Tailoring the structural and magnetic properties of sol-gel derived Sm-Co nanogranular films

In this study, we investigated the microstructure, phase evolution and magnetic properties of nanogranular films of Sm-Co compounds processed by the sol-gel method. By controlling the compositional ratio of Sm:Co precursor concentration, nanogranular films consisting of three distinct hard magnetic phases namely, Sm₂Co₇, SmCo₅ and Sm₂Co₁₇ with coercivity values of 1.78, 2.94 and 2.12 kOe, respectively, were obtained through this technique.     

Effect of annealing temperature on the structural, photoluminescence and magnetic properties of sol-gel derived Magnetoplumbite-type (M-type) hexagonal strontium ferrite

Magnetoplumbite-type (M-type) hexagonal strontium ferrite particles were synthesized via sol-gel technique employing ethylene glycol as the gel precursor at two different calcination temperatures (800 and 1000 °C). Structural properties were systematically investigated via X-ray diffraction (XRD), field emission scanning electron microscopy, high resolution transmission electron microscopy (HRTEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), photoluminescence spectrophotometry and superconducting quantum interference device magnetometer. XRD results showed that the sample synthesized at 1000 °C was of single-phase with a space group of P6₃/mmc and lattice cell parameter values of a=5.882 Å and c=23.048 Å. EDS confirmed the composition of strontium ferrite calcined at 1000 °C being mainly of M-type SrFe₁₂O₁₉ with HRTEM micrographs confirming the ferrites exhibiting M-type long range ordering along the c-axis of the crystal structure. The photoluminescence (PL) property of strontium ferrite was examined at excitation wavelengths of 260 and 270 nm with significant PL emission peaks centered at 350 nm being detected. Strontium ferrite annealed at higher temperature (1000 °C) was found to have grown into larger particle size, having higher content of oxygen vacancies and exhibited 83-85% more intense PL. Both the as-prepared strontium ferrites exhibited significant oxygen vacancies defect structures, which were verified via TGA. Higher calcination temperature turned strontium ferrite into a softer ferrite.     

Structure and magnetic properties of Co-substituted NiZn ferrite thin films synthesized by the sol-gel process

Co-substituted NiZn ferrite thin films, Ni_0.5Zn_0.5Co_xFe_2−xO₄ (0≤x≤0.2), were synthesized by the sol-gel process. The structure and magnetic properties of Ni_0.5Zn_0.5Co_xFe_2−xO₄ ferrite thin films have been investigated. The diffraction peak shifted towards the lower angle and the lattice parameter increased with Co substitution. There is little influence of Co substitution on the microstructure of NiZn ferrite thin films. The saturation magnetization gradually increases with the increase in Co substitution when x≤0.10, and decreases when x>0.10. Meanwhile, the coercivity initially decreases with the increase in Co substitution when x≤0.10, and increases when x>0.10.     

Structural and magnetic properties of self-assembled Sm-Co spherical aggregates

Self-assembled Sm-Co nanoparticles in the form of spherical aggregates (referred as nanospheres) with diameter ranging from 50 to 180 nm were achieved by means of polyol technique. The size distribution of the Sm-Co nanospheres can be regulated close to ∼100 nm by controlling the molar ratio of Sm:Co precursor. The spherical aggregates exhibited Sm₂Co₇ phase as a major constituent; while the aggregates obtained at higher Co concentration showed co-existence of Co-phase with Sm₂Co₇ phase. Upon annealing, the biphasic nature of nanospheres (Sm₂Co₇/Co) transformed into Sm₂Co₁₇ structure. By varying the Sm:Co precursor ratio from 1:5 to 1:9, the coercivity (H_c) and magnetization (M_s) values of the as-synthesized nanospheres can be tuned from 336 to 140 Oe and from 63.7 to 108 emu/g, respectively, and these values significantly improved after annealing. Maximum values of H_c (1050 Oe) at the Sm:Co molar ratio of 1:5 and M_s of 184.6 emu/g at the Sm:Co molar ratio of 1:9 were achieved in the annealed samples.     

