Rapid microwave-assisted preparation of binary and ternary transition metal sulfide compounds

Abstract

Rapid microwave-assisted preparation of binary and ternary transition metal sulfide compounds AbstractTransition metal chalcogenides are of interest for energy applications, including energy generation in photoelectrochemical cells and as electrodes for next-generation electrochemical energy storage.Synthetic routes for such chalcogenides typically involve extended heating at elevated temperatures for multiple weeks. We demonstrate here the feasibility of rapidly preparing select sulfide compounds in a matter of minutes, rather than weeks, using microwave-assisted heating in domestic microwaves. We report the preparations of phase pure FeS 2 , CoS 2 , and solid solutions thereof from the elements with only 40 minutes of heating. Conventional furnace and rapid microwave preparations of CuTi 2 S 4 both result in a majority of the targeted phase, even with the significantly shorter heating time of 40 minutes for microwave methods relative to 12 days using a conventional furnace. The preparations we describe for these compounds can be extended to related structures and chemistries and thus enable rapid screening of the properties and performance of various compositions of interest for electronic, optical, and electrochemical applications.

Protocols for High Temperature Assisted-Microwave Preparation of Inorganic Compounds

“…59,60 Butala et al demonstrated microwave preparation of Fe 1−x Co x S 2 and CuTi 2 S 4 , accelerating reaction times to less than 40 minutes. 61 The microwave electromagnetic field interacts strongly with the transition metal, selectively heating the metal powder and allowing the reaction to occur rapidly at metal sites before significant sublimation of the chalcogen. 11,15 Since chalcogens are usually weakly absorbing, they do not heat up as quickly, which is advantageous because of issues of pressure build-up in the ampoule.…”

Direct Nano‐Synthesis Methods Notably Benefit Mg‐Battery Cathode Performance

“…While a wide variety of synthetic methods have been developed to directly prepare nano‐sized oxide and binary sulfide materials, most ternary sulfides are prepared with a high‐temperature solid state synthesis that produces micron‐sized particles. [ 48–50 ] In these cases, nano‐sized particles must be obtained post‐synthesis through a mechanical ball milling process.…”

Design Principles for Multinary Metal Chalcogenides: Toward Programmable Reactivity in Energy Conversion

“…The complex nature of the interplay between dimensionality and electrocatalytic reactivity in dimensionally controlled chalcogenides remains to be fully unraveled. However, there are many examples of solid-state, , hydrothermal/solvothermal, , chemical vapor deposition, − ionic liquid, and surfactant-assisted , methodologies for synthesizing dimensionally and compositionally controlled chalcogenide structures. Zhang et al synthesized the entire range of 0D–3D structures based on thioarsenate motifs in their work where polyvinylpyrrolidone, polyethylene glycol-400, and 1-hexadecyl-3-methylimidazolium chloride were used as surfactants to generate 0D [NH 4 ] 8 [Mn 2 As 4 S 16 ], 1D [Mn­(NH 3 ) 6 ]­[Mn 2 As 2 S 8 (N 2 H 4 )], 2D [enH]­[Cu 3 As 2 S 5 ], and 3D [NH 4 ]­[MnAs 3 S 6 ] .…”

“…The complex nature of the interplay between dimensionality and electrocatalytic reactivity in dimensionally controlled chalcogenides remains to be fully unraveled. However, there are many examples of solid-state, 57,58 hydrothermal/solvothermal, 59,60 chemical vapor deposition, 61−63 ionic liquid, 64 and surfactant-assisted 65,66 67 Additional studies involving surfactants for the synthesis of chalcogenide materials extended this methodology to other new 2D selenidostannates, 68 oxosulfides, 69 chalcogenidogermanates, 70 and numerous others. 65,66 The successful linking of chalcogenide motifs through surfactant chemistry is a very promising route toward novel composites having dimensionality-directed physicochemical properties, and may therefore offer a low-cost and scalable alternative to existing solid-state synthetic methods.…”