Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?

Today, magnetic nanoparticles are present in multiple medical and industrial applications. We take a closer look at the synthesis of magnetic iron oxide nanoparticles through the co-precipitation of iron salts in an alkaline environment. The variation of the synthesis parameters (ion concentration,...

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Main Authors: Sebastian P. Schwaminger, Christopher Syhr, Sonja Berensmeier
Format: Article
Language:English
Published: MDPI AG 2020-03-01
Series:Crystals
Subjects:
Online Access:https://www.mdpi.com/2073-4352/10/3/214
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author Sebastian P. Schwaminger
Christopher Syhr
Sonja Berensmeier
author_facet Sebastian P. Schwaminger
Christopher Syhr
Sonja Berensmeier
author_sort Sebastian P. Schwaminger
collection DOAJ
description Today, magnetic nanoparticles are present in multiple medical and industrial applications. We take a closer look at the synthesis of magnetic iron oxide nanoparticles through the co-precipitation of iron salts in an alkaline environment. The variation of the synthesis parameters (ion concentration, temperature, stirring rate, reaction time and dosing rate) change the structure and diameter of the nanoparticles. Magnetic iron oxide nanoparticles are characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). Magnetic nanoparticles ranging from 5 to 16 nm in diameter were synthesized and their chemical structure was identified. Due to the evaluation of Raman spectra, TEM and XRD, the magnetite and maghemite nanoparticles can be observed and the proportion of phases and the particle size can be related to the synthesis conditions. We want to highlight the use of Raman active modes A<sub>1g</sub> of spinel structured iron oxides to determine the content of magnetite and maghemite in our samples. Magnetite nanoparticles can be derived from highly alkaline conditions even without establishing an inert atmosphere during the synthesis. The correlation between the particle properties and the various parameters of the synthesis was modelled with linear mixture models. The two models can predict the particle size and the oxidation state of the synthesized nanoparticles, respectively. The modeling of synthesis parameters not only helps to improve synthesis conditions for iron oxide nanoparticles but to understand crystallization of nanomaterials.
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spelling doaj.art-0bbc253609344ace915a6f6f5abd0bd52022-12-22T02:55:30ZengMDPI AGCrystals2073-43522020-03-0110321410.3390/cryst10030214cryst10030214Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?Sebastian P. Schwaminger0Christopher Syhr1Sonja Berensmeier2Bioseparation Engineering Group, Department of Mechanical Engineering, Technical University of Munich, 85748 Garching, GermanyBioseparation Engineering Group, Department of Mechanical Engineering, Technical University of Munich, 85748 Garching, GermanyBioseparation Engineering Group, Department of Mechanical Engineering, Technical University of Munich, 85748 Garching, GermanyToday, magnetic nanoparticles are present in multiple medical and industrial applications. We take a closer look at the synthesis of magnetic iron oxide nanoparticles through the co-precipitation of iron salts in an alkaline environment. The variation of the synthesis parameters (ion concentration, temperature, stirring rate, reaction time and dosing rate) change the structure and diameter of the nanoparticles. Magnetic iron oxide nanoparticles are characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). Magnetic nanoparticles ranging from 5 to 16 nm in diameter were synthesized and their chemical structure was identified. Due to the evaluation of Raman spectra, TEM and XRD, the magnetite and maghemite nanoparticles can be observed and the proportion of phases and the particle size can be related to the synthesis conditions. We want to highlight the use of Raman active modes A<sub>1g</sub> of spinel structured iron oxides to determine the content of magnetite and maghemite in our samples. Magnetite nanoparticles can be derived from highly alkaline conditions even without establishing an inert atmosphere during the synthesis. The correlation between the particle properties and the various parameters of the synthesis was modelled with linear mixture models. The two models can predict the particle size and the oxidation state of the synthesized nanoparticles, respectively. The modeling of synthesis parameters not only helps to improve synthesis conditions for iron oxide nanoparticles but to understand crystallization of nanomaterials.https://www.mdpi.com/2073-4352/10/3/214iron oxide nanoparticlesco-precipitationsynthesismagnetic nanoparticlesx-ray diffractionraman spectroscopytransmission electron microscopydesign of experiments
spellingShingle Sebastian P. Schwaminger
Christopher Syhr
Sonja Berensmeier
Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?
Crystals
iron oxide nanoparticles
co-precipitation
synthesis
magnetic nanoparticles
x-ray diffraction
raman spectroscopy
transmission electron microscopy
design of experiments
title Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?
title_full Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?
title_fullStr Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?
title_full_unstemmed Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?
title_short Controlled Synthesis of Magnetic Iron Oxide Nanoparticles: Magnetite or Maghemite?
title_sort controlled synthesis of magnetic iron oxide nanoparticles magnetite or maghemite
topic iron oxide nanoparticles
co-precipitation
synthesis
magnetic nanoparticles
x-ray diffraction
raman spectroscopy
transmission electron microscopy
design of experiments
url https://www.mdpi.com/2073-4352/10/3/214
work_keys_str_mv AT sebastianpschwaminger controlledsynthesisofmagneticironoxidenanoparticlesmagnetiteormaghemite
AT christophersyhr controlledsynthesisofmagneticironoxidenanoparticlesmagnetiteormaghemite
AT sonjaberensmeier controlledsynthesisofmagneticironoxidenanoparticlesmagnetiteormaghemite