Effect of aluminum substitution on the structural and magnetic properties of cobalt ferrite synthesized by sol-gel auto combustion process

Aluminum substituted cobalt ferrite powders (CoFe_2−xAl_xO₄) with varying composition from 0.0 to 1.0 in the step of 0.2 have been obtained by sol-gel auto combustion technique using citric acid as a fuel. The metal nitrate to fuel ratio was maintained 1:4 throughout the synthesis of CoFe_2−xAl_xO₄. The thermal analysis of as prepared samples is done by TGA technique. The compositional stoichiometry of the prepared samples is confirmed by Energy dispersive X-ray analysis technique. Single phase cubic spinel structure and nano phase structure of the synthesized powders were confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallite size of 16-26 nm was obtained using Scherrer formula. SEM analysis shows the formation of uniform grain growth. The grain size obtained from SEM results is of the order of 30 nm. Maximum specific surface area was observed to be of the order of 52 m²/gm. The highest value of saturation magnetization and coercivity was observed for pure cobalt ferrite sample and it decreases as the aluminum content x increases. A strong co-relation between the saturation magnetization and aluminum content was observed. The decrease in magnetic properties is due to the substitution of aluminum ions in place of Fe³⁺.     

Effect of microstructural characteristics on the magnetic properties of sol-gel synthesized ZnMnO

In this paper we report the effect of microstructural characteristics on the magnetic properties of sol-gel synthesized Mn-doped ZnO. The microstructural characteristics of the samples (e.g., grain sizes and their distribution) have been varied by changing the sintering temperature (T_S) and sintering duration (T_H). Weak room temperature ferromagnetism (RTFM) has been observed in the samples sintered for ∼8 h at 500, 600, 700, 800 and 900 °C. The ferromagnetic fraction and the saturation magnetization, however, first increase as T_S increases from 500 to 600 °C and after that both start decreasing. On the other hand, the samples sintered for ∼12 h at the same temperatures show paramagnetic behavior at room temperature. Field emission scanning electron microscope (FESEM) results show enhancement in the grain sizes with the increase in both T_S and T_H. Energy dispersive X-ray (EDAX) results show increase in the oxygen content in the sample with increase in both T_S and T_H. X-ray diffractometer (XRD) measurements reveal that the basic crystal structure of all the samples corresponds to the wurtzite structure of pure ZnO together with some minor impurities. The correlation between the observed magnetic properties and the microstructural characteristics of the samples has been discussed in this paper.     

Influence of annealing temperature on the formation, microstructure and magnetic properties of spinel nanocrystalline cobalt ferrites

Nanocrystalline cobalt ferrites were synthesized by a simple, general, one-step sol–gel auto-combustion method. An interpretation based on the measurement of the adiabatic flame temperature and the amounts of gas evolved during reaction had been proposed for the nature of combustion. The influence of annealing temperatures on the magnetic properties was investigated. The microstructure was characterized by means of X-ray diffractometer (XRD) and transmission electron microscopy (TEM). It was found that the particle size and magnetic properties of the as-prepared ferrite samples showed strong dependence on the annealing temperature. The coercivity initially increased and then decreased with increasing annealing temperature whereas the particle size and saturation magnetization continuously increased.     

Structure and luminescent properties of LaNbO4 synthesized by sol-gel process

The luminescence properties of LaNbO₄ synthesized by the citric gel process were investigated. The crystallized orthorhombic and monoclinic biphasic structure forms at temperatures below 1100 °C and well-crystallized monoclinic LaNbO₄ is obtained by heat treatment at a temperature of 1200 °C for 3 h. All of LaNbO₄ phosphors derived from the citric gel method exhibit red-shifted excitation spectra as the calcining temperature increased from 700 to 1200 °C. The effect of the heat treatment conditions on the peak shape and the peak positions of the photoluminescence (PL) emission are undetectable, and the PL spectra excited at 260 nm have a blue emission band maximum at 408 nm, corresponding to the self-activated luminescence center of LaNbO₄. The sample heat treated at 1100 °C for 3 h showed the highest absorption and fluorescence intensities among the prepared samples.     

