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Issue 4, 2019, Issue in Progress
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Synthesis and characterization of methylammonium phosphates as crystalline approximants for anhydrous, low melting phosphate glasses

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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.

Graphical abstract: Synthesis and characterization of methylammonium phosphates as crystalline approximants for anhydrous, low melting phosphate glasses

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Supplementary files

Article information


Submitted
17 Sep 2018
Accepted
27 Dec 2018
First published
15 Jan 2019

This article is Open Access

RSC Adv., 2019,9, 1822-1830
Article type
Paper

Synthesis and characterization of methylammonium phosphates as crystalline approximants for anhydrous, low melting phosphate glasses

M. Mangstl, J. K. Wied, J. Weber, C. Pritzel, R. Trettin and J. Schmedt auf der Günne, RSC Adv., 2019, 9, 1822
DOI: 10.1039/C8RA07736C

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