P2S5Reactive Flux Method for the Rapid Synthesis of Mono- And Bimetallic 2D Thiophosphates M2- xM′xP2S6

Daniel G. Chica, Abishek K. Iyer, Matthew Cheng, Kevin M. Ryan, Patrick Krantz, Craig Laing, Roberto Dos Reis, Venkat Chandrasekhar, Vinayak P. Dravid, Mercouri G. Kanatzidis*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

18 Scopus citations


We report a reactive flux technique using the common reagent P2S5 and metal precursors developed to circumvent the synthetic bottleneck for producing high-quality single- and mixed-metal two-dimensional (2D) thiophosphate materials. For the monometallic compound, M2P2S6 (M = Ni, Fe, and Mn), phase-pure materials were quickly synthesized and annealed at 650 °C for 1 h. Crystals of dimensions of several millimeters were grown for some of the metal thiophosphates using optimized heating profiles. The homogeneity of the bimetallic thiophosphates MM′P2S6 (M, M′ = Ni, Fe, and Mn) was elucidated using energy-dispersive X-ray spectroscopy and Rietveld refinement. The quality of the selected materials was characterized by transmission electron microscopy and atomic force microscopy measurements. We report two novel bimetallic thiophosphates, MnCoP2S6 and FeCoP2S6. The Ni2P2S6 and MnNiP2S6 flux reactions were monitored in situ using variable-temperature powder X-ray diffraction to understand the formation reaction pathways. The phases were directly formed in a single step at approximately 375 °C. The work functions of the semiconducting materials were determined and ranged from 5.28 to 5.72 eV.

Original languageEnglish (US)
Pages (from-to)3502-3513
Number of pages12
JournalInorganic chemistry
Issue number6
StatePublished - Mar 15 2021

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Physical and Theoretical Chemistry


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