Detailed Record



Intercalation-Induced Topotactic Phase Transformation of Tungsten Disulfide Crystals


Abstract Recent research has demonstrated the potential for topological superconductivity, anisotropic Majorana bound states, optical nonlinearity, and enhanced electrochemical activity for transition metal dichalcogenides (TMDs) with a 2M structure. These unique TMD compounds exhibit metastability and, upon heating, undergo a transition to the thermodynamically stable 2H phase. The 2M phase is commonly made at high temperatures using traditional solid-state methods, and this metastability further complicates the growth of large 2M WS2 crystals. Herein, a novel synthetic method was developed, focusing on a molten salt reaction to synthesize large 2H crystals and then inducing transformation to the 2M phase through intercalation and thermal treatment. The 2H crystals were intercalated via a room-temperature sodium naphthalenide solution, producing a previously unreported Na-intercalated 2H WS2 phase. Thermal heating was required to facilitate the phase transition to the intercalated 2M crystal structure. This phase transition was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), electron dispersive X-ray spectroscopy (EDS), and Raman spectroscopy, which confirmed the synthesis of the intercalated 2M phase. Upon deintercalation, crystal and powder samples showed superconductivity with a Tc of 8.6–8.7 K, similar to previously reported values. The generality of this process was further demonstrated using alkali metal triethyl borohydride to intercalate 2H WS2 and produced the desired 2M phase. This novel synthetic method has broad implications for discovering metastable phases in other TMD families and layered materials. Separation of the intercalation and phase transition also has the potential to allow for large-scale synthesis of this technologically important phase with greater control over each step of the reaction.
Authors Alamgir Hossain University of Wyoming , Joseph McBride University of Wyoming , Masoumeh Mahmoudi Gahrouei University of Wyoming , Sabin Gautam University of Wyoming , J. Carter University of Wyoming , Piumi Samarawickrama University of Wyoming , John Ackerman University of Wyoming , Laura de Sousa Oliveira University of WyomingORCID , Jinke Tang University of WyomingORCID , Jifa Tian University of WyomingORCID , Brian M. Leonard University of WyomingORCID
Journal Info American Chemical Society | Chemistry of Materials
Publication Date 12/17/2024
ISSN 0897-4756
TypeKeyword Image article
Open Access closed Closed Access
DOI https://doi.org/10.1021/acs.chemmater.4c02160
KeywordsKeyword Image Selected area diffraction (Score: 0.49792123) , Metastability (Score: 0.45440525) , Crystal (programming language) (Score: 0.4534001)