The formation of nanocrystalline SrFeO(3-delta) using mechano-synthesis and subsequent sintering: structural and Mössbauer studies.
The influence of mechanical milling and subsequent sintering of a 2:1 molar mixture of SrCO3 and alpha-Fe2O3 on the formation of SrFeO(3-delta) pervoskite-related nanocrystalline particles is investigated. The structural evolution during the formation process is systematically investigated using X-ray diffraction, thermal analysis, X-ray photoelectron spectroscopy and Mössbauer spectroscopy. Pre-milling the mixture in air for 120 h leads to the incorporation of Sr2+ in the alpha-Fe2O3 crystal structure thus facilitating the formation of a 2:1 nanocrystalline mixture of SrFeO3 and SrFeO2.875 by sintering the pre-milled mixture in air at 800 degrees C (12 h). This temperature is approximately 300 degrees C lower than those at which SrFeO(3-delta) phases are synthesized by the conventional ceramic techniques. Pre-milling the precursors was found to result in a smaller oxygen deficiency (delta) relative to conventional ceramic synthesis of SrFeO(3-delta). Rietveld refinement of the X-ray diffraction shows the interatomic distances in the resulting SrFeO2.875 nanocrystalline phase to be slightly different from those of the conventionally prepared bulk leading, in turn, to a crystal structure with tilted polyhedral cationic sites. This structural distortion is related to both small-size and surface effects in the nanoparticles that have no counterparts in the corresponding bulk material. The surface structure of the attained SrFeO(3-delta) nanocrystalline particles shows a significant partial reduction of Fe4+ to Fe3+ due to ambient conditions and the presence of an appreciable amount of SrCO3 as well.
Widatallah
H M
HM
Department of Physics, Sultan Qaboos University, P.O. Box 36, 123, Muscat, Oman.
Al-Rawas
A D
AD
Johnson
C
C
Al-Harthi
S H
SH
Gismelseed
A M
AM
Moore
E A
EA
Stewart
S J
SJ