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Synthesis,characterization and in situ monitoring of the mechanochemical reaction process of two manganese(II)-phosphonates with N-containing ligands
Authors:Irina Akhmetova  Konstantin Schutjajew  Manuel Wilke  Ana Buzanich  Klaus Rademann  Christina Roth  Franziska Emmerling
Affiliation:1.Federal Institute for Materials Research and Testing (BAM),Berlin,Germany;2.Institute for Chemistry and Biochemistry,Freie Universit?t Berlin,Berlin,Germany;3.Swiss Light Source, Material Science Beamline, Paul Scherrer Institute (PSI),Villigen,Switzerland;4.Department of Chemistry,Humboldt-Universit?t zu Berlin,Berlin,Germany
Abstract:Two divalent manganese aminophosphonates, manganese mono(nitrilotrimethylphosphonate) (MnNP3) and manganese bis(N-(carboxymethyl)iminodi(methylphosphonate)) (Mn(NP2AH)2), have been prepared by mechanochemical synthesis and characterized by powder X-ray diffraction (PXRD). The structure of the novel compound Mn(NP2AH)2 was determined from PXRD data. MnNP3 as well as Mn(NP2AH)2 exhibits a chain-like structure. In both cases, the manganese atom is coordinated by six oxygen atoms in a distorted octahedron. The local coordination around Mn was further characterized by extended X-ray absorption fine structure. The synthesis process was followed in situ by synchrotron X-ray diffraction revealing a three-step reaction mechanism. The as-prepared manganese(II) phosphonates were calcined on air. All samples were successfully tested for their suitability as catalyst material in the oxygen evolution reaction.
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