Synthesis and characterization of NiCoMnCuFe1.96O4 for circulator application

Modern accelerator design practice includes the use of high-quality ferrites for circulator applications with ever-increasing requirements on power handling ability. Modeling studies of new designs are of increasing economic importance, but are frequently hindered by lack of measured values of the ceramic loss factors. We have developed a nanocrystalline ferrite material with composition Ni_0.94Co_0.03Mn_0.04Cu_0.03Fe_1.96O₄. Nanocrystalline NiCoMnCu ferrite powders were synthesized using a microwave-hydrothermal method at 160 °C for 40 min. The ferrite formation conditions, such as pH, temperature and time, were optimized. The phase of the samples was identified by X-ray diffraction and was characterized by Fourier transformation infrared spectroscopy. The size of the nanocrystalline ferrite of as-synthesized powders was 10 nm. The powder was densified at different temperatures using a microwave sintering method. The complex permittivity and permeability of the sintered samples were measured over a frequency range from 10 kHz to 1.8 GHz at room temperature. The applicability of the samples for circulators was tested via the measurement of the ferromagnetic resonance linewidth and the results are presented.     

Ultrasonic cavitation induced water in vegetable oil emulsion droplets--a simple and easy technique to synthesize manganese zinc ferrite nanocrystals with improved magnetization

In the present investigation, synthesis of manganese zinc ferrite (Mn_0.5Zn_0.5Fe₂O₄) nanoparticles with narrow size distribution have been prepared using ultrasound assisted emulsion (consisting of rapeseed oil as an oil phase and aqueous solution of Mn²⁺, Zn²⁺ and Fe²⁺ acetates) and evaporation processes. The as-prepared ferrite was nanocrystalline. In order to remove the small amount of oil present on the surface of the ferrite, it was subjected to heat treatment at 300 °C for 3 h. Both the as-prepared and heat treated ferrites have been characterized by X-ray diffraction (XRD), infrared spectroscopy (IR), TGA/DTA, transmission electron microscopy (TEM) and energy dispersion X-ray spectroscopy (EDS) techniques. As-prepared ferrite is of 20 nm, whereas the heat treated ferrite shows the size of 33 nm. In addition, magnetic properties of the as-prepared as well as the heat treated ferrites have also been carried out and the results of which show that the spontaneous magnetization (σ_s) of the heat treated sample (24.1 emu/g) is significantly higher than that of the as-synthesized sample (1.81 emu/g). The key features of this method are avoiding (a) the cumbersome conditions that exist in the conventional methods; (b) usage of necessary additive components (stabilizers or surfactants, precipitants) and (c) calcination requirements. In addition, rapeseed oil as an oil phase has been used for the first time, replacing the toxic and troublesome organic nonpolar solvents. As a whole, this simple straightforward sonochemical approach results in more phase pure system with improved magnetization.     

Studies of structural evolution and sensing properties of ZnO nanocrystalline films

ZnO nanocrystalline films have been prepared on Si(1 0 0) substrate using direct current (D.C) magnetron sputtering technique at room temperature. The thickness of nanocrystalline films almost linearly increased with deposition duration and the sizes of crystalline grains almost kept unchanged. After deposition, thermal annealing was performed at 800 °C in atmosphere for 2 h in order to improve the qualities of ZnO thin films. Scanning electron microscope (SEM) images showed the surface roughness of the films less than 45 nm. X-ray diffraction (XRD) patterns revealed the slight evolution of the crystal structures. Raman scattering spectra confirmed the data obtained from X-ray diffraction measurements.With these ZnO nanocrystalline films, prototypic gas sensors were fabricated. Both sensitivity and response of the sensors to different gases (H₂ and CH₄) were investigated. A quick response of time, less than 1 second to CH₄ gas sensor has been achieved.     

