Sol-gel preparation and characterization of CoFe2O4-SiO2 nanocomposites

Magnetic nanocomposites formed by cobalt ferrite particles dispersed in a silica matrix were prepared by a sol-gel process. The effects of the thermal treatment temperature and the salt concentration on the structural and magnetic properties of the composites were investigated. By controlling these parameters, CoFe₂O₄/SiO₂ nanocomposites with different crystallite size and magnetic properties were obtained. By increasing the annealing temperature and salt concentration, composites with a progressive increase in the coercive field and of the density of magnetization were produced. In particular, a nanocomposite, with a Fe/Si molar concentration of 21%, obtained by drying the gel at 150 °C and further annealing at 800 °C, has a coercivity of 2000 Oe, which is more than twice higher than the coercivity of bulk cobalt ferrite.     

Preparation and characterization of NiFe2O4/NiO composite film via a single-source precursor route

NiFe₂O₄/NiO nanocomposite thin films have been successfully prepared through a facile route using nickel iron layered double hydroxide (NiFe-LDH) as a single-source precursor. This synthetic approach mainly involves the formation of NiFe-LDH film by casting the slurry of NiFe-LDH precursor on the α-Al₂O₃ substrate, followed by high-temperature calcination. The composition, microstructure and properties of the films were characterized in detail by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX) and vibrating sample magnetometer (VSM). The results indicate that NiFe₂O₄/NiO composite film was composed of granules with diameter less than 100 nm, and the thickness of the film was in the range 1-2 μm. The magnetization of the film can be tuned by alternating the Ni/Fe molar ratio of LDH precursor. In addition, the method developed should be easily extended to fabricate other MFe₂O₄/MO composite film systems with specific applications just by an appropriate combination of divalent/trivalent composition in the precursor of LDHs.     

Solid state reaction synthesis of NiFe2O4 nanoparticles

Ni-ferrite (NiFe₂O₄) nanoparticles have been synthesized via a solid state reaction process. Ni and Fe bi-metallic nanoparticles in the form of Ni₃₃Fe₆₇ alloy nanopowder are first synthesized by simultaneous evaporation of the required amounts of pure Ni and Fe metals followed by rapid condensation of the evaporated metal flux into solid state by means of an inert gas, helium, using the process of inert gas condensation (IGC). In order to form the NiFe₂O₄ structure, as-synthesized samples (Ni₃₃Fe₆₇) are annealed for 12 h in ambient conditions at different annealing temperatures. Structural analyses show that NiFe₂O₄ starts to form at around 450 °C and gets progressively well defined with increasing annealing temperatures yielding particle with size ranging between 15 and 50 nm. Besides successfully forming NiFe₂O₄, NiO/Fe₃O₄ core/shell nanoparticles have also been synthesized by adjusting the annealing conditions. Three different structures, Ni₃₃Fe₆₇, NiO/Fe₃O₄, and NiFe₂O₄, obtained in this study are compared with respect to their structural and magnetic properties.     

Non-isothermal decomposition of NiC2O4-FeC2O4 mixture aiming at the production of NiFe2O4

The non-isothermal decomposition of NiC₂O₄·2H₂O-FeC₂O₄·2H₂O (1:2 mole ratio) mixture was studied on heating to the formation of NiO-Fe₂O₃ mixture at 350 °C in air atmosphere using thermogravimetry. Kinetic analysis of data according to the integral composite method showed that the oxidative decomposition of FeC₂O₄ and NiC₂O₄ are best described by the three-dimensional phase boundary model. The activation parameters were calculated and discussed. The solid products at different decomposition stages were identified using XRD, Mössbauer and FT-IR spectroscopic techniques. Some characteristic XRD lines of NiFe₂O₄ start to appear at 800 °C beside the characteristic lines of NiO and Fe₂O₃, whereas at 1000 °C, only the characteristic lines of single phase cubic NiFe₂O₄ appeared. The Mössbauer spectrum at 1000 °C fitted into two Zeeman sextets characteristic of Fe³⁺ on the tetrahedral (A) and octahedral (B) sites of NiFe₂O₄ inverse spinel. Consistent results were obtained using FT-IR where the absorption bands appeared at 602 and 407 cm⁻¹ for the mixture calcined at 1000 °C. These can be assigned to the intrinsic vibrations of tetrahedral and octahedral sites of NiFe₂O₄, respectively.     