Effect of Cd on the structural, magnetic and electrical properties of nanostructured Mn-Zn ferrite

Nanoparticles of Mn_0.5Zn_0.5−xCd_xFe₂O₄ (x=0.0, 0.1, 0.2 and 0.3) have been synthesized by a chemical co-precipitation method. The lattice constant increases with increasing Cd content. X-ray calculations indicate that there is deviation in the cation distribution in the nanostructured spinel ferrite. The dielectric constant and dielectric loss decrease for the samples with Cd content up to x=0.2. However the dielectric constant rises for x=0.3. This is due to an increase in the hopping process at the octahedral (B sites). The dielectric constant increases with increase in temperature, indicating a thermally activated hopping process. The DC resistivity increases with Cd content up to x=0.2 and decreases for Cd content x=0.3. The maximum magnetization of all the samples decreases with increase in Cd content.     

Effect of cobalt doping and annealing on properties of titania thin films prepared by sol-gel process

Undoped and cobalt doped titania (TiO₂) thin films have been prepared on Si(1 0 0) monocrystal and quartz substrate using the sol-gel deposition method and annealed in air at 450, 550, 650, 750, 850, 950 and 1050 °C. Several experimental techniques (AFM, XRD, Raman spectroscopy, XRR, EDX, XPS, XAS, UV-VIS spectroscopy) have been used to characterize these films. Further more the degree of light induced hydrophilicity was estimated by measuring the contact angle of a water droplet on the film. Increase of the annealing temperature and in smaller degree also cobalt doping predispose titania crystallite growth. The rutile phase was detected at lower temperatures in the cobalt doped films than in the undoped titania films. Cobalt in the cobalt doped TiO₂ was seen to be in Co²⁺ oxidation state, mainly in CoTiO₃ phase when films were annealed at temperatures higher than 650 °C. Cobalt compounds segregated into the sub-surface region and to the surface of the titania, where they formed islands. Cobalt doping red-shifted the fundamental absorption edge further into the visible range, however it did not enhance the light induced hydrophilicity of the thin film surface as compared to the undoped titania thin films.     

Effect of cation distribution on the structural and magnetic properties of nickel substituted nanosized Mn–Zn ferrites prepared by co-precipitation method

Nano particles of Mn_(0.5–x)Ni_xZn_0.5Fe₂O₄ (x=0.0, 0.1, 0.2, 0.3) have been synthesized by chemical co-precipitation method. The lattice constant and distribution of cation in the tetrahedral and octahedral sites have been deduced through X-ray diffraction (XRD) data analysis. The lattice constant (Å) for all Mn/Ni concentration is found to be less than that for the corresponding bulk values. X-ray intensity calculations indicate that there is deviation in the normal cation distribution. Magnetization decreases with increasing Ni concentration except for x=0.3, where it shows increasing trend. This is due to migration of Fe³⁺ ions from B-site to A-site, which reduces the B–B coupling and there by the spin canting in the B sublattice. The Curie temperature was found to decrease with increase in nickel concentration except for x=0.3, where it shows a rise. Coercivity is very low and is found to be inversely proportional to the grain size.     

Photoluminescent properties of boehmite whisker prepared by sol-gel process

A boehmite whisker powder with the aspect ratio and mean diameter of 10-40 and 2-6 nm was prepared by the sol-gel process using aluminum alkoxide as precursor. The main absorption bands located at 234 (5.31 eV), and 254.5 (4.88 eV) nm are presented in the excitation spectrum of sample. It is observed that all the spectra show two main broad bands emission whose maximum shows a large shift, which depends on the excitation wavelength. It is suggested that the ultraviolet photoluminescence emission in boehmite whisker prepared by the sol-gel process may be associated with anionic vacancies (F and F⁺ centers, or grouping of these two types of defects), and the non-bridging oxygen hole center (NBOHC)=Al-O.     

