NDLI: Synthesis of nanostructured iron oxides dispersed in carbon materials and in situ XRD study of the changes caused by thermal treatment

Content Provider	Springer Nature Link
Author	Gonçalves, Gustavo R. Schetti, Miguel A. Morigaki, Milton K. Nunes, Evaristo Cunha, Alfredo G. Emmerich, Francisco G. Passamani, Edson C. Baggio Saitovitch, Elisa Freitas, Jair C. C.
Copyright Year	2015
Abstract	Carbon-based magnetic nanocomposites are of large interest for applications in catalysis, magnetic separation, water cleaning, and magnetic resonance imaging, among others. This work describes the synthesis of nanocomposites consisting of iron oxides dispersed into a char (obtained from the carbonization at 700 °C of a lignocellulosic precursor) and the study of the thermal transformations occurring in these materials as a consequence of heat treatments. The materials were prepared by impregnation of the char with iron nitrate in the presence of ammonium hydroxide in aqueous suspension. X-ray diffraction experiments performed using synchrotron radiation and Mössbauer spectroscopy showed that the as-prepared material was composed of amorphous Fe$^{3+}$ oxides. Scanning electron microscopy images combined with energy-dispersive X-ray spectrometry indicated a homogeneous dispersion of iron oxides and of silica particles (naturally present in the lignocellulosic precursor) throughout the char. X-ray diffractograms recorded in situ during the heat treatment of the as-prepared material showed the presence of small hematite crystallites (average size ~22 nm) starting from ca. 300 °C. Further heating caused a progressive growth of the hematite crystallites up to ca. 500 °C, when the conversion to magnetite (Fe$_{3}$O$_{4}$) started to take place. At higher temperatures, wüstite (Fe$_{1−x}$O) was detected as an intermediate phase and austenitic iron (γ-Fe) became the dominant phase at temperatures from 900 °C. A steep weight loss was observed in the TG curve accompanying this last reduction stage; upon cooling, γ-Fe was converted into α-Fe (ferrite), which was the dominant phase at room temperature in this heat-treated sample.
Starting Page	1
Ending Page	11
Page Count	11
File Format	PDF
ISSN	13880764
Journal	Journal of Nanoparticle Research
Volume Number	17
Issue Number	7
e-ISSN	1572896X
Language	English
Publisher	Springer Netherlands
Publisher Date	2015-07-11
Publisher Place	Dordrecht
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Magnetic nanoparticles Iron oxides Carbon materials X-ray diffraction In situ analysis Nanotechnology Inorganic Chemistry Characterization and Evaluation of Materials Physical Chemistry Optics, Optoelectronics, Plasmonics and Optical Devices
Content Type	Text
Resource Type	Article
Subject	Chemistry Nanoscience and Nanotechnology Atomic and Molecular Physics, and Optics Condensed Matter Physics Bioengineering Modeling and Simulation

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