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.     

Grain size effect on the dielectric and magnetic properties of NiFe2O4 ceramics

Nanocrystalline NiFe₂O₄ powders with different crystal sizes were hydrothermally synthesized with different alkali concentrations at 230 °C. Then the NiFe₂O₄ nanopowders were sintered at various temperatures to obtain NiFe₂O₄ ceramics with different grain sizes. The NiFe₂O₄ ceramic properties were strongly dependent on the grain size. With the increase in the grain size, saturation magnetization (M_s) and magnetic permeability (μ) increased, Curie temperature (T_c) decreased. Dielectric constant enhanced and dielectric loss decreased in nanoferrites. The possible mechanism of grain size dependences was discussed in detail.     

Analysis of exchange bias effect of NiO+NiFe2O4 composites

Exchange bias (EB) and magnetic properties of ferrimagnetic (FI) NiFe₂O₄ and antiferromagnetic (AFM) NiO bulk composites, prepared by a chemical co-precipitation and post-thermal decomposition method from Fe-doped NiO matrix, have been investigated. Enhanced coercivities and shifted hysteresis loops are still observed for these samples after field cooling. But the vertical magnetization shifts are not observed. In comparison with the bulk samples, a NiO/10% NiFe₂O₄ nanocomposite was also prepared via direct mixture, in which both the horizontal and vertical shift in the hysteresis loops are observed at 10 K. The observed phenomena are explained in terms of interfacial exchange interaction between the two phases and the finite-size effect, respectively.     

Al2O3/SiO2 films prepared by electron-beam evaporation as UV antireflection coatings on 4H-SiC

Al₂O₃/SiO₂ films have been deposited as UV antireflection coatings on 4H-SiC by electron-beam evaporation and characterized by reflection spectrum, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The reflectance of the Al₂O₃/SiO₂ films is 0.33% and 10 times lower than that of a thermally grown SiO₂ single layer at 276 nm. The films are amorphous in microstructure and characterize good adhesion to 4H-SiC substrate. XPS results indicate an abrupt interface between evaporated SiO₂ and 4H-SiC substrate free of Si-suboxides. These results make the possibility for 4H-SiC based high performance UV optoelectronic devices with Al₂O₃/SiO₂ films as antireflection coatings.     

Effect of SnO2 coating on the magnetic properties of nanocrystalline CuFe2O4

Nanocrystalline CuFe₂O₄ and CuFe₂O₄/xSnO₂ nanocomposites (x=0, 1, 5 wt%) have been successfully synthesized by one-pot reaction of urea-nitrate combustion method. The transmission electron microscope study reveals that the particle size of the as synthesized CuFe₂O₄ and CuFe₂O₄/5 wt%SnO₂ are 10 and 20 nm, respectively. The SnO₂ coating on the nanocrystalline CuFe₂O₄ was confirmed from HRTEM studies. The resultant products were sintered at 1100 °C and characterized by XRD and SQUID for compound formation and magnetic studies, respectively. The X-ray diffraction pattern shows the well-defined sharp peak that confirms the phase pure compound formation of tetragonal CuFe₂O₄. The zero field cooled (ZFC) and field cooled (FC) magnetization was performed using SQUID magnetometer from 2 to 350 K and the magnetic hysteresis measurement was carried out to study the magnetic properties of nanocomposites.     

