title: Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu3-xP.
abstract: Polycrystalline Cu3-xP was successfully synthesized in different ionic liquids comprising imidazolium and phosphonium cations. The reaction of elemental copper and red phosphorus in trihexyltetradecylphosphonium chloride at 200 °C led to single-phase Cu3-xP (x = 0.05) within 24 h with a quantitative yield (99%). Liquid-state nuclear magnetic resonance spectroscopy of the ionic liquids revealed degeneration of the imidazolium cations under the synthesis conditions, while phosphonium cations remain stable. The solid products were characterized with X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, solid-state nuclear magnetic resonance spectroscopy, and elemental analysis. A reinvestigation of the electronic transport properties of Cu2.95(4)P showed metallic behavior for the bulk material. The formation of CuP2 during the synthesis of phosphorus-rich Cu3-xP (x ≥ 0.1) was observed.
authors: Alexander
authors: A
authors: Wolff
authors: Julia
authors: J
authors: Pallmann
authors: Richard
authors: R
authors: Boucher
authors: Alexander
authors: A
authors: Weiz
authors: Eike
authors: E
authors: Brunner
authors: Thomas
authors: T
authors: Doert
authors: Max Planck Institute for Chemical Physics of Solids , 01187 Dresden, Germany.
authors: Michael
authors: M
authors: Ruck