Solvothermal one-step synthesis of MWCNTs/Ni0.5Zn0.5Fe2O4 magnetic composites

A magnetic multi-walled carbon nanotubes-based (MWCNTs-based) composite, MWCNTs/Ni_0.5Zn_0.5Fe₂O₄, was synthesized via a facile solvothermal approach. The composites were characterized by X-ray diffraction analysis, transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and vibrating sample magnetometry. The results confirmed that MWCNTs and Ni_0.5Zn_0.5Fe₂O₄ coexisted in the composites. The TEM and HRTEM results showed a thick layer of Ni_0.5Zn_0.5Fe₂O₄ was intimately connected to the surface of MWCNTs. The saturation magnetization value of the composites was 45.8 emu/g. Furthermore, the probable synthesis mechanism of the magnetic composites was also investigated based on the experimental results.     

The structure and magnetic properties of Zn1−xNixFe2O4 ferrite nanoparticles prepared by sol–gel auto-combustion

Zn_1−xNi_xFe₂O₄ ferrite nanoparticles were prepared by sol–gel auto-combustion and then annealed at 700 °C for 4 h. The results of differential thermal analysis indicate that the thermal decomposition temperature is about 210 °C and Ni–Zn ferrite nanoparticles could be synthesized in the self-propagating combustion process. The microstructure and magnetic properties were investigated by means of X-ray diffraction, scanning electron microscope, and Vibrating sample magnetometer. It is observed that all the spherical nanoparticles with an average grain size of about 35 nm are of pure spinel cubic structure. The crystal lattice constant declines gradually with increasing x from 0.8435 nm (x=0.20) to 0.8352 nm (x=1.00). Different from the composition of Zn_0.5Ni_0.5Fe₂O₄ for the bulk, the maximum M_s is found in the composition of Zn_0.3Ni_0.7Fe₂O₄ for nanoparticles. The H_c of samples is much larger than the bulk ferrites and increases with the enlarging x. The results of Zn_0.3Ni_0.7Fe₂O₄ annealed at different temperatures indicate that the maximum M_s (83.2 emu/g) appears in the sample annealed at 900 °C. The H_c of Zn_0.3Ni_0.7Fe₂O₄ firstly increases slightly as the grain size increases, and presents a maximum value of 115 Oe when the grains grow up to about 30 nm, and then declines rapidly with the grains further growing. The critical diameter (under the critical diameter, the grain is of single domain) of Zn_0.3Ni_0.7Fe₂O₄ nanoparticles is found to be about 30 nm.     

Synthesis of nanocrystalline Zn0.5Mn0.5Fe2O4 via in situ polymerization technique

Nanocrystalline Zn_0.5Mn_0.5Fe₂O₄ was synthesized through the pyrolysis of polyacrylate salt precursors prepared via in situ polymerization of the metal salts and acrylic acid. The pyrolysis behavior of the polymeric precursors was studied by use of thermal analysis. The as-obtained product was characterized by powder X-ray diffraction (XRD), transmission electron microscope (TEM), electron diffraction (ED) pattern, scanning electron microscopy (SEM) and electron dispersive X-ray (EDX) analysis. The results revealed that the particle size is in the range of 15–25 nm for Zn-Mn ferrites with good crystallinity. Magnetic properties of the sample at 300 K were measured using a vibrating sample magnetometer, which showed that the sample exhibited characteristics of superparamagnetism.     

Surface magnetic disorder in nanostructured Ni0.5Zn0.5Fe2O4 particles

Nanostructured ferroxide particles with initial formula Ni_0.5Zn_0.5Fe₂O₄ are investigated. The aim was to explore the monodomain and the superparamagnetic states of the ferrospinel and the impact of the surface magnetic disorder on the magnetization processes. Mössbauer spectroscopy (MöS) demonstrated that the ion distribution follows the general formula (Zn_0.5Fe_0.5)_A[Ni_0.5Fe_1.5]_BO₄, where A is the tetrahedral and B, the octahedral sublattice. MöS in an external magnetic field (5 T) at 4.2 K shows non-collinearity of the sublattices’ magnetic moments and deviations in the hyperfine magnetic field that could be related to a canting effect. Magnetic measurements were applied to characterize the temperature behavior of the magnetic properties and the a.c. complex magnetic susceptibility.     

