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Boucher, Richard
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article
Resource-Efficient High-Yield Ionothermal Synthesis of Microcrystalline Cu3-xP
Abstract
<p>Polycrystalline Cu<sub>3-x</sub>P 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 Cu<sub>3-x</sub>P (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 Cu<sub>2.95(4)</sub>P showed metallic behavior for the bulk material. The formation of CuP<sub>2</sub> during the synthesis of phosphorus-rich Cu<sub>3-x</sub>P (x ≥ 0.1) was observed.</p>