Scalable Bulk Synthesis of Phase-Pure γ-Sn 3 N 4 as a Model for an Argon-Flow-Mediated Metathesis Reaction.

Autor: Zipkat M; Department of Chemistry, University of Munich (LMU), Butenandtstraße 5-13, (D) 81377, Munich, Germany., Koldemir A; Institut für Anorganische und Analytische Chemie, Universität Münster, Corrensstraße 30, 48149, Münster, Germany., Block T; Institut für Anorganische und Analytische Chemie, Universität Münster, Corrensstraße 30, 48149, Münster, Germany., Ceniza C; Department of Physics and Engineering Physics, University of Saskatchewan, 116 Science Place, Saskatoon, Saskatchewan, S7N SE2, Canada., Boyko TD; Canadian Light Source, 44 Innovation Blvd, Saskatoon, Saskatchewan, S7N SE2, Canada., Kläger S; Department of Chemistry, University of Munich (LMU), Butenandtstraße 5-13, (D) 81377, Munich, Germany., Pritzl RM; Department of Chemistry, University of Munich (LMU), Butenandtstraße 5-13, (D) 81377, Munich, Germany., Moewes A; Department of Physics and Engineering Physics, University of Saskatchewan, 116 Science Place, Saskatoon, Saskatchewan, S7N SE2, Canada., Pöttgen R; Institut für Anorganische und Analytische Chemie, Universität Münster, Corrensstraße 30, 48149, Münster, Germany., Rudel SS; Department of Chemistry, University of Munich (LMU), Butenandtstraße 5-13, (D) 81377, Munich, Germany., Schnick W; Department of Chemistry, University of Munich (LMU), Butenandtstraße 5-13, (D) 81377, Munich, Germany.
Jazyk: angličtina
Zdroj: Chemistry (Weinheim an der Bergstrasse, Germany) [Chemistry] 2024 Nov 18, pp. e202403745. Date of Electronic Publication: 2024 Nov 18.
DOI: 10.1002/chem.202403745
Abstrakt: Nitrides represent a promising class of materials for a variety of applications. However, bulk synthesis remains a challenging task due to the stability of the N 2 molecule. In this study, we introduce a simple and scalable approach for synthesizing nitride bulk materials. Moderate reaction temperatures are achieved by using reactive starting materials, slow and continuous mixing of the starting materials, and by dissipating heat generated during the reaction. The impact on the synthesis of using different starting materials as nitrogen source and the influence of a flux were examined. γ-Sn 3 N 4 was selected as the model compound. The synthesis of pure γ-Sn 3 N 4 bulk material on a large scale has still been a challenge, although a few synthesis methods were already described in the literature. Here we synthesized γ-Sn 3 N 4 by metathesis reaction of argon-diluted SnCl 4 with Li 3 N, Mg 3 N 2 or Ca 3 N 2 as nitrogen sources. Products were characterized by powder X-ray diffraction, scanning and transmission electron microscopy, energy-dispersive X-ray spectroscopy, dynamic flash combustion analysis, hot gas extraction analysis, X-ray photoelectron spectroscopy, Mössbauer spectroscopy and X-ray absorption and emission spectroscopy. Additionally, single-crystal diffraction data of γ-Sn₃N₄, previously unavailable, were successfully collected.
(© 2024 The Author(s). Chemistry - A European Journal published by Wiley-VCH GmbH.)
Databáze: MEDLINE
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