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Microwave-assisted deep eutectic-solvothermal preparation of iron oxide nanoparticles for photoelectrochemical solar water splitting

Hammond, Oliver S. ; Eslava, Salvador ; Smith, Andrew J. ; Zhang, Jifang and Edler, Karen J. LU orcid (2017) In Journal of Materials Chemistry A 5(31). p.16189-16199
Abstract

Here, we present a new microwave-solvothermal method for the preparation of iron oxide nanostructures using deep eutectic solvents as a more sustainable reaction medium. By varying the synthesis temperature and solvent water fraction, the methodology offers control over iron oxide phase, size, and morphology, using efficient, rapid (10 minute) microwave heating. Synthesis with pure DES gives small (<5 nm) superparamagnetic samples of γ-Fe2O3 or α-Fe2O3, whereas hydrated DES yielded either nanoshards or large rhombohedral nanoparticles without the superparamagnetic response. Nanostructures were solution-cast onto F:SnO2 films. The photoelectrochemical response of the prepared... (More)

Here, we present a new microwave-solvothermal method for the preparation of iron oxide nanostructures using deep eutectic solvents as a more sustainable reaction medium. By varying the synthesis temperature and solvent water fraction, the methodology offers control over iron oxide phase, size, and morphology, using efficient, rapid (10 minute) microwave heating. Synthesis with pure DES gives small (<5 nm) superparamagnetic samples of γ-Fe2O3 or α-Fe2O3, whereas hydrated DES yielded either nanoshards or large rhombohedral nanoparticles without the superparamagnetic response. Nanostructures were solution-cast onto F:SnO2 films. The photoelectrochemical response of the prepared photoanodes was assessed, with a maximum measured photocurrent response of 0.7 mA cm-2 at 1.23 V vs. RHE. We measured the solvent structure using synchrotron WAXS, demonstrating the differences between the dry and hydrated solvent before and after heat-treatment, and showing that the hydrated solvent is remarkably resilient to extensive degradation.

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author
; ; ; and
publishing date
type
Contribution to journal
publication status
published
in
Journal of Materials Chemistry A
volume
5
issue
31
pages
11 pages
publisher
Royal Society of Chemistry
external identifiers
  • scopus:85027134941
ISSN
2050-7488
DOI
10.1039/c7ta02078c
language
English
LU publication?
no
additional info
Publisher Copyright: © 2017 The Royal Society of Chemistry.
id
21d61625-edc0-4c66-8f48-b6167ef32359
date added to LUP
2023-01-18 09:14:26
date last changed
2023-02-03 13:41:42
@article{21d61625-edc0-4c66-8f48-b6167ef32359,
  abstract     = {{<p>Here, we present a new microwave-solvothermal method for the preparation of iron oxide nanostructures using deep eutectic solvents as a more sustainable reaction medium. By varying the synthesis temperature and solvent water fraction, the methodology offers control over iron oxide phase, size, and morphology, using efficient, rapid (10 minute) microwave heating. Synthesis with pure DES gives small (&lt;5 nm) superparamagnetic samples of γ-Fe<sub>2</sub>O<sub>3</sub> or α-Fe<sub>2</sub>O<sub>3</sub>, whereas hydrated DES yielded either nanoshards or large rhombohedral nanoparticles without the superparamagnetic response. Nanostructures were solution-cast onto F:SnO<sub>2</sub> films. The photoelectrochemical response of the prepared photoanodes was assessed, with a maximum measured photocurrent response of 0.7 mA cm<sup>-2</sup> at 1.23 V vs. RHE. We measured the solvent structure using synchrotron WAXS, demonstrating the differences between the dry and hydrated solvent before and after heat-treatment, and showing that the hydrated solvent is remarkably resilient to extensive degradation.</p>}},
  author       = {{Hammond, Oliver S. and Eslava, Salvador and Smith, Andrew J. and Zhang, Jifang and Edler, Karen J.}},
  issn         = {{2050-7488}},
  language     = {{eng}},
  number       = {{31}},
  pages        = {{16189--16199}},
  publisher    = {{Royal Society of Chemistry}},
  series       = {{Journal of Materials Chemistry A}},
  title        = {{Microwave-assisted deep eutectic-solvothermal preparation of iron oxide nanoparticles for photoelectrochemical solar water splitting}},
  url          = {{http://dx.doi.org/10.1039/c7ta02078c}},
  doi          = {{10.1039/c7ta02078c}},
  volume       = {{5}},
  year         = {{2017}},
}