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

DOI: 10.1039/C7TA02078C DOI Help

Authors: Oliver S. Hammond (University of Bath) , Salvador Eslava (University of Bath) , Andrew J. Smith (Diamond Light Source) , Jifang Zhang (University of Bath) , Karen J. Edler (University of Bath)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: J. Mater. Chem. A , VOL 10

State: Published (Approved)
Published: June 2017
Diamond Proposal Number(s): 15194

Open Access Open Access

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.

Subject Areas: Chemistry

Instruments: I22-Small angle scattering & Diffraction


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