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Journal Article

Resource-Efficient High-Yield lonothermal Synthesis of Microcrystalline Cu3-xP


Ruck,  Michael
Michael Ruck, Max Planck Fellow, Max Planck Institute for Chemical Physics of Solids, Max Planck Society;

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Wolff, A., Pallmann, J., Boucher, R., Weiz, A., Brunner, E., Doert, T., et al. (2016). Resource-Efficient High-Yield lonothermal Synthesis of Microcrystalline Cu3-xP. INORGANIC CHEMISTRY, 55(17), 8844-8851. doi:10.1021/acs.inorgchem.6b01397.

Cite as: https://hdl.handle.net/11858/00-001M-0000-002B-A089-3
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 degrees 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 CuP2 during the synthesis of phosphorus-rich Cu3-xP (x >= 0.1) was observed.