of key intermediates (e.g. CO_ads). Chevrel phases and extended Mo-Mo chain phases offer a unique platform to study structure function relationships in ternary materials in part to their tunable framework. This work presents a facile microwave-assisted solid-state method to access KMo₆S₈ and K_xMo₁₅S₁₉ (x = 1.89, 2.42), in addition to full characterization of materials. HER experiments were carried out on K_1.89Mo₁₅S₁₉ and K_2.42Mo₁₅S₁₉ to see how potassium content affects charge transfer, in addition to preliminary CO₂R experiments with KMo₆S₈ and K_xMo₁₅S₁₉.