Mechanochemical Synthesis and Micro-Electron Diffraction Analysis of Rare Earth-Aminopolycarboxylate Coordination Compounds

Ecem Celik; Pierre LeMagueres; Eric W. Reinheimer; Korey Prescott Carter; Tori Forbes

doi:10.1039/D5CE00935A

$Mechanochemical Synthesis and Micro-Electron Diffraction Analysis of Rare Earth-Aminopolycarboxylate Coordination Compounds$

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Mechanochemical Synthesis and Micro-Electron Diffraction Analysis of Rare Earth-Aminopolycarboxylate Coordination Compounds

Ecem Celik, Pierre LeMagueres, Eric W. Reinheimer, Korey Prescott Carter and Tori Forbes

CrystEngComm, Vol.28(1), pp.255-269

2026

DOI: 10.1039/D5CE00935A

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Abstract

Mechanochemical synthesis offers novel pathways to new materials that are inaccessible via traditional solvent-based approaches. In this work, we evaluate how mechanochemical synthetic variables (e.g. time, frequency, liquid assisted grinding (LAG), metal precursors) impact the products obtained for reactions within the La(III) and ethylenediaminetetraacetic acid (EDTA) system. We found that tuning mechanochemical parameters (i.e., time and frequency) affect reactivity and use of different La(III) salt precursors (La2O3, LaCl3•7H2O, LaPO4•xH2O, La(NO3)3•6H2O, and La(OOCCH3)3•1.5H2O) led to variations in solid-state products. Reactivity trends were largely consistent with trends in the relative lattice energies of the lanthanum starting materials, with the outlier (La2O3) potentially undergoing additional hydroxylation on particle surfaces during LAG. Two products were successfully isolated and structurally characterized using electron diffraction, including a 1-D chain and a 2-D sheet prepared from La2O3 (LaEDTA1) and LaCl3•7H2O (LaEDTA2), respectively. Detailed structural analysis revealed protonation sites on EDTA ligands that contribute to overall charge neutrality of both compounds. Infrared spectroscopy confirmed further confirmed ligand protonation in LaEDTA1 and LaEDTA2, while thermogravimetric measurements provided thermal behaviors for the two La(III)–EDTA compounds. Finally, field emission scanning electron microscopy results confirmed elemental compositions of both products, with observable trace levels of iron likely originating from the stainless-steel milling media.

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Details

Title: Subtitle: Mechanochemical Synthesis and Micro-Electron Diffraction Analysis of Rare Earth-Aminopolycarboxylate Coordination Compounds
Creators: Ecem Celik
Pierre LeMagueres
Eric W. Reinheimer
Korey Prescott Carter
Tori Forbes
Resource Type: Journal article
Publication Details: CrystEngComm, Vol.28(1), pp.255-269
DOI: 10.1039/D5CE00935A
ISSN: 1466-8033
eISSN: 1466-8033
Publisher: Royal Society of Chemistry
Language: English
Electronic publication date: 11/24/2025
Date published: 2026
Academic Unit: Civil and Environmental Engineering; Core Research Facilities; Chemistry
Record Identifier: 9985035037302771

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