Single crystalline nickel ferrite (NiFe2O4) which has an inverse spinel structure is reported to exhibit a mixed spinel structure when its grain size is reduced to nanometer range. It is known that structural transformations in the nanosize regime are not akin to those of bulk crystals. Additionally, magnetic properties like superparamagnetism and contribution to it by surface layers are critically influenced by the synthesis route of the samples. In this article, we present an investigation on the structural transformation of nanostructured NiFe2O4 using x-ray diffraction (XRD), Mössbauer and magnetization measurements, and Fourier transform infrared (FTIR) and micro-Raman spectroscopy. Nanostructured NiFe2O4 samples were synthesized by a coprecipitation technique followed by thermal processing. Four samples having average grain sizes 13, 20, 26, and 51 nm were synthesized. XRD results confirmed the samples to be nanostructured NiFe2O4 and gave evidence for the mixed spinel structure of the samples of lower grain sizes. Mössbauer study of the smallest and largest grain-sized samples revealed surface spin canting and change in coordination of the iron ions at tetrahedral and octahedral sites with reduction in grain size. The spin canting angle and the coordination factor were determined from the Mössbauer spectra. Vibrating sample magnetometer measurements gave a lower value of magnetization for the samples of lowest grain size and this observation could be explained on the basis of a structural transformation of the sample from inverse to mixed spinel. FTIR and micro-Raman spectroscopic studies also yielded convincing evidence for a transformation of the structure. The results of the present study lead to the inference that the properties of nanosized NiFe2O4 particle emerged from a transformation of their structure from inverse spinel structure to mixed spinel.

The reduction in the grain size to nanometer range can bring about radical changes in almost all of the properties of semiconductors. CdS nanoparticles have attracted considerable scientific interest because they exhibit strongly size-dependent optical and electrical properties. In the case of nanostructured materials, confinement of optical phonons can produce noticeable changes in their vibrational spectra compared to those of bulk crystals. In this paper we report the study of optical phonon modes of nanoparticles of CdS using Raman spectroscopy. Nanoparticle sample for the present study was synthesized through chemical precipitation technique. The CdS nanoparticles were then subjected to heat treatment at low temperature (150°C) for extended time intervals. The crystal structure and grain size of the samples were determined using X-ray diffraction and HRTEM. The Raman spectra of the as-prepared and heat treated samples were recorded using conventional Raman and micro-Raman techniques. The spectrum of as prepared sample exhibited an intense, broad peak at 301 cm -1 corresponding to the LO phonon mode. Higher order phonon modes were also observed in the spectra. A noticeable asymmetry in the Raman line shape indicated the effect of phonon confinement. Other features in the spectra are discussed in detail.

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