2908
S.P. Pati et al. / Journal of Solid State Chemistry 183 (2010) 2903–2909
reflected in the marked diverging behaviour. The out of phase
component,
//, exhibits a pronounced peak at around 154 K for
w
110 Hz, below which it falls rapidly. With increase of frequency to
710 Hz, this peak shifts towards higher temperature region i.e. to
169 K. This behaviour is attributed to the spin glass like phase,
formed at the AFM–FM interface [26]. This fact is also supported
by temperature dependent dc magnetization measurement that
shows a change of slope around 130 K (Fig. 6).
4. Conclusion
To conclude, Fe–NiO nanocomposites with Fe concentration
varying from 20 to 50 wt% were prepared successfully by a soft
chemical route. XRD and SAED results confirmed the formation of
pure phase nanocomposites. The HRTEM image confirmed the
presence of structurally disordered regions in the FM–AFM
interfaces. Mo¨ssbauer spectroscopy confirmed the presence of
a-Fe nanoparticles in a blocked state giving typical sextet pattern.
Weak dipolar interaction among Fe nanoparticles, Fe nanoparti-
cles at the disordered NiO interfaces and Fe nanoparticles away
from the ordered NiO interface were argued to be possible causes
of appearance of doublets in the Mo¨ssbauer spectra. The observed
hysteresis loop shift along the field axis and enhancement in
coercivity in field-cooled condition confirmed the presence of
exchange bias in the nanocomposites. Irreversibility in the FC
and ZFC curves confirmed strong FM–AFM exchange coupling in
the Fe–NiO nanocomposite system. A change of slope in the ZFC
curve around 130 K has been assigned to transition to a spin
glass like state which is confirmed by ac susceptibility
measurements.
Fig. 6. MꢃT curves of FN50 nanocomposite at an applied field of 100 Oe.
Acknowledgments
The authors are grateful to Dr. S. Das, Jadavpur University,
Kolkata for XRD measurements. Thanks are also due to Dr. K.
Mondal, S N Bose National Centre for Basis Sciences, Kolkata for
VSM measurements. One of the authors (B. Bhushan) thanks CSIR,
Govt. of India for the award of senior research fellowship.
Fig. 7. Temperature dependent out of phase component of ac susceptibility of
FN50. The inset shows the variation of the in-phase component with temperature.
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