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Synthetic mechanism studies of iron selenides: an emerging class of materials for electrocatalysis

Hou, Bo ORCID: https://orcid.org/0000-0001-9918-8223, Benito-Alifonso, David, Webster, Richard F., Cherns, David, Galan, M. Carmen and Fermín, David J. 2021. Synthetic mechanism studies of iron selenides: an emerging class of materials for electrocatalysis. Catalysts 11 (6) , 681. 10.3390/catal11060681

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Abstract

Solution-processed iron selenide nanocrystals (NCs) have recently attracted considerable attention in electrocatalysis water splitting. Nevertheless, a primary challenge in current iron-based NCs chemical synthesis is controlling phase purities between each chalcogen (monochalcogenide, dichalcogenides, and oxides), which requires a comprehensive understanding of the reaction mechanisms at the early stages of nucleation. Herein, we investigate the fundamental steps in transforming molecular organoiron and organoselenium precursors to iron selenides NCs with the view of developing universal synthesis protocols for phase pure metal selenium and metal oxides NCs. The main intermediate species and volatile by-products are identified by high-resolution electron microscopy and Nuclear Magnetic Resonance (NMR) spectroscopy (1H, 13C, and 31P). Experimental evidence suggests that the phase determining factor is the coordinating reactivity difference between olefins (1-octadecene, oleylamine), tributylphosphine and trioctylphosphine associated with their corresponding Se bond cleavage. This work proposes organoselenium interconversion reaction mechanisms during iron selenides synthesis, offering a universal synthetic strategy for other electrocatalytically or photocatalytically active layered metal selenides materials.

Item Type: Article
Date Type: Publication
Status: Published
Schools: Physics and Astronomy
Additional Information: This is an open access article distributed under the Creative Commons Attribution License
Publisher: MDPI
ISSN: 2073-4344
Date of First Compliant Deposit: 1 June 2021
Date of Acceptance: 26 May 2021
Last Modified: 05 Nov 2022 08:04
URI: https://orca.cardiff.ac.uk/id/eprint/141685

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