Effect of zinc substitution on magnetic and electrical properties of nanocrystalline nickel ferrite synthesized by refluxing method

Nanocrystalline Nickel ferrite (NiFe₂O₄) and Zn substituted nickel ferrite (NiZnFe₂O₄) have been synthesized by the refluxing method. These ferrites were characterized by XRD, TEM, Mossbauer spectroscopy and VSM in order to study the effect of zinc substitution in nickel ferrite. XRD diffraction results confirm the spinel structure for the prepared nanocrystalline ferrites with an average crystallite size of 14-16 nm. Lattice parameter was found to increase with the substitution of Zn²⁺ ions from 8.40 Å to 8.42 Å. TEM images confirmed average particle size of about 20 nm and indicates nanocrystalline nature of the compounds. A shift in isomeric deviation with the doublet was observed due to the influence of Zn substitution in the nickel ferrite. The Zn content has a significant influence on the magnetic behavior and electrical conductivity of NiFe₂O₄. Saturation magnetization drastically increased whereas room temperature electrical conductivity decreased due to the addition of Zn content in NiFe₂O₄, indicating super magnetic material with lesser coercivity.     

Comparative study of structural and magnetic properties of nano-crystalline Li0.5Fe2.5O4 prepared by various methods

Lithium ferrite has been considered as one of the highly strategic magnetic material. Nano-crystalline Li_0.5Fe_2.5O₄ was prepared by four different techniques and characterized by X-ray diffraction, vibrating sample magnetometer (VSM), transmission electron microscope (TEM) and Fourier transform infrareds (FTIR). The effect of annealing temperature (700, 900 and 1050 °C) on microstructure has been correlated to the magnetic properties. From X-ray diffraction patterns, it is confirmed that the pure phase of lithium ferrite began to form at 900 °C annealing. The particle size of as-prepared lithium ferrite was observed around 40, 31, 22 and 93 nm prepared by flash combustion, sol-gel, citrate precursor and standard ceramic technique, respectively. Lithium ferrite prepared by citrate precursor method shows a maximum saturation magnetization 67.6 emu/g at 5 KOe.     

Iron-based soft magnetic composites with Mn–Zn ferrite nanoparticles coating obtained by sol–gel method

This paper focuses on iron-based soft magnetic composites which were synthesized by utilizing Mn–Zn ferrite nanoparticles to coat iron powder. The nanocrystalline iron powders, with an average particle diameter of 20 nm, were obtained via the sol–gel method. Scanning electron microscopy, energy dispersive X-ray spectroscopy and distribution maps show that the iron particle surface is covered with a thin layer of Mn–Zn ferrites. Mn–Zn ferrite uniformly coated the surface of the powder particles, resulting in a reduced imaginary permeability, increased electrical resistivity and a higher operating frequency of the synthesized magnets. Mn–Zn ferrite coated samples have higher permeability and lower magnetic loss when compared with the non-magnetic epoxy resin coated compacts. The real part of permeability increases by 33.5% when compared with the epoxy resin coated samples at 10 kHz. The effects of heat treatment temperature on crystalline phase formation and on the magnetic properties of the Mn–Zn ferrite were investigated via X-ray diffraction and a vibrating sample magnetometer. Ferrites decomposed to FeO and MnO after annealing above 400 °C in nitrogen; thus it is the optimum annealing temperature to attain the desired permeability.     

Magnetic properties of xNi0.53Cu0.12Zn0.35Fe1.88O4+(1−x)BaTiO3 nanocomposites

The nanocrystalline Ni_0.53Cu_0.12Zn_0.35Fe_1.88O₄ and BaTiO₃ powders were prepared using Microwave-Hydrothermal (M-H) method at 160 °C/45 min. The as synthesized powders were characterized using the X-ray diffraction (XRD) and Transmission Electron Microscope (TEM). The size of the powders that were synthesized using M-H system was found to be ∼30 and ∼50 nm for ferrite phase and ferroelectric phases, respectively. The powders were densified using microwave sintering method at 900 °C/30 min. The ferrite and ferroelectric phases were observed from XRD and morphology of the composites was observed with the Scanning Electron Microscope (SEM).The magnetic hysteresis loops were recorded using the Vibrating Sample Magnetometer (VSM).The frequency dependence of real (μ′) and imaginary (μ″) parts of permeability was measured in the range of 1 MHz-1.8 GHz. The permeability decreases with an increase of BaTiO₃ content at 1 MHz. The transition temperature (T_C) of ferrite was found to be 245 °C. The T_C of composite materials decreases with an increase in BaTiO₃ content.     

