Synthesis and characterization of Zn{sub 1-x}Ni{sub x}Fe{sub 2}O{sub 4} spinels prepared by a citrate precursor

Journal Article · Fri Apr 15 04:00:00 EDT 2005 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2005.01.009· OSTI ID:20725876

Mouallem-Bahout, Mona ^[1]; Bertrand, Sarah ^[1]; Pena, Octavio ^[1]

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1. Laboratoire de Chimie du Solide et Inorganique Moleculaire, UMR 6511 CNRS, Universite de Rennes 1, Institut de Chimie de Rennes, 35042 Rennes, Cedex (France)

Nanocrystalline single-phase samples of Zn{sub 1-x}Ni{sub x}Fe{sub 2}O{sub 4} ferrites (0<x<1) have been obtained via a soft-chemistry method based on citrate-ethylene glycol precursors, at a relatively low temperature (650 deg. C). The influence of the nickel and zinc contents as well as that of heat treatments were investigated by means of X-ray powder diffraction, Brunauer-Emmett-Teller (BET) surface area, scanning electron microscopy (SEM) and Fourier Transform Infrared (FTIR) Spectroscopy. Higher Ni content increases the surface areas, the largest one ({approx}20m{sup 2}/g) being obtained for NiFe{sub 2}O{sub 4} annealed at 650 deg. C for 15h. For all compositions, the surface area decreases for prolonged annealing at 650 deg. C and for higher annealing temperatures. Those results were correlated to the particle size evolution; the smallest particles ({approx}50nm) observed in the NiFe{sub 2}O{sub 4} sample (650 deg. C, 15h) steadily increase as Ni ions were replaced by Zn, reaching {approx}100nm in the ZnFe{sub 2}O{sub 4} sample (650 deg. C, 15h). For all the Zn{sub 1-x}Ni{sub x}Fe{sub 2}O{sub 4} samples and, whatever the heat treatments was, the FTIR spectra show two fundamental absorption bands in the range 650-400cm{sup -1}, characteristics of metal vibrations, without any superstructure stating for cation ordering. The highest {nu}{sub 1}-tetrahedral stretching, observed at {approx}615cm{sup -1} in NiFe{sub 2}O{sub 4}, shifts towards lower values with increasing Zn, whereas the {nu}{sub 2}-octahedral vibration, observed at 408cm{sup -1} in NiFe{sub 2}O{sub 4}, moves towards higher wavenumbers, reaching 453cm{sup -1} in ZnFe{sub 2}O{sub 4}. in ZnFe{sub 2}O{sub 4}.

• OSTI ID: 20725876
• Journal Information: Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Journal Issue: 4 Vol. 178; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
ANNEALING
CITRATES
CRYSTALS
FERRITES
FOURIER TRANSFORMATION
INFRARED SPECTRA
NANOSTRUCTURES
NICKEL IONS
PARTICLE SIZE
SCANNING ELECTRON MICROSCOPY
SPECIFIC SURFACE AREA
SPECTROSCOPY
SPINELS
SURFACE AREA
SYNTHESIS
TEMPERATURE RANGE 0400-1000 K
X-RAY DIFFRACTION
ZINC COMPOUNDS