Structural and magnetic properties of nano nickel-zinc ferrite synthesized by reverse micelle technique

Nanocrystalline nickel-zinc ferrites (Ni_0.58Zn_0.42Fe₂O₄) at different pH values (less than 9.6, 9.6, 10.96, and 11.40) for the alkali-precipitating reaction were synthesized by reverse micelle technique. X-ray diffraction reveals a well-defined nickel-zinc ferrite crystal phase at pH=9.6. Increase in pH value obstructs pure-phase formation and results in partial formation of α-Fe₂O₃. The magnetic behaviour of the samples was studied by superconducting quantum interference device. All the samples show superparamagnetic behaviour at room temperature (300 K) and negligible hysteresis at low temperature (5 K). The low value of saturation magnetization is explained on the basis of spin canting. The high-field irreversibility and shifting of the hysteresis loop detected in single-phase sample has been assigned to a spin-disordered phase, which has a spin-freezing temperature of approximately 42 K and other two samples have an antiferromagnetic phase (α-Fe₂O₃) coupled to the ferromagnetic phase.     

Effect of temperature of annealing on optical, structural and electrochromic properties of sol-gel dip coated molybdenum oxide films

The sol-gel dip-coating method is used for the preparation of MoO₃ thin films. The 6 layered MoO₃ films were prepared and annealed at various temperatures in the range of 200-350 °C. The band gap value for MoO₃ films were calculated from optical absorption measurements and it is in the range of 3.55-3.73 eV. XRD spectrum reveals (0 2 0) is the major diffraction plane for the films prepared above 250 °C, which reveals the formation of MoO₃ in α-orthorhombic phase. The films prepared at 200 °C and 250 °C exhibits amorphous nature. The FTIR spectrum confirms the presence of Mo-O-Mo and MoO bonds. Nanorods were observed in the SEM images in the case of MoO₃ films prepared above 250 °C. The films prepared at 250 °C exhibit maximum anodic diffusion coefficient of 9.61 × 10⁻¹¹ cm²/s. The same film exhibits the change in optical transmission of 58.4% at 630 nm with the optical density of 0.80.     

Electrical and optical properties of Al-doped ZnO thin films by sol-gel process

Al-doped ZnO (AZO) thin films oriented along the (0 0 2) plane have been prepared by the sol-gel process and their electrical and optical properties with post-deposition heating temperature were investigated. The preferred c-axis orientation along the (0 0 2) plane was enhanced with increasing post-deposition heating temperature and the surface of the films showed a uniform and nano-sized microstructure. The electrical resistivity of the films decreased from 73 to 22 Ω cm as the post-deposition heating temperature increased from 500 to 650 °C; however, the film postheated at 700 °C increased greatly to 580 Ω cm. The optical transmittance of the films postheated below 650 °C was over 86%, but it decreased at 700 °C. The electrical and optical properties of the AZO films with post-deposition heating temperature are discussed.     

Investigation of magnetic properties of Al substituted nickel ferrite nanopowders, synthesized by the sol-gel method

NiFe_2−xAl_xO₄ nanopowders, where x is from 0 to 1.5 with a step of 0.5, have been synthesized by the sol-gel method and the effect of non-magnetic aluminum content on their structural and magnetic properties were investigated. The X-ray diffraction (XRD) patterns revealed that the synthesized nanopowders are single phase with a spinel structure. Mean crystallite sizes of the samples were calculated by Scherrer's formula and were in the range 20-31 nm. The morphology of the nanopowders was investigated by TEM and the mean particle sizes of the samples were in the range 55-80 nm. Magnetic hysteresis loops were recorded at room temperature in a maximum applied field of 3000 Oe. The results show that by increasing the aluminum content, the magnetizations of the nanopowders are decreased. This reduction is caused by non-magnetic Al³⁺ ions, which by their substitutions the super exchange interactions between different sites will be reduced. It is also seen that the magnetizations of the nanopowders are lower than those related to their bulk counterparts. This reduction was found to be as a consequence of surface spin disorder. M-T curves of the samples were obtained using a Faraday balance and by which the Curie temperatures of the powders were determined. The results that are obtained show that the Curie temperatures of the nanopowders are higher than those of their bulk counterparts.     

