Preparation and characterization of nanosized magnesium ferrite powders by a starch-gel process and corresponding ceramics
The synthesis and characterization of nanosized MgFe 2 O 4 by a starch-gel method is described herein. A phase-pure nanosized MgFe 2 O 4 powder ( 1a ) was obtained after calcining a (MgFe)-starch gel at 550 °C. The powder has a specific surface area of 60.6 m 2 /g and a crystallite size of 9 nm. TEM...
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Veröffentlicht in: | Journal of materials science 2013-10, Vol.48 (19), p.6509-6518 |
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Format: | Artikel |
Sprache: | eng |
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Zusammenfassung: | The synthesis and characterization of nanosized MgFe
2
O
4
by a starch-gel method is described herein. A phase-pure nanosized MgFe
2
O
4
powder (
1a
) was obtained after calcining a (MgFe)-starch gel at 550 °C. The powder has a specific surface area of 60.6 m
2
/g and a crystallite size of 9 nm. TEM investigations reveal particles in the range of 7–15 nm. The activation energy of the crystallite growth process was calculated as 89 ± 14 kJ/mol. The shrinkage and sintering behaviour of resulting compacts were studied. UV–Vis investigations of the nanosized powder
1a
reveal an optical band gap of 2.38 eV, whereas calcination at 1100 °C (powder
1g
) leads to a crystallite size of 129 nm and a band gap of 2.16 eV. Magnetization loops at 300 K and the temperature dependence of both the field-cooled and the zero-field-cooled magnetization indicate a superparamagnetic behaviour. The blocking temperature for powder
1a
was determined as 140 K at a field of
H
= 500 Oe. We found different saturation magnetizations (
M
s
) depending on the calcination temperature. Calcination at 550 °C (
1a
) results in
M
s
= 20.0 emu/g which increases with calcination temperature to a maximum of 37.7 emu/g for powder
1e
calcined at 900 °C. Ceramic bodies sintered between 1450 and 1600 °C exhibit
M
s
values of 25–28 emu/g. Magnetic investigations at 10 K on powders
1a
–
1g
show hysteresis loops with coercivities up to 950 Oe, remanences to 10 emu/g and
M
s
values to 50.4 emu/g. Additionally, the nanoscaled powders show a shift of the hysteresis loops. |
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ISSN: | 0022-2461 1573-4803 |
DOI: | 10.1007/s10853-013-7447-x |