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|Dokument Type:||Article||metadata.dc.title:||Synthesis and characterization of methylammonium phosphates as crystalline approximants for anhydrous, low melting phosphate glasses||Authors:||Schmedt auf der Günne, Jörn ItemCrisRefDisplayStrategy.rp.unknown.icon
Wied, Jan Konrad
|Institute:||Department Chemie - Biologie||Free keywords:||Phosphate glasses||Dewey Decimal Classification:||540 Chemie||GHBS-Clases:||UQL
|Issue Date:||2019||Publish Date:||2021||Source:||RSC Advances, 9(4), S. 1822 - 1830. - https://doi.org/10.1039/C8RA07736C||Abstract:||
Low-melting methylammonium phosphate glasses are synthesized from crystalline starting agents. To this end crystalline tris(methylammonium) cyclotriphosphate [CH3NH3]3P3O9, was synthesized by a novel and simple synthesis route from P4O10 and N-methylformamide. It, undergoes an irreversible phase transition to methylammonium catena-polyphosphate [CH3NH3]PO3. The crystal structure of the catena-polyphosphate was solved and refined from X-ray powder diffraction data by the Rietveld method using constraints obtained by solid-state 31P and 1H NMR spectroscopy. This compound crystallizes in a triclinic space group with a = 13.2236(9), b = 7.8924(6), c = 4.6553(2) Å, α = 91.068(4), β = 87.840(5) and γ = 106.550(3)°. Quantum chemical calculations confirm that the obtained structure lies at an energetic minimum. Finally the reaction of tris(methylammonium) cyclotriphosphate and P4O10 into methylammonium phosphate glass is presented. The synthesized, water-free phosphate glass shows a very low glass transition temperature Tg of 33 °C, which was verified by dynamic scanning calorimetry and NMR. The chain-like crystal structure of the high-temperature methylammoniumphosphate [CH3NH3]PO3 serves as an approximation for the short-range order of the glass.
Finanziert aus dem DFG-geförderten Open-Access-Publikationsfonds der Universität Siegen für Zeitschriftenartikel
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