Mössbauer analysis on the magnetic properties of Fe–Co nanoparticles synthesized by chemical vapor condensation process

The magnetic properties of Fe–Co nanoparticles synthesized by chemical vapor condensation (CVC) process were investigated. Effect of CVC processing variables on the magnetic properties was analyzed in detail, using Mössbauer spectroscopy, XRD, BET and HRTEM. The synthesized particles were nearly spherical, and their surfaces were identified to be -FeOOH, γ-FeOOH and Fe₃O₄, but not -Fe₂O₃. The magnetic properties were strongly influenced by CVC processing parameters. The increase of cobalt content had changed the magnetic property of the sample. However, when the decomposition temperature and the oxygen content in the carrier gas (Ar) were increased, the magnetic property reduced with decreasing the average particle size. Increasing the vacuum pressure in the chamber resulted in that the magnetic field reinforced with the increase of average particle size.     

Influence of rare earth Ce on structural, electrical and magnetic properties of Sr based W-type hexagonal ferrites

A series of single phase W-type Sr_3−xCe_xFe₁₆O₂₇ (x=0, 0.02, 0.04, 0.06, 0.08, 0.10) hexagonal ferrites prepared by the Sol-Gel method was sintered at 1050 °C for 5 h. The X-ray diffraction analysis reveals that all the samples belong to the family of W-type hexagonal ferrites. The c/a ratio falls in the range of W-type hexagonal ferrites. The grain size was measured by SEM varies from 0.7684 to 0.4366 μm which shows that the Ce³⁺ substituted samples have smaller grain size than pure ferrite Sr₃Fe₁₆O₂₇ which results from the difference in ionic radii of Ce³⁺ (1.034 Å) and Sr²⁺ (1.12 Å). The room temperature resistivity of the present samples varies from 6.5×10⁸ to 272×10⁸ Ω-cm. The coercivity increases from 1370 to 1993 Oe which is consistent with the decrease in grain size. The coercivity values indicate that the present samples fall in the range of hard ferrites. The large value of H_c may be due to domain wall pinning at the grain boundaries.     

Preparation of barium hexaferrite nanopowders by the sol-gel method, using goethite

A series of barium hexaferrite nanoparticles (BaO·nFe₂O₃) with different n values were prepared by the sol-gel method, using goethite and Ba carbonate as raw materials. Phase identification of the samples was investigated by X-ray diffraction (XRD). XRD investigations show that the samples with n=5 and calcined at temperatures higher than 875 °C are single-phase Ba ferrite. An average crystallite size of 22 nm was obtained for the single-phase sample with minimum calcining temperature of 875 °C, using the Scherrer's formula. The morphology of the samples was checked by transmission electron microscope (TEM) and magnetic properties were measured by a sensitive permeameter. The results show that the samples have nonzero coercivities, which shows the particle size are not less than the critical size of Ba ferrite and then are not superparamagnet.     

Effect of annealing conditions on structural and magnetic properties of laser ablated copper ferrite thin films

The effect of annealing conditions on structural and magnetic properties of copper ferrite thin films on (100) Si substrates was examined in detail. After deposition, the ferrite thin films were post-annealed in vacuum and in oxygen atmosphere for several hours. It is found that the crystal structure of CuFe₂O₄ thin films changed drastically depending on different heating process. A maximum magnetization was achieved in the film that was vacuum annealed and it decreased remarkably after oxygen annealing.