Structural characterization and magnetic properties of superparamagnetic zinc ferrite nanoparticles synthesized by the coprecipitation method

Single phase zinc ferrite (ZnFe₂O₄) nanoparticles have been prepared by the coprecipitation method without any subsequent calcination. The effects of precipitation temperature in the range 20–80 °C on the structural and the magnetic properties of zinc ferrite nanoparticles were investigated. The crystallite size, microstructure and magnetic properties of the prepared nanoparticles were studied using X-ray diffraction (XRD), Fourier transmission infrared spectrum, transmission electron microscope (TEM), energy dispersive X-ray spectrometer and vibrating sample magnetometer. The XRD results showed that the coprecipitated nanoparticles were single phase zinc ferrite with mixture of normal and inverse spinel structures. Furthermore, ZnFe₂O₄ nanoparticles have the crystallite size in the range 5–10 nm, as confirmed by TEM. The magnetic measurements exhibited that the zinc ferrite nanoparticles synthesized at 40 °C were superparamagnetic with the maximum magnetization of 7.3 emu/g at 10 kOe.     

Synthesis and luminescence properties of nanocrystalline LiF:Mg,Cu,P phosphor

Nanocrystalline LiF:Mg,Cu,P phosphor material of different shapes and sizes (microcrystalline cubic shape, nanorod shape and nanocrystalline cubical shaped) have been prepared by the chemical co-precipitation method. Thermoluminescence (TL) and other dosimetric characteristics of the phosphor are studied and presented here. The formation of the materials was confirmed by the X-ray diffraction (XRD). Its shapes and sizes were also observed using scanning electron microscope (SEM). The TL glow curve of the microcrystalline powder shows a prominent single peak at 408 K along with another peak of lesser intensity at around 638 K. On the contrary, the nanocrystalline rod shaped particles show a peak of low intensity at 401 K and a prominent peak around 700 K while the nanocrystalline particles in cubical shapes again show two peaks, one at around 407 K and the other at around 617 K, of which the lower temperature (407 K) peak is more prominent. The glow curve structure changes at very high doses (100 kRad) and some new peaks appear at around 525 and 637 K also the first peak appearing at around 401 K becomes prominent. The observed changes in TL due to the change in the shape and sizes of the nanophosphor have been reported. The PL has also been studied and various excitation and emission peaks observed due to the presence of various impurities are explained. The observed results have been explained in the light of asymmetrical crystal field effects due to asymmetrical shapes of the nanocrystalline phosphor. The comparison of these properties with the microcrystalline material prepared by the same co-precipitation method is also done.     

Novel combustion route of synthesis and characterization of nanocrystalline mixed ferrites of Ni-Zn

A novel combustion method of synthesis has been employed in this study for the preparation of nanoparticles of Ni-Zn ferrites. The preparation method is simple yet effective and its novelty lies in the direct mixing of reactants and the fuel. The structural and morphological studies on the nanoparticles of Ni-Zn ferrites have been carried out using X-ray diffractometer (XRD) and scanning electron microscope (SEM). The values of grain size of the ferrites obtained using the Scherrer's formula are in the range between 10 and 20 nm. The mean value of X-ray density of the Ni-Zn ferrites is around 5343 Kg/m³, which is more than the one experimentally observed for their bulk counterparts. The distribution of cations has been proposed theoretically for each concentration of Ni-Zn ferrite with reference to their respective experimental lattice constant values. Room-temperature magnetic measurements are carried out using vibrating sample magnetometer (VSM) with a view to understand the impact of the nano-regime on the magnetic parameters. The observed values of magnetization are in the range from 4 to 26 emu/g which is lower than that of bulk particles of Ni-Zn ferrite.     

Magnetic and structural studies of the Mn-doped Mg–Zn ferrite nanoparticles synthesized by the glycine nitrate process

In this study, Nanocrystalline Mn–Mg–Zn ferrite with the chemical formula Mn_xMg_0.5−xZn_0.5Fe₂O₄ (x=0, 0.1, 0.2, 0.3, 0.4, 0.5) was successfully synthesized by the glycine-nitrate autocombustion process using glycine as a fuel and nitrates as oxidants. The as-synthesized powders were characterized by the X-ray diffraction analysis, field emission scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer. The X-ray diffraction data was used to determine the lattice constant, cation distribution and the oxygen position parameter. The results reveal that the nanocrystalline Mn–Mg–Zn ferrite has an average crystallite size of 35–67 nm and particle size of 40 nm. The lattice parameter increases linearly with an increase in the Mn content. The FTIR analysis confirms the intrinsic vibrational frequencies of the tetrahedral and octahedral of the spinel structure. The magnetic measurements indicate that the coercivity decreases, and the magnetization increases by increasing the Mn content.     

