Surfactant effects on the synthesis of oxide nanoparticles using deep eutectic solvents

Iva Manasi; Ronak Kakadiya; Ria S. Atri; Michael S. Fairclough; James Doutch; Karen J. Edler

doi:10.1039/d5nj00465a

Surfactant effects on the synthesis of oxide nanoparticles using deep eutectic solvents

Iva Manasi, Ronak Kakadiya, Ria S. Atri, Michael S. Fairclough, James Doutch, Karen J. Edler

Research output: Contribution to journal › Article › peer-review

Abstract

In this work we report the solvothermal synthesis of iron oxide and zinc oxide using a ternary eutectic mixture of choline chloride, urea and glycerol at three molar ratio of the components 1 : 1 : 1, 1 : 1.5 : 0.5 and 1 : 0.5 : 1.5. The synthesised iron oxide is nanocrystalline with a crystallite size of 67.5 ± 8.9 nm, however ZnO formed larger particles. Water and surfactants can be added to these solvents to change the morphology and porosity of the iron oxide nanoparticles. Hexadecyltrimethylammonium (CTAB) surfactant is shown to form micelles in these solvents, and was used to alter the properties of the synthesised iron oxide. Iron oxide formed in the presence of surfactant remains crystalline with a crystallite size of 55.3 ± 13.6 nm, and contains mesopores that are not present in samples synthesised without surfactant. However, addition of surfactant also decreases the nitrogen accessible surface area of the iron oxide nanoparticles. In contrast, addition of water to the DES increases both the crystallite size and the surface area of the nanoparticles.

Original language	English
Pages (from-to)	10035-10046
Journal	New Journal of Chemistry
Volume	49
Issue number	24
Early online date	26 May 2025
DOIs	https://doi.org/10.1039/d5nj00465a
Publication status	Published - 28 Jun 2025

Data Availability Statement

The data supporting this article have been included as part of the ESI.

Acknowledgements

We thank Dr Gabriele Kociok-Köhn and Dr Remi Castaing at the Material and Chemical Characterisation (MC2) Facility at the University of Bath for their help with the acquisition of the PXRD and the N2 sorption data, respectively. We also thank Crispin Hetherington, research engineer at the National Centre for High-Resolution Microscopy (nCHREM) at Lund University (Sweden) for his support in collecting TEM images. We thank the ISIS Neutron and Muon Source for neutron beamtime (Experiment RB1910484; DOI: 10.5286/ISIS.E.RB1910484) and the ISIS Deuteration Lab for providing the isotopically labelled CTAB surfactant. This work benefited from the use of the SasView application, originally developed under NSF award DMR-0520547. SasView contains code developed with funding from the European Unions Horizon 2020 research and innovation programme under the SINE2020 project, Grant No. 654000.

Funding

I. M. acknowledges funding from EPSRC (Grant Number EP/S020772/1). R. S. A. acknowledges funding from the EPSRC Centre for Doctoral Training in Sustainable Chemical Technologies, EPSRC Grant EP/L016354/1.

Funders	Funder number
Engineering and Physical Sciences Research Council	EP/S020772/1 , EP/L016354/1

ASJC Scopus subject areas

Catalysis
General Chemistry
Materials Chemistry

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abstract = "In this work we report the solvothermal synthesis of iron oxide and zinc oxide using a ternary eutectic mixture of choline chloride, urea and glycerol at three molar ratio of the components 1 : 1 : 1, 1 : 1.5 : 0.5 and 1 : 0.5 : 1.5. The synthesised iron oxide is nanocrystalline with a crystallite size of 67.5 ± 8.9 nm, however ZnO formed larger particles. Water and surfactants can be added to these solvents to change the morphology and porosity of the iron oxide nanoparticles. Hexadecyltrimethylammonium (CTAB) surfactant is shown to form micelles in these solvents, and was used to alter the properties of the synthesised iron oxide. Iron oxide formed in the presence of surfactant remains crystalline with a crystallite size of 55.3 ± 13.6 nm, and contains mesopores that are not present in samples synthesised without surfactant. However, addition of surfactant also decreases the nitrogen accessible surface area of the iron oxide nanoparticles. In contrast, addition of water to the DES increases both the crystallite size and the surface area of the nanoparticles.",

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Surfactant effects on the synthesis of oxide nanoparticles using deep eutectic solvents

Abstract

Data Availability Statement

Acknowledgements

Funding

ASJC Scopus subject areas

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