Magnetic characterization of Co1-xNixFe2O4 (0 <= x <= 1) nanoparticles prepared by co-precipitation route

Magnetic nanoparticles of Ni-doped cobalt ferrite [Co1-xNixFe2O4(0 <= x <= 1)] synthesized by coprecipitation route have been studied as a function of doping concentration (x) and particle size. The size of the particles as determined by X-ray diffractometer (XRD) and transmission electron microscope (TEM) analyses was found in the range 12-48 nm. The coercivity (H-C) and saturation magnetization (M-S) showed a decreasing behavior with increasing Ni concentration. M-S of all the samples annealed at 600 degrees C lies in the range 65.8-13.7 emu/gm. Field-cooled (FC) studies of the samples showed horizontal shift (exchange bias) and vertical shift in the magnetization loop. Strong decrease in exchange bias (H-b) and vertical shift (delta M) was found for low Ni concentrations while negligible decrease was found at higher concentrations. The presence of exchange bias in the low Ni-concentration region has been explained with reference to the interface spins interaction between a surface region (with structural and spin disorder) and a ferrimagnetic core region. M(T) graphs of the samples showed a decreasing trend of blocking temperature (T-b) with increasing Ni concentration. The decrease of T-b with increasing Ni concentration has been attributed to the lower anisotropy energy of Ni+2 ions as compared to Co+2 that increases the probability of the jump across the anisotropy barrier which in turn decreases the blocking temperature of the system.

Characterization of metal-containing molecular sieves and their catalytic properties in the selective oxidation of cyclohexane

Three types of metal-containing molecular sieves with AFI, AEL and CHA structures (Me = Co, Mn, Cr and V) were synthesized hydrothermally and characterized by XRD, XRF, TG, TPR, NH3-TPD and FT-IR. It was revealed that metals were incorporated into the framework of molecular sieves and induced the presence of charge centers. Both cobalt and manganese in the framework of AIPO-5, AlPO-11 and SAPO-34 were not reducible before the structure collapse. The redox behaviours of these catalysts in cyclohexane oxidation at 403 K using O-2 as oxidant were examined. CoAPO-11 exhibited best activity and good selectivities for the monofunctional oxidation products (88.5%). Cyclohexanol was the major product over most catalysts, whereas for Cr-containing molecular sieves, high selectivity of cyclohexanone was observed. Investigation of reaction mechanism based on CoAPO-11 and CrAPO-5 catalysts indicated that the decomposition of cyclohexyl hydroperoxide (CHHP), the intermediate in cyclohexane oxidation, followed the pathway: cyclohexanone <-- CHHP --> cyclohexanol -->cyclohexanone. (C) 2004 Elsevier B.V. All rights reserved.