Fabrication and magnetic properties of Ni0.50.5Zn0.5Fe2O4 nanofibres by electrospinning

NiZn ferrite/polyvinylpyrrolidone composite fibres were prepared by sol–gel assisted electrospinning.Ni0.5Zn0.5Fe2O4 nanofibres with a pure cubic spinel structure were obtained subsequently by calcination of the composite fibres at high temperatures.This paper investigates the thermal decomposition process,structures and morphologies of the electrospun composite fibres and the calcined Ni0.5Zn0.5Fe2O4 nanofibres at different temperatures by thermogravimetric and differential thermal analysis,x-ray diffraction,Fourier transform infrared spectroscopy and field emission scanning electron microscopy.The magnetic behaviour of the resultant nanofibres was studied by a vibrating sample magnetometer.It is found that the grain sizes of the nanofibres increase significantly and the nanofibre morphology gradually transforms from a porous structure to a necklace-like nanostructure with the increase of calcination temperature.The Ni0.5Zn0.5Fe2O4 nanofibres obtained at 1000 C for 2 h are characterized by a necklace-like morphology and diameters of 100–200 nm.The saturation magnetization of the random Ni0.5Zn0.5Fe2O4 nanofibres increases from 46.5 to 90.2 emu/g when the calcination temperature increases from 450 to 1000 C.The coercivity reaches a maximum value of 11.0 kA/m at a calcination temperature of 600 C.Due to the shape anisotropy,the aligned Ni0.5Zn0.5Fe2O4 nanofibres exhibit an obvious magnetic anisotropy and the ease magnetizing direction is parallel to the nanofibre axis.     

Maxwell-Wagner characterization of dielectric relaxation in Ni0.8Zn0.2Fe2O4/Sr0.5Ba0.5Nb2O6 composite

Dense composites were prepared through incorporating the dispersed Ni_0.8Zn_0.2Fe₂O₄ ferromagnetic particles into Sr_0.5Ba_0.5Nb₂O₆ ferroelectric matrix. Extrinsic dielectric relaxation and associated high permittivities of the materials are reported in the composites. We used an ideal equivalent circuit to explain electrical responses in impedance formalism. A Debye-like relaxation in the permittivity formalism was also found. Interestingly, real permittivity (ε′) of the sample containing 30% Ni_0.8Zn_0.2Fe₂O₄ shows obvious independence of the temperature at 100 kHz. Dielectric relaxation and high-ε′ properties of the composites are explained in terms of the Maxwell-Wagner (MW) polarization model.     

Microwave anneal effect on magnetic properties of Ni0.6Zn0.4Fe2O4 nano-particles prepared by conventional hydrothermal method

Ni_0.6Zn_0.4Fe₂O₄ ferrite nano-particles with a crystallite size of about 20 nm were prepared by the conventional hydrothermal method, followed by annealing in a microwave oven for 7.5-15 min. The microstructure and magnetic properties of the samples were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The microwave annealing process has slight effect on the morphology and size of Ni_0.6Zn_0.4Fe₂O₄ ferrite nano-particles. However it reduces the lattice parameter and enhances the densification of the particles, and then greatly increases the saturation magnetization (50-56 emu/g) and coercive force of the samples as compared to the non-annealing condition. The microwave annealing process is an effective way to rapidly synthesize high performance ferrite nano-particle.     

Milling time and BPR dependence on permeability and losses of Ni0.5Zn0.5Fe2O4 synthesized via mechanical alloying process

Ni_0.5Zn_0.5Fe₂O₄ has been synthesized using mechanical alloying method with two variables (milling time and ball-to-powder weight ratio (BPR)) were varied in order to study its effect on the magnetic properties of the material. The effects of these two variables were studied using XRD, SEM, TEM and later by impedance analyzer with the frequency range from 1 MHz to 1.8 GHz. The results obtained however show that there are no significant trends to relate the milling time and BPR with the permeability and losses of the material studied. After being sintered at 1150 °C, all the effects of alloying process seem to diminish.     

