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Structural Properties and ELNES of Polycrystalline and Nanoporous Mg3N2

Published online by Cambridge University Press:  10 January 2020

Olivia Wenzel ,
Viktor Rein ,
Radian Popescu ,
Claus Feldmann  and
Dagmar Gerthsen
Olivia Wenzel*
Affiliation:
Laboratory for Electron Microscopy (LEM), Karlsruhe Institute of Technology (KIT), Engesserstr. 7, 76131Karlsruhe, Germany
Viktor Rein
Affiliation:
Institute for Inorganic Chemistry (AOC), Karlsruhe Institute of Technology (KIT), Engesserstr. 15, 76131Karlsruhe, Germany
Radian Popescu
Affiliation:
Laboratory for Electron Microscopy (LEM), Karlsruhe Institute of Technology (KIT), Engesserstr. 7, 76131Karlsruhe, Germany
Claus Feldmann
Affiliation:
Institute for Inorganic Chemistry (AOC), Karlsruhe Institute of Technology (KIT), Engesserstr. 15, 76131Karlsruhe, Germany
Dagmar Gerthsen
Affiliation:
Laboratory for Electron Microscopy (LEM), Karlsruhe Institute of Technology (KIT), Engesserstr. 7, 76131Karlsruhe, Germany
*
*Author for correspondence: Olivia Wenzel, E-mail: olivia.wenzel@kit.edu
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Abstract

Nanoporous, high-purity magnesium nitride (Mg3N2) was synthesized with a liquid ammonia-based process, for potential applications in optoelectronics, gas separation and catalysis, since these applications require high material purity and crystallinity, which has seldom been demonstrated in the past. One way to evaluate the degree of crystalline near-range order and atomic environment is electron energy-loss spectroscopy (EELS) in a transmission electron microscope. However, there are hardly any data on Mg3N2, which makes identification of electron energy-loss near-edge structure (ELNES) features difficult. Therefore, we have studied nanoporous Mg3N2 with EELS in detail in comparison to EELS spectra of bulk Mg3N2, which was analyzed as a reference material. The N-K and Mg-K edges of both materials are similar. Despite having the same crystal structure, however, there are differences in fine-structural features, such as shifts and absences of peaks in the N-K and Mg-K edges of nanoporous Mg3N2. These differences in ELNES are attributed to coordination changes in nanoporous Mg3N2 caused by the significantly smaller crystallite size of 2–6 nm compared to the larger (25–125 nm) crystal size in a bulk material.

Keywords

crystal size effectselectron energy-loss spectroscopymagnesium nitridesurface effects
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 26 , Issue 1 , February 2020 , pp. 102 - 111
Copyright
Copyright © Microscopy Society of America 2020

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