Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles

Novel magnetic nanohybrids composed of nanomaghemite covered by organic molecules were successfully synthesized at room temperature with different functionalization agents (sodium polystyrene sulfonate, oxalic acid, and cetyltrimethylammonium bromide) in low and high concentrations. Structural, vibr...

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Main Authors: Diego A. Flores-Cano, Noemi-Raquel Checca-Huaman, Isabel-Liz Castro-Merino, Camila N. Pinotti, Edson C. Passamani, Fred Jochen Litterst, Juan A. Ramos-Guivar
Format: Article
Language:English
Published: MDPI AG 2022-07-01
Series:International Journal of Molecular Sciences
Subjects:
Online Access:https://www.mdpi.com/1422-0067/23/15/8279
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author Diego A. Flores-Cano
Noemi-Raquel Checca-Huaman
Isabel-Liz Castro-Merino
Camila N. Pinotti
Edson C. Passamani
Fred Jochen Litterst
Juan A. Ramos-Guivar
author_facet Diego A. Flores-Cano
Noemi-Raquel Checca-Huaman
Isabel-Liz Castro-Merino
Camila N. Pinotti
Edson C. Passamani
Fred Jochen Litterst
Juan A. Ramos-Guivar
author_sort Diego A. Flores-Cano
collection DOAJ
description Novel magnetic nanohybrids composed of nanomaghemite covered by organic molecules were successfully synthesized at room temperature with different functionalization agents (sodium polystyrene sulfonate, oxalic acid, and cetyltrimethylammonium bromide) in low and high concentrations. Structural, vibrational, morphological, electron energy-loss spectroscopy, magnetic, and Mössbauer characterizations unraveled the presence of mainly cubic inverse spinel maghemite (γ-Fe<sub>2</sub>O<sub>3</sub>), whilst X-ray diffraction and <sup>57</sup>Fe Mössbauer spectroscopy showed that most samples contain a minor amount of goethite phase (α-FeOOH). Raman analysis at different laser power revealed a threshold value of 0.83 mW for all samples, for which the γ-Fe<sub>2</sub>O<sub>3</sub> to α-Fe<sub>2</sub>O<sub>3</sub> phase transition was observed. Imaging microscopy revealed controlled-size morphologies of nanoparticles, with sizes in the range from 8 to 12 nm. Organic functionalization of the magnetic nanoparticles was demonstrated by vibrational and thermogravimetric measurements. For some samples, Raman, magnetic, and Mössbauer measurements suggested an even more complex core-shell-like configuration, with a thin shell containing magnetite (Fe<sub>3</sub>O<sub>4</sub>) covering the γ-Fe<sub>2</sub>O<sub>3</sub> surface, thus causing an increase in the saturation magnetization of approximately 11% against nanomaghemite. Field cooling hysteresis curves at 5 K did not evidence an exchange bias effect, confirming that the goethite phase is not directly interacting magnetically with the functionalized maghemite nanoparticles. These magnetic nanohybrids may be suitable for applications in effluent remediation and biomedicine.
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spelling doaj.art-2776a39130464c49b12e0fc438eb19422023-12-03T12:39:39ZengMDPI AGInternational Journal of Molecular Sciences1661-65961422-00672022-07-012315827910.3390/ijms23158279Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide NanoparticlesDiego A. Flores-Cano0Noemi-Raquel Checca-Huaman1Isabel-Liz Castro-Merino2Camila N. Pinotti3Edson C. Passamani4Fred Jochen Litterst5Juan A. Ramos-Guivar6Grupo de Investigación de Nanotecnología Aplicada para Biorremediación Ambiental, Energía, Biomedicina y Agricultura (NANOTECH), Facultad de Ciencias Físicas, Universidad Nacional Mayor de San Marcos, Av. Venezuela Cdra 34 S/N, Ciudad Universitaria, Lima 15081, PeruCentro Brasileiro de Pesquisas Físicas (CBPF), R. Xavier Sigaud, 150, Urca, Rio de Janeiro 22290-180, BrazilCentro Brasileiro de Pesquisas Físicas (CBPF), R. Xavier Sigaud, 150, Urca, Rio de Janeiro 22290-180, BrazilPhysics Department, Federal University of Espírito Santo, Vitória 29075-910, BrazilPhysics Department, Federal University of Espírito Santo, Vitória 29075-910, BrazilInstitut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38106 Braunschweig, GermanyGrupo de Investigación de Nanotecnología Aplicada para Biorremediación Ambiental, Energía, Biomedicina y Agricultura (NANOTECH), Facultad de Ciencias Físicas, Universidad Nacional Mayor de San Marcos, Av. Venezuela Cdra 34 S/N, Ciudad Universitaria, Lima 15081, PeruNovel magnetic nanohybrids composed of nanomaghemite covered by organic molecules were successfully synthesized at room temperature with different functionalization agents (sodium polystyrene sulfonate, oxalic acid, and cetyltrimethylammonium bromide) in low and high concentrations. Structural, vibrational, morphological, electron energy-loss spectroscopy, magnetic, and Mössbauer characterizations unraveled the presence of mainly cubic inverse spinel maghemite (γ-Fe<sub>2</sub>O<sub>3</sub>), whilst X-ray diffraction and <sup>57</sup>Fe Mössbauer spectroscopy showed that most samples contain a minor amount of goethite phase (α-FeOOH). Raman analysis at different laser power revealed a threshold value of 0.83 mW for all samples, for which the γ-Fe<sub>2</sub>O<sub>3</sub> to α-Fe<sub>2</sub>O<sub>3</sub> phase transition was observed. Imaging microscopy revealed controlled-size morphologies of nanoparticles, with sizes in the range from 8 to 12 nm. Organic functionalization of the magnetic nanoparticles was demonstrated by vibrational and thermogravimetric measurements. For some samples, Raman, magnetic, and Mössbauer measurements suggested an even more complex core-shell-like configuration, with a thin shell containing magnetite (Fe<sub>3</sub>O<sub>4</sub>) covering the γ-Fe<sub>2</sub>O<sub>3</sub> surface, thus causing an increase in the saturation magnetization of approximately 11% against nanomaghemite. Field cooling hysteresis curves at 5 K did not evidence an exchange bias effect, confirming that the goethite phase is not directly interacting magnetically with the functionalized maghemite nanoparticles. These magnetic nanohybrids may be suitable for applications in effluent remediation and biomedicine.https://www.mdpi.com/1422-0067/23/15/8279iron oxidenanoparticlesroom-temperature synthesisfunctionalization
spellingShingle Diego A. Flores-Cano
Noemi-Raquel Checca-Huaman
Isabel-Liz Castro-Merino
Camila N. Pinotti
Edson C. Passamani
Fred Jochen Litterst
Juan A. Ramos-Guivar
Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles
International Journal of Molecular Sciences
iron oxide
nanoparticles
room-temperature synthesis
functionalization
title Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles
title_full Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles
title_fullStr Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles
title_full_unstemmed Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles
title_short Progress toward Room-Temperature Synthesis and Functionalization of Iron-Oxide Nanoparticles
title_sort progress toward room temperature synthesis and functionalization of iron oxide nanoparticles
topic iron oxide
nanoparticles
room-temperature synthesis
functionalization
url https://www.mdpi.com/1422-0067/23/15/8279
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