一维Ni0.5Zn0.5Fe2O4/SiO2复合纳米结构的制备及其磁性能

采用溶胶-凝胶法结合静电纺丝技术制备了Ni_0.5Zn_0.5Fe₂O₄/SiO₂复合纳米纤维.利用热重-差热分析、X射线衍射、场发射扫描电镜、高分辨透射电镜和振动样品磁强计研究了前驱体纤维的热分解及相转化过程以及焙烧温度和SiO₂含量对目标纳米纤维的相组成、微观结构、形貌及磁性能的影响.结果表明,在450 ℃焙烧时,立方尖晶石结构已基本形成.随着焙烧温度由450 ℃升高到100     

Reentrant spin glass behavior and large initial permeability of Co0.5−xMnxZn0.5Fe2O4

A series of polycrystalline ferrites having nominal chemical composition Co_0.50−xMn_xZn_0.5Fe₂O₄ (0<x<0.4) have been synthesized by the solid-state reaction technique. The XRD analysis confirms single phase cubic spinel structure for all compositions. Lattice constant increases from 0.84195 to 0.84429 nm with the increasing Mn content and obeys Vegard's law. The average grain size increases by increasing both Mn content and sintering temperatures. Room temperature saturation magnetization increases for x=0.1 and decreases for increasing Mn content. The coercivity decreases with increasing Mn content due to the decrease of anisotropy constant. A reentrant spin glass behavior of these samples is observed from the zero field cooled magnetization measurements. The real part of the initial permeability increases by increasing both Mn content and sintering temperatures. This is due to the homogeneous grain growth and densification of the ferrites. The highest initial permeability 137 is observed for x=0.4 sintered at 1573 K on the other hand, the highest relative quality factor (2522) is obtained for the sample Co_0.2Mn_0.3Zn_0.5Fe₂O₄ sintered at 1523 K. The Mn substituted Co_0.50−xMn_xZn_0.5Fe₂O₄ ferrites showed improved magnetic properties.     

In situ synthesis and characterization of LiNi0.5La0.08Fe1.92O4-polyaniline core-shell nanocomposites

Core-shell-structured LiNi_0.5La_0.08Fe_1.92O₄-polyaniline (PANI) nanocomposites with magnetic behavior were synthesized by in situ polymerization of aniline in the presence of LiNi_0.5La_0.08Fe_1.92O₄ nanoparticles. The structure, morphology and magnetic properties of samples were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), UV-vis absorption, transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) technique. The results of spectroanalysis indicated that there was interaction between PANI chains and ferrite particles. TEM study showed that LiNi_0.5La_0.08Fe_1.92O₄-PANI nanocomposites presented a core-shell structure with a magnetic core of 30-50 nm diameter and an amorphous shell of 10-20 nm thickness. The nanocomposites under applied magnetic field exhibited the hysteresis loops of the ferromagnetic nature. The saturation magnetization and coercivity of nanocomposites decreased with decreasing content of LiNi_0.5La_0.08Fe_1.92O₄. The polymerization mechanism and bonding interaction in the nanocomposites have been discussed.     

Synthesis and magnetic characterization of Zn0.7Ni0.3Fe2O4 nanoparticles via microwave-assisted combustion route

We report on the synthesis of Zn_0.7Ni_0.3Fe₂O₄ nanoparticles via microwave assisted combustion route by using urea as fuel. XRD and FT-IR analyses confirm the composition and structure as spinel ferrite. The crystallite size estimated from XRD (16.4 nm) and the magnetic core size (15.04 nm) estimated from VSM agree well, while a slightly smaller magnetic diameter reflects a very thin magnetically dead layer on the surface of the nanoparticles. Morphological investigation of the products was done by TEM which revealed the existence of irregular shapes such spherical, spherodial and polygon. Magnetization measurements performed on Zn_0.7Ni_0.3Fe₂O₄ nanoparticles showed that saturation was not attained at even in the high magnetic field. The sample shows superparamagnetic behavior at around the room temperature and ferromagnetic behavior below the blocking temperature which is measured as 284 K.     