Influence of acid catalysts on the structural and magnetic properties of nanocrystalline barium ferrite prepared by sol–gel method

BaFe₁₂O₁₉ powders with nanocrystalline size were prepared by sol–gel techniques. Nitric, hydrochloric, acetic and stearic acid were used to improve the magnetic properties. Amorphous gels were formed with Fe/Ba molar ratio of 10.5. Then powders were obtained by subsequent heat treatment at 800–1000 °C for 1 h. Barium ferrite powder was also synthesized by solid state reaction at 1210 °C. X-ray diffraction, scanning electron microscopy and transmission electron microscopy (TEM) experiments were conducted to evaluate structural properties of the samples. The value of the effective magnetic susceptibility was measured. The results show that the magnetoplumbite structure was formed in all of the powders. The TEM observation showed that the minimum particle size (20 nm) was produced with the stearic acid catalyst. The highest value of the effective magnetic susceptibility was achieved also using stearic acid.     

Synthesis and magnetic properties of cobalt ferrite (CoFe2O4) nanoparticles prepared by wet chemical route

Magnetic nanoparticles of cobalt ferrite have been synthesized by wet chemical method using stable ferric and cobalt salts with oleic acid as the surfactant. X-ray Diffraction (XRD) and Transmission Electron Microscope (TEM) confirmed the formation of single-phase cobalt ferrite nanoparticles in the range 15–48 nm depending on the annealing temperature and time. The size of the particles increases with annealing temperature and time while the coercivity goes through a maximum, peaking at around 28 nm. A very large coercivity (10.5 kOe) is observed on cooling down to 77 K while typical blocking effects are observed below about 260 K. The high field moment is observed to be small for smaller particles and approaches the bulk value for large particles.     

Room temperature single-step electrosynthesized copper ferrite thin films and study of their magnetic properties

A single-step electrosynthesis of copper ferrite thin films from aqueous bath (which avoids anodization step for an incorporation of oxygen species into deposit) has been carried out at room temperature. Observed tetrahedral structured nanocrystalline copper ferrite thin films showed smooth, uniform and compact surface morphology. After annealing, increase in dielectric constant and reduced dielectric loss were observed. The saturation magnetization for annealed films was 292 emu/cm³ comparable to that of other reported ferrites.     

Investigating the magnetic properties of soft magnetic composites based on mechanically alloyed nanocrystalline Fe-5 wt% Ni powders

In this work, the soft magnetic composites (SMCs) of the nanocrystalline Fe-5 wt% Ni powders coated with phenolic resin were studied. The nanocrystalline powders with an average diameter of 10 nm were obtained by mechanical alloying up to 96 h milling in a high-energy planetary ball mill. The microstructure and magnetic properties of the milled powders were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy and a vibrating sample magnetometer. The results of X-ray diffraction showed that the bcc Fe(Ni) solid solution is formed after 24 h milling. Magnetic measurements indicated that the 96 h milled powders with a steady-state grain size of 10 nm have the highest saturation magnetization and the lowest coercivity. The SMCs based on nanocrystalline powders showed higher electrical resistivity and magnetic permeability up to 1 MHz, as compared with the pure iron-based composites. Besides, the nanocrystalline-based SMCs exhibited higher relaxation frequency and a significantly lower loss factor up to 1 MHz.     

Effects of applied magnetic field and pressures on the magnetic properties of nanocrystalline CoFe2O4 ferrite

Nanocrystalline CoFe₂O₄ ferrite with crystallite sizes of 30 nm have been successfully prepared by an emulsion method. X-ray diffractometer (XRD) shows that nanocrystalline CoFe₂O₄ ferrite possesses face center cubic structure. Crystal structure of the CoFe₂O₄ nanocrystals will not be changed by the applied magnetic field and pressures. The obtained CoFe₂O₄ nanocrystalline powders were pressed into thin columns with different pressures. Meanwhile, the dependences of the applied pressures and the direction of applied magnetic field on the magnetic properties of the CoFe₂O₄ nanocrystals were investigated in detail using vibrating sample magnetometer (VSM). The pressed CoFe₂O₄ nanocrystal gains the most excellent magnetisms in a parallel applied magnetic field.     

