High heat generation ability in AC magnetic field for nano-sized magnetic Y3Fe5O12 powder prepared by bead milling

Nano-sized magnetic Y₃Fe₅O₁₂ ferrite having a high heat generation ability in an AC magnetic field was prepared by bead milling. A commercial powder sample (non-milled sample) of ca. 2.9 μm in particle size did not show any temperature enhancement in the AC magnetic field. The heat generation ability in the AC magnetic field improved with a decrease in the average crystallite size for the bead-milled Y₃Fe₅O₁₂ ferrites. The highest heat ability in the AC magnetic field was for the fine Y₃Fe₅O₁₂ powder with a 15-nm crystallite size (the samples were milled for 4 h using 0.1 mm? beads). The heat generation ability of the excessively milled Y₃Fe₅O₁₂ samples decreased. The main reason for the high heat generation property of the milled samples was ascribed to an increase in the Néel relaxation of the superparamagnetic material. The heat generation ability was not influenced by the concentration of the ferrite powder. For the samples milled for 4 h using 0.1 mm? beads, the heat generation ability (W g⁻¹) was estimated using a 3.58×10⁻⁴ fH² frequency (f/kHz) and the magnetic field (H/kA m⁻¹), which is the highest reported value of superparamagnetic materials.     

Thickness and microstructure dependent transport and MR in La0.7Pb0.3MnO3 manganite films

Thickness dependent modifications in the structure and microstructure and their effect on the transport and magnetotransport in chemical solution deposition (CSD) grown La_0.7Pb_0.3MnO₃ (LPMO) manganite thin films grown on single crystalline LaAlO₃ (LAO) (1 0 0) substrates have been studied. X-ray diffraction (XRD) measurements show the reduction in the microstrain at the film-substrate interface with increasing thickness. Increase in grain size and island like grain growth with the reduction in surface roughness as a function of film thickness has been observed from the microstructural studies using atomic force microscopy (AFM) and lateral force microscopy (LFM) measurements. Improvement in the surface to volume ratio (D⁻¹) resulting in the modifications in transport and magnetotransport properties of the LPMO films has been discussed in detail in the light of thickness dependent microstructural effects on the resistivity and magnetoresistance (MR) behavior. The variations in intrinsic and extrinsic MR with D⁻¹ show an interesting interplay between them, which can be explained on the basis of thickness dependent grain size, grain boundary density and grain boundary nature.     

Temperature dependence of magnetic properties of NiFe2O4 nanoparticles embeded in SiO2 matrix

Spinel ferrite NiFe₂O₄ nanoparticles (?25 nm) in SiO₂ matrix were prepared by sol–gel method. The phase and average crystallite size of the samples were determined by X-ray diffraction method and the particle size distributions were studied by a transmission electron microscope. Magnetic properties of the samples were investigated with different ferrite particle sizes and at various temperatures down to 10 K. Superparamagnetic properties were observed at room temperature when the particle size is less than 10 nm.In superparamagnetic state, the field dependence of magnetization follows Langevin function which was originally developed for paramagnetism. The effective anisotropy constant K_eff is found to increase significantly with the decrease in particle volume and an order of magnitude higher than that of the bulk samples when the particle size is below 5 nm due to the dominance of surface anisotropy. In case of nanosized systems, the effect of size reduction on the law of approach to saturation has also been studied in detail.     

Magnetic and structural studies of mechanically alloyed nanostructured Fe49Co49V2 powders

Nanostructured Fe₄₉Co₄₉V₂ powders were produced by high energy milling at different milling times and then examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The saturation magnetization and coercivity of samples were measured at room temperature by a vibration sample magnetometer (VSM). Structural studies show that as the milling time increases from 0 to 125 h, the average grain size reduces from 130 to about 8-10 nm, while the microstrain increases up to 1.7%. The lattice parameter decreases from 0 to 36 h and then increases up to 125 h. According to the XRD patterns, the formation of intermetallic compound of (Fe, Co)V after about 16 h affects the magnetic properties. The coercivity totally increases up to 61 Oe due to the introduction of microstrain during the milling process. Magnetic measurements reveal that the saturation magnetization has some fluctuations during the milling treatment and finally at 125 h reaches about 180 emu/g     

Heat generation ability in AC magnetic field of nano MgFe2O4-based ferrite powder prepared by bead milling