Effect of calcination temperature on the structure and hydroxylation activity of Ni0.5Cu0.5Fe2O4 nanoparticles

Nanocrystalline Ni_0.5Cu_0.5Fe₂O₄ was synthesized by sol-gel method with varying calcination temperature over the range of 500-1000. The powders obtained were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). In addition, thermal analysis (TG-DTG-DTA) of the precursor was carried out. The study reveals the simultaneous decomposition and ferritization process at rather low temperature (280-350). For the crystalline structure investigated, single cubic spinel is gained when the precursor was decomposed at 800-1000, whereas separated crystal CuO formed when calcination temperature is below 800. The increase of calcination temperature favors the appearance of Fe_B³⁺, Cu_A²⁺ and O on the spinel surface. The hydroxylation activity is relative to the amount of Cu_B²⁺ species on the spinel surface. The lattice oxygen species on the spinel surface are favorable for the deep oxidation of phenol.     

Chemical synthesis of spinel nickel ferrite (NiFe2O4) nano-sheets

The present investigation is related to the deposition of single-phase nano-sheets spinel nickel ferrite (NiFe₂O₄) thin films onto glass substrates using a chemical method. Nano-sheets nickel ferrite films were deposited from an alkaline bath containing Ni²⁺ and Fe²⁺ ions. The films were characterized for their structural, surface morphological and electrical properties by means of X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and two-point probe electrical resistivity techniques. The X-ray diffraction pattern showed that NiFe₂O₄ nano-sheets are oriented along (3 1 1) plane. The FT-IR spectra of NiFe₂O₄ films showed strong absorption peaks around 600 and 400 cm⁻¹ which are typical for cubic spinel crystal structure. Microstructural study of NiFe₂O₄ film revealed nano-sheet like morphology with average sheet thickness of 30 nm. The room temperature electrical resistivity of the NiFe₂O₄ nano-sheets was 10⁷ Ω cm.     

Synthesis and magnetic properties of hard/soft SrFe12O19/Ni0.7Zn0.3Fe2O4 nanocomposite magnets

Magnetic nanocomposite SrFe₁₂O₁₉/Ni_0.7Zn_0.3Fe₂O₄ powders with different weight fractions of the Ni_0.7Zn_0.3Fe₂O₄ soft ferrite were synthesized by a combination of the sol–gel self-propagation and glyoxilate precursor methods. The results of magnetic measurements revealed the higher Mr/Ms ratio for the nanocomposites than that for the single phase SrFe₁₂O₁₉ which proves the existence of the intergrain exchange coupling between hard and soft magnetic phases with the exchange spring behavior. The highest Mr/Ms ratio of 0.63 was obtained in the composite consisting of 80 wt% of SrFe₁₂O₁₉ and 20 wt% Ni_0.7Zn_0.3Fe₂O₄. The microstructural studies of this sample exhibited the average dimensions of hard and soft phases about 20 nm and 15 nm, respectively which are small enough for strong exchange coupling according to the theoretical studies. The variations of the reduced remanence (Mr/Ms) with increasing the weight fraction of the soft phase could be also explained by the role of the exchange and dipolar interactions in tuning the magnetic properties of the nanocomposites.     

Estimating the cation distributions in the spinel ferrites Cu0.5−xNi0.5ZnxFe2O4 (0.0≤x≤0.5)

Ferrite samples of the composition Cu_0.5−xNi_0.5Zn_xFe₂O₄ (0.0≤x≤0.5) were synthesized by chemical co-precipitation. The samples exhibited a single phase cubic spinel structure, and the saturation magnetization of the samples was found to increase with increasing Zn content. Using a quantum mechanical method proposed by our group, the cation distributions in the samples were estimated. Estimated cation distributions obtained by fitting the magnetic moments of the samples were then used to perform Rietveld fitting for X-ray diffraction patterns. The acceptable error parameters in the Rietveld fitting indicate that the estimated cation distributions in the samples are reasonable.     