Nanocrystalline formation and optical properties of germanium thin films prepared by physical vapor deposition

Amorphous and nanocrystalline germanium thin films were prepared on glass substrates by physical vapor deposition (PVD). The influence of thermal annealing on the characteristics of the Ge thin films has been investigated. X-ray diffraction (XRD) and SEM show amorphous structure of films deposited at room temperature. After thermal annealing, the crystallinity was improved when the annealing temperature increases. The Ge thin films annealed at different temperatures in air were nanocrystalline, having the face-centered cubic structure with preferred orientation along the 〈1 1 1〉 direction. The nanostructural parameters have been evaluated by using a single-order Voigt profile analysis. Moreover, the analysis of the optical transmission and reflection behavior was carried out. The values of direct and indirect band gap energies for amorphous and nanocrystalline phases are 0.86±0.02, 0.65±0.02 and 0.79±0.02, 0.61±0.02 eV, respectively. In addition, the complex optical functions for the wavelength range 600-2200 nm are reported. The refractive index of the nanocrystalline phase drops from 4.80±0.03 to 2.04±0.02, and amorphous phase changes from 5.18±0.03 to 2.42±0.02 for the whole wavelength range. The dielectric functions ε₁ and ε₂ of the deposited films were recorded as a function of wavelength within the range from 600 to 2200 nm.     

Fabrication and characterization of nanocrystalline n-CdO/p-Si as a solar cell

A nanocrystalline CdO/Si solar cell was fabricated via deposition of a CdO thin film on p-type silicon substrate with approximately 370 nm thickness using solid–vapor deposition for Cd powder at 1274 K with argon and oxygen flow. Scanning electron microscopy revealed that the product was a Cadmium oxide nanocrystalline. X-ray diffraction and energy dispersive X-ray analysis were used to characterize the structural properties of the solar cell. The nanocrystalline thin film had a grain size of 38 nm. The solar cell yielded a minimum effective reflectance that exhibited excellent light-trapping at wavelengths ranging from 400 to 1000 nm. Photoluminescence spectroscopy was conducted to investigate the optical properties. The direct band gap energy of the nanocrystalline CdO thin film was 2.46 eV. CdO/Si solar cell photovoltaic properties were examined under 100 mW/cm² solar radiation. The cell showed an open circuit voltage (V_oc) of 457 mV, a short-circuit current density (J_sc) of 18.5 mA/cm², a fill factor (FF) of 0.652, and a conversion efficiency (η) of 5.51%.     

Second and third order nonlinear optical properties of nanostructured ZnO thin films deposited on α-BBO and LiNbO3

The nanocrystalline ZnO films were deposited on α-BaB₂O₄ (0 0 1 2) and LiNbO₃ (0 0 0 1) single crystals by RF-magnetron sputtering technique. Their structure was studied using X-ray diffractometry, scanning electron microscopy and atomic force microscopy. Besides, the optical absorption spectra were investigated. The second and third harmonic generation measurements were performed by means of the rotational Maker fringe technique using Nd:YAG laser at 1064 nm in picoseconds regime. Finally, the second and third order nonlinear susceptibilities were determined and their values have been found and compared.     

Ni–Zn nanoferrite for radar-absorbing material

Nanoparticles of nickel–zinc ferrite have been prepared by using the citrate precursor method. According to scanning electron microscopy (SEM), the particle size is nanometric for the powder calcined at 350 °C/3.5 h. The phase formation has been studied by applying different calcining atmospheres, such as air and argon. Pure Ni–Zn ferrite has been observed when calcined in argon at the temperature of 350 °C. Hysteresis analyses have been done with magnetization of 53.01 emu/g at 350 °C and obtaining 84.62 emu/g at 1100 °C due to an optimization of domains formation at high temperature. Measures of reflectivity of Ni–Zn ferrite/epoxy composite have been obtained below 21% at 350 °C and above 96% at 1100 °C with a coercive field of 26.61 Oe. Low value of coercive field increased the mobilization of domains wall and increased the radiation absorption.