Journal
CURRENT APPLIED PHYSICS
Volume 12, Issue 3, Pages 817-825Publisher
ELSEVIER
DOI: 10.1016/j.cap.2011.11.013
Keywords
Nano particle; Iron oxide; XANES; Fe K-shell
Funding
- European Community's Sixth Framework Marie Curie International Reintegration Program [042095]
- Seventh Framework Program [FP7/2007-2013]
- Novel Materials for Energy Applications (NanoPEC) [227179]
- Swiss NSF [200021-116688, IZK0Z2-133944]
- Swiss Federal Office of Energy [153613-102809, 153476-102691]
- Swiss National Science Foundation (SNF) [IZK0Z2_133944] Funding Source: Swiss National Science Foundation (SNF)
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Iron oxide nano particles with nominal Fe2O3 stoichiometry were synthesized by a wet, soft chemical method with heat treatment temperatures from 250 degrees C to 900 degrees C in air. The variation in the structural properties of the nano particles with the heat treatment temperature was studied by X-ray diffraction and Fe K-shell X-ray absorption spectroscopy. X-ray diffractograms show that at lower annealing temperatures the nano particle comprise both maghemite and hematite phases. With increasing temperature, the remainder of the maghemite phase transforms completely to hematite. Profile analysis of the leading Bragg reflections reveals that the average crystallite size increases from 50 nm to 150 nm with increasing temperature. The mean primary particle size decreases from 105 nm to 90 nm with increasing heat treatment temperature. The X-ray diffraction results are paralleled by systematic changes in the pre-edge structure of the Fe K-edge X-ray absorption spectra, in particular by a gradual decrease of the t(2g)/e(g) peak height ratio of the two leading pre-edge resonances, confirming oxidation of the Fe from Fe2+ towards Fe3+. Transmission electron microscopy (TEM) on the samples treated at temperatures as high as 900 degrees C showed particles with prismatic morphology along with the formation of stacking fault like defects. High resolution TEM with selected area electron diffraction (SAED) of samples heat treated above 350 degrees C showed that the nano particles have well developed lattice fringes corresponding to that of (110) plane of hematite. (C) 2011 Elsevier B.V. All rights reserved.
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