Nanosized MgFe₂O₄-based ferrite powder having heat generation ability in an AC magnetic field was prepared by bead milling and studied for thermal coagulation therapy applications. The crystal size and the particle size significantly decreased by bead milling. The heat generation ability in an AC magnetic field improved with the milling time, i.e. a decrease in crystal size. However, the heat generation ability decreased for excessively milled samples with crystal sizes of less than 5.5 nm. The highest heat ability (ΔT=34 °C) in the AC magnetic field (370 kHz, 1.77 kA/m) was obtained for fine MgFe₂O₄ powder having a ca. 6 nm crystal size (the samples were milled for 6-8 h using 0.1 mm ? beads). The heat generation of the samples was closely related to hysteresis loss, a B-H magnetic property. The reason for the high heat generation properties of the samples milled for 6-8 h using 0.1 mm ? beads was ascribed to the increase in hysteresis loss by the formation of a single domain. Moreover, the improvement in heating ability was obtained by calcination of the bead-milled sample at low temperature. In this case, the maximum heat generation (ΔT=41 °C) ability was obtained for a ca. 11 nm crystal size sample was prepared by crystal growth during the sample calcination. On the other hand, the ΔT value for Mg_0.5Ca_0.5Fe₂O₄ was synthesized using a reverse precipitation method decreased by bead milling.     

Structure and magnetic properties of nanocrystalline Fe75Si25 powders prepared by mechanical alloying

Nanocrystalline Fe₇₅Si₂₅ powders were prepared by mechanical alloying in a planetary ball mill. The evolution of the microstructure and magnetic properties during the milling process were studied by X-ray diffraction, scanning electron microscope and vibrating sample magnetometer measurements. The evolution of non-equilibrium solid solution Fe (Si) during milling was accompanied by refinement of crystallite size down to 10 nm and the introduction of high density of dislocations of the order of 10¹⁷ m⁻². During the milling process, Fe sites get substituted by Si. This structural change and the resulting disorder are reflected in the lattice parameters and average magnetic moment of the powders milled for various time periods. A progressive increase of coercivity was also observed with increasing milling time. The increase of coercivity could be attributed to the introduction of dislocations and reduction of powder particle size as a function of milling time.     

Structural and electrical properties of high-energy ball-milled NASICON type Li1.3Ti1.7Al0.3(PO4)2.9(VO4)0.1 ceramics

Nano-crystallites of Li_1.3Ti_1.7Al_0.3(PO₄)_2.9(VO₄)_0.1 NASICON type material are prepared by means of solid-state reaction of a stoichiometric mixture after milling it for 22 and 55 h. The milling reduces the average crystallite size of the ceramic to 80 and 60 nm, respectively. Mechanical milling changes structural parameters and the strain induced at the grain-boundaries plays a major role in improving electrical conductivity. An order of magnitude increase in electrical conductivity is observed in the material milled for 55 h compared to the unmilled material, which is also reflected in permittivity loss. Modulus and permittivity representations substantiate the constriction effect of grain-boundaries observed in the complex impedance representation.     

Superparamagnetic behavior of La0.67Sr0.33MnO3 nanoparticles prepared via sol-gel method

Magnetic nanoparticles of La_0.67Sr_0.33MnO₃ (LSMO) manganite were prepared by sol-gel method. Phase formation and crystal structure of the synthesized powder were examined by the X-ray diffraction (XRD) using the Rietveld analysis. The mean particle size was determined by the transmission electron microscopy (TEM). Infrared transmission spectroscopy revealed that stretching and bending modes are influenced by calcinations temperature. The temperature dependence of the ac magnetic susceptibility was measured at different frequencies and ac magnetic fields in the selected ranges of 40-1000 Hz and 80-800 A/m, respectively. The temperature dependence of ac susceptibility shows a characteristic maxima corresponding to the blocking temperature near room temperature. The frequency dependence of the blocking temperature is well described by the Vogel-Fulcher law. By fitting the experimental data with this law, the relaxation time τ₀=1.7×10⁻¹² s, characteristic temperature T₀=262±3 K, anisotropy energy E_a/k=684±15 K and effective magnetic anisotropy constant k_eff=2.25×10⁴ erg/cm³ have been obtained. dc Magnetization measurement versus magnetic field shows that some of LSMO nanoparticles are blocked at 293 K. The role of magnetic interparticle interactions on the magnetic behavior is also investigated.     

Superspin glass state in MnFe2O4 nanoparticles

Nanosized MnFe₂O₄ ferrites were synthesized by a simple method, which is based on the solid state ball-milling and calcinations of nitrate precursors and citric acid. The samples were characterized by using different methods. The results indicate that the products mainly consist of MnFe₂O₄ nanoparticles. The effect of different annealing temperatures on particle sizes and crystallinity of the samples was also studied. By increasing the particle size, the coercivity and magnetization of the samples increase. The increase of magnetization by increasing the crystallite size could be attributed to the lower surface spin canting and surface spin disorder of the larger magnetic nanoparticles. Our analysis of ac susceptibility measurements shows that the interparticle magnetic interaction leads to the superspin glass-like behavior in these nanoparticle samples.     