Effect of grain size on the magnetic properties of superparamagnetic Ni0.5Zn0.5Fe2O4 nanoparticles by co-precipitation process

Ni_0.5Zn_0.5Fe₂O₄ (NZFO) spinel-type nanoparticles were directly fabricated by the chemical co-precipitation process using metal nitrate and acetate as precursors since nitrogen and carbon would be taken away in the forms of oxynitride and oxycarbide, respectively, after the precursors were annealed and then investigated in detail by employing X-ray diffraction (XRD), magnetic measurement and Raman spectroscopy. XRD analysis indicates that the as-prepared nanocrystals are all of a pure cubic spinel structure with their sizes ranging from 20.8 to 53.3 nm, as well as peaks of some samples shifting to lower angles due to lattice expansion. Calculations from the derived XRD data indicate that the activation energy is 30.83 kJ/mol. The magnetic measurements show that these samples are superparamagnetic. The saturation magnetization increases with annealing temperature, which may be explained by super-exchange interactions of Fe ions occurring at A- and B-sites. The variation of coercivity with particle size is interpreted on the basis of domain structure and crystal anisotropy. Furthermore, these nanoparticles exhibit a redshift phenomenon at lower temperatures seen in the Raman spectra, which could be related to ionic substitution.     

Preparation and magnetic properties of BaFe12O19/Ni0.8Zn0.2Fe2O4 nanocomposite ferrite

Nanocomposite of hard (BaFe₁₂O₁₉)/soft ferrite (Ni_0.8Zn_0.2Fe₂O₄) have been prepared by the sol–gel process. The nanocomposite ferrite are formed when the calcining temperature is above 800 °C. It is found that the magnetic properties strongly depend on the presintering treatment and calcining temperature. The “bee waist” type hysteresis loops for samples disappear when the presintering temperature is 400 °C and the calcination temperature reaches 1100 °C owing to the exchange-coupling interaction. The remanence of BaFe₁₂O₁₉/Ni_0.8Zn_0.2Fe₂O₄ nanocomposite ferrite with the mass ratio of 5:1 is higher than a single phase ferrite. The specific saturation magnetization, remanence magnetization and coercivity are 63 emu/g, 36 emu/g and 2750 G, respectively. The exchange-coupling interaction in the BaFe₁₂O₁₉/Ni_0.8Zn_0.2Fe₂O₄ nanocomposite ferrite is discussed.     

Preparation and characterization of Zn2SiO4: Mn phosphors with hydrothermal methods

Mn²⁺-doped Zn₂SiO₄ phosphors had been prepared by hydrothermal method in stainless-steel autoclaves. Effects of synthesized methods, reaction temperature, ambience of heat treatment on the structure and the luminescence properties of this silicate were studied with X-ray diffraction apparatus (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM) and fluorescence spectrum. Results show that Zn₂SiO₄ nanocrystalline can be obtained by hydrothermal method at relatively low temperatures. The absorption pattern shows an absorption edge at about 380 nm originated from ZnO crystals and two absorption bands at about 215 and 260 nm. Mn²⁺-doped Zn₂SiO₄ has a luminescence band with the wavelength at about 522 nm under 255 nm excitation, and the luminescent intensity increases after being heat treated.     

Dependence of magnetic properties and microstructure of mechanically alloyed Ni0.5Zn0.5Fe2O4 on soaking time

Possible soaking-time effects on the magnetic and microstructural properties of polycrystalline samples of Ni_0.5Zn_0.5Fe₂O₄ have been studied. Nanosize powder produced by mechanical alloying was sintered at 800 °C with various soaking times. All samples showed the signature peak of Ni_0.5Zn_0.5Fe₂O₄ even with one hour of soaking time. The size distributions show a slow growth of microstructural evolution related to density, porosity and also to the magnetic hysteresis loops. Within these distributions it is observed that the formation of multi-domains is not possible and probably there are the regions of superparamagnetic and single-domain grains. From the permeability studies, it is believed that the rise of the magnetic moment on the B sites give rise to the total saturation magnetization with increase of soaking time. The hysteresis loop of one-hour soaking time showed paramagnetic behavior dominating while longer soaking times showed ferromagnetic behavior starting to dominate. The coercivity was observed to increase with soaking time, signaling the increase of the anisotropy fields which was attributed to the shape anisotropy and also to the magnetocrystalline anisotropy. By correlating the morphology, phase analysis, permeability and hysteresis loops results, it is believed that there was an increase in number of crystalline-growth regions which together formed a total mass of mixed superparamagnetic and ferromagnetic grains with the latter starting to dominate the samples.