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

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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[thin space (1/6-em)]:[thin space (1/6-em)]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.
LanguageEnglish
Pages16189-16199
JournalJournal of Materials Chemistry A
Volume5
Issue number31
DOIs
StatusPublished - 5 Jun 2017

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Iron oxides
Eutectics
Microwaves
Nanoparticles
Water
Nanostructures
Microwave heating
Synchrotrons
Photocurrents
Heat treatment
ferric oxide
Degradation
Temperature

Cite this

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title = "Microwave-assisted deep eutectic-solvothermal preparation of iron oxide nanoparticles for photoelectrochemical solar water splitting",
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[thin space (1/6-em)]:[thin space (1/6-em)]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.",
author = "Hammond, {Oliver S.} and Salvador Eslava and Smith, {Andrew J.} and Jifang Zhang and Edler, {Karen J.}",
year = "2017",
month = "6",
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doi = "10.1039/C7TA02078C",
language = "English",
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journal = "Journal of Materials Chemistry A",
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publisher = "Royal Society of Chemistry",
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TY - JOUR

T1 - Microwave-assisted deep eutectic-solvothermal preparation of iron oxide nanoparticles for photoelectrochemical solar water splitting

AU - Hammond,Oliver S.

AU - Eslava,Salvador

AU - Smith,Andrew J.

AU - Zhang,Jifang

AU - Edler,Karen J.

PY - 2017/6/5

Y1 - 2017/6/5

N2 - 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[thin space (1/6-em)]:[thin space (1/6-em)]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.

AB - 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[thin space (1/6-em)]:[thin space (1/6-em)]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.

UR - https://doi.org/10.1039/C7TA02078C

U2 - 10.1039/C7TA02078C

DO - 10.1039/C7TA02078C

M3 - Article

VL - 5

SP - 16189

EP - 16199

JO - Journal of Materials Chemistry A

T2 - Journal of Materials Chemistry A

JF - Journal of Materials Chemistry A

SN - 2050-7488

IS - 31

ER -