Structural characterization of thermally evaporated Bi2Te3 thin films

Thermally evaporated Bi₂Te₃ thin films were deposited on glass substrates. X-ray diffraction study confirmed that the growned films are polycrystalline in nature having hexagonal structure. The film exhibits preferential orientation along the [0 1 5] direction for the films of all thickness together with other abundant planes [0 1 1 1] and [1 1 0]. Various structural parameters such as lattice constants, crystallite size, strain, and dislocation density have been calculated and they are found to be thickness dependent. The lattice parameters are found to be a=4.38 Å and c=30.40 Å. The grain size of the films increases with thickness as the dislocation density and the microstrain decreases with thickness. The mean bond energy and the average coordination number of Bi₂Te₃ thin film are found to be 1.72 eV and 2.4, respectively.     

Structural,magnetic and electrical properties of Co1−xZnxFe2O4 synthesized by co-precipitation method

Nanoparticles of Co_1−xZn_xFe₂O₄ with stoichiometric proportion (x) varying from 0.0 to 0.6 were prepared by the chemical co-precipitation method. The samples were sintered at 600 °C for 2 h and were characterized by X-ray diffraction (XRD), low field AC magnetic susceptibility, DC electrical resistivity and dielectric constant measurements. From the analysis of XRD patterns, the nanocrystalline ferrite had been obtained at pH=12.5–13 and reaction time of 45 min. The particle size was calculated from the most intense peak (3 1 1) using the Scherrer formula. The size of precipitated particles lies within the range 12–16 nm, obtained at reaction temperature of 70 °C. The Curie temperature was obtained from AC magnetic susceptibility measurements in the range 77–850 K. It is observed that Curie temperature decreases with the increase of Zn concentration. DC electrical resistivity measurements were carried out by two-probe method from 370 to 580 K. Temperature-dependent DC electrical resistivity decreases with increase in temperature ensuring the semiconductor nature of the samples. DC electrical resistivity results are discussed in terms of polaron hopping model. Activation energy calculated from the DC electrical resistivity versus temperature for all the samples ranges from 0.658 to 0.849 eV. The drift mobility increases by increasing temperature due to decrease in DC electrical resisitivity. The dielectric constants are studied as a function of frequency in the range 100 Hz–1 MHz at room temperature. The dielectric constant decreases with increasing frequency for all the samples and follow the Maxwell–Wagner's interfacial polarization.     

Size-induced effect on nano-crystalline CoFe2O4

Cobalt ferrite (CoFe₂O₄) nano-particles have been synthesized successfully and we studied the effect of temperature on them. The particles have been annealed at different temperatures ranging from 373 to 1173 K. Significant effect on the physical parameters like crystalline phase, crystallite size, particle size, lattice strain and magnetic properties of the nano-particles has been investigated. The studies have been carried out using a powder X-ray diffractometer (XRD), a transmission electron microscope (TEM) and a vibrating sample magnetometer (VSM). A thorough study of the variation of specific surface area and particle size with annealing is presented here, with their effects on saturation magnetization.     

Magnetic behavior of nanocrystalline LaMn2Ge2

The compound, LaMn₂Ge₂, crystallizing in ThCr₂Si₂-type tetragonal crystal structure, has been known to undergo ferromagnetic order below (T_C=) 326 K. In this article, we report the magnetic behavior of nanocrystalline form of this compound, obtained by high-energy ball milling. T_C of this compound is reduced marginally for the nanoform, whereas there is a significant reduction of the magnitude of the saturation magnetic moment with increasing milling time. The coercive field however increases with decreasing particle size. Thus, this work provides a route to tune these parameters by reducing the particle size in this ternary family.     

Enhanced ferromagnetism in nano-sized Zn0.95Mn0.05O grains

The present work reports ferromagnetism by doping magnetic Mn atoms in the diamagnetic ZnO matrix and the ferromagnetism has been extended up to 640 K in nano-grained Zn_0.95Mn_0.05O samples. The bulk and nano-grained samples were stabilized in hexagonal crystal structure with space group p63mc. The grain size and lattice strain of the samples were estimated from room temperature XRD spectrum. Surface morphology of the samples was examined at room temperature using SEM picture and EDX spectrum. The ferromagnetism of the bulk material shows enhancement in nano-grained samples, which was mainly due to the solution of Mn atoms into the lattice sites of ZnO by mechanical milling. The enhancement of magnetic moment and ferromagnetic ordering temperature with reduction in grain size has been understood in terms of the core-shell structure and existing theoretical models. The present work also demonstrated the role of surface spin disorder on the enhancement of ferromagnetism in Zn_0.95Mn_0.05O nanograins.     

Microstructural characterisation of nanoparticles using, XRD line profiles analysis, FE-SEM and FT-IR

In this investigation, the structural characteristics of α- Fe₂O₃ nanoparticles synthesised by a mechanical milling have been explored. The structure and morphology of samples were characterized by X-ray powder diffraction, field-emission scanning electron microscope (FE-SEM) and FT-IR measurements. The crystallite size and internal strain were evaluated by XRD patterns using Williamson-Hall and Scherrer methods. The results did not reveal any phase change during the milling. The average particle size decreases with a prolongation of milling times, while the lattice parameters and internal strain increase. It was found that using this method allowed the formation of hematite nanoparticles.     

Dielectric and AC conductivity behavior of BaBi2Nb2O9 ceramics

The complex dielectric and AC conductivity response of BaBi₂Nb₂O₉ relaxor ferroelectric ceramics were studied as a function of frequency (100 Hz-10 MHz) at various temperatures. The observed dielectric behavior was characterized by two types of relaxation processes which were described by the ‘universal relaxation law’. The frequency dependence of conductivity which showed a classical relaxor behavior followed the Jonscher's universal law σ(ω)=σ₀+Aωⁿ. The exponent n exhibited a minimum in the vicinity of temperatures of dielectric anomaly while the pre-factor A showed a maximum. The temperature dependence of n followed the Vogel-Fulcher relation with activation energy of about 0.14 eV.     

Multiferroic magnetoelectric coupling and relaxor ferroelectric behavior in 0.7BiFeO3-0.3BaTiO3 nanocrystals

The structural, microstructural, polarization, magnetization, dielectric constant, and relaxor characteristics of 0.7BiFeO₃-0.3BaTiO₃ (BF-BT) nanocrystals have been studied. BF-BT nanocrystals were prepared by a chemical route using polyvinyl alcohol as surfactant. The phase structure is confirmed by X-ray diffraction and average particle size by transmission and scanning electron microscopy. The magnetoelectric coupling is studied by polarization hysteresis loops under the influence of applied magnetic field and the phase transition anomaly. The diffuse phase transition is studied by modified Curie-Weiss law and relaxor characteristics by Vogel-Fulcher relation.     

Structure,magnetic and magnetoresistance properties of Pr0.67Sr0.33MnO3 manganite oxide prepared by ball milling method

A sample of Pr_0.67Sr_0.33MnO₃ nanoparticles was synthesized by the ball milling method. X-ray diffraction pattern of the sample showed orthorhombic system with Pnma space group. The average crystallite size of 110 nm was obtained by both Scanning Electron Microscopy and X-ray diffraction. Magnetic measurements showed para-to-ferromagnetic transition with a Curie temperature of T_C=269 K. Electrical investigations showed that all our samples exhibit a semi-conducting behavior above T_C and a metallic-like one at lower temperatures. The sample exhibited a large magnetoresistance of 30% at room temperature in an applied magnetic field of 2 T. The transport and the magnetic properties were interpreted in terms of the existence of magnetic polarons in the sample.     

Preparation and photoluminescence characteristics of Eu-doped MgAl1.8Y0.2O4 nanocrystals

A simple combustion route was employed for the preparation of Eu³⁺-doped MgAl_1.8Y_0.2−xO₄ nanocrystals using metal nitrates as precursors and urea as a fuel in a preheated furnace at 500 °C. The powders thus obtained were then fired at 1000 °C for 3 h to get better luminescent properties. The incorporation of Eu³⁺ activator in these nanocrystals was checked by luminescence characteristics. These nanocrystals displayed bright red color on excitation under 254 nm UV source. The main emission peak was assigned to the transition [⁵D₀→⁷F₂] at 615 nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) studies were carried out to understand surface morphological features and the particle size. Crystal structures of the nanocrystals were investigated by the X-ray diffraction (XRD) technique. The crystallite size of the as-prepared nanocrystals was around 29 nm, which was evaluated from the broad XRD peaks. The crystallite size increased to ∼45 nm on further heat treatment at 1000 °C.     

Evolution of structure, microstructure and hyperfine properties of nanocrystalline Fe50Co50 powders prepared by mechanical alloying

Nanostructured Fe₅₀Co₅₀ powders were prepared by mechanical alloying of Fe and Co elements in a vario-planetary high-energy ball mill. The structural properties, morphology changes and local iron environment variations were investigated as a function of milling time (in the 0-200 h range) by means of X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray analysis and ⁵⁷Fe Mössbauer spectroscopy. The complete formation of bcc Fe₅₀Co₅₀ solid solution is observed after 100 h milling. As the milling time increases from 0 to 200 h, the lattice parameter decreases from 0.28655 nm for pure Fe to 0.28523 nm, the grain size decreases from 150 to 14 nm, while the meal level of strain increases from 0.0069% to 1.36%. The powder particle morphology at different stages of formation was observed by SEM. The parameters derived from the Mössbauer spectra confirm the beginning of the formation of Fe₅₀Co₅₀ phase at 43 h of milling. After 200 h of milling the average hyperfine magnetic field of 35 T suggests that a disordered bcc Fe-Co solid solution is formed.