压力对纳米CoFe2O4/SiO2复合材料结构的影响

 采用溶胶-凝胶工艺和高温高压实验技术,制备了纳米CoFe₂O₄/SiO₂复合材料。利用X射线衍射仪、扫描电子显微镜和振动样品磁强计,对样品的结构、微观形貌和磁性进行了研究,并对CoFe₂O₄中阳离子的占位情况进行了讨论。结果表明,随着处理压力的升高,样品的晶粒尺寸增大,晶格常数减小,比饱和磁化强度增大。通过计算结果可以推断,压力的升高导致CoFe₂O₄中的部分Fe³⁺从A位移向了B位,而部分Co²⁺则从B位移向了A位。     

Optical and electronic properties of NiFe2O4 and CoFe2O4 thin films

We report the optical and electronic properties of the inverse spinel ferrite NiFe₂O₄ and CoFe₂O₄ thin films deposited on single crystal sapphire by electron beam deposition. We carried out variable temperature (78–500 K) transmittance measurements on the thin films to investigate the optical properties and electronic structures of these ferrites. The absorption spectra of both NiFe₂O₄ and CoFe₂O₄ thin films show insulating characters with Ni (Co) d to d on-site transitions below 3 eV. The energy bands above 3 eV are mainly due to the O 2p to Fe 3d charge transfer transitions. The observed electronic transitions have been assigned based on the first principles calculations and comparisons with structurally similar Ni and Co-containing compounds. The Co²⁺ d to d transition in the CoFe₂O₄ thin film shows a strong temperature dependence, likely due to the spin-charge coupling effect.     

Reduced dielectric loss and leakage current in CaCu3Ti4O12/SiO2/CaCu3Ti4O12 multilayered films

The CaCu₃Ti₄O₁₂/SiO₂/CaCu₃Ti₄O₁₂ (CCTO/SiO₂/CCTO) multilayered films were prepared on Pt/Ti/SiO₂/Si substrates by pulsed laser deposition method. It has been demonstrated that the dielectric loss and the leakage current density were significantly reduced with the increase of the SiO₂ layer thickness, accompanied with a decrease of the dielectric constant. The CCTO film with a 20 nm SiO₂ layer showed a dielectric loss of 0.065 at 100 kHz and the leakage current density of 6×10⁻⁷ A/cm² at 100 kV/cm, which were much lower than those of the single layer CCTO films. The improvement of the electric properties is ascribed to two reasons: one is the improved crystallinity; the other is the reduced free carriers in the multilayered films.     

Synthesis and characterization of thermoluminescent glass-ceramics Li2O-Al2O3-SiO2:CeO2

Vitroceramic powders of Li₂O-Al₂O₃-SiO₂ systems (LAS), doped with 1% (LAS:1Ce) and 10% (LAS:10Ce) molar of cerianite (CeO₂) were synthesized by means of the gelification technique of metal formates of aluminum and lithium, in the presence of tetraethoxy silane and CeO₂. The gels obtained were dried (120 °C, 2.5 h), calcined (480 °C, 5 h) and sinterized (1250 °C, 30 min). The sinterized samples were characterized by X-ray difraction (XRD), scanning electron microscopy (SEM) and microchemical analysis (EDS). There is evidence for a mixture of two phases of 64% β-spodumene (Li₂O-Al₂O₃-4SiO₂) and 36% β-eucryptite (Li₂O-Al₂O₃-2SiO₂). The LAS:1Ce system was enriched in aluminum, the LAS:10Ce system showed areas of heterogeneous composition; some regions with a shortage of CeO₂, while others zones with cerium cumulus. From the microscopy images it was found that CeO₂ acts as a densificant agent in LAS system, favoring the sintering in the host. The chemical route and the sintering processes utilized allow the production of samples exhibiting an acceptable linear correlation between total thermoluminescent emission intensity and the irradiation dose when the CeO₂ concentration is low (less than 1%), opening the possibility of using this kind of glass-ceramic in dosimetry.     

Effects of precursor types of Fe and Ni components on the properties of NiFe2O4 powders prepared by spray pyrolysis

The effects of the precursor types of Ni and Fe components on the morphology, mean size, and magnetic property of NiFe₂O₄ powders prepared by spray pyrolysis from the spray solution, with citric acid were studied. The precursor powders with hollow and thin wall structure turned to the nano-sized NiFe₂O₄ powders after post-treatment at a temperature of 800 °C. The nickel ferrite powders obtained from the spray solution with ferric chloride had nanometer sizes and narrow size distributions irrespective of the types of nickel precursor. The nickel ferrite powders obtained from the spray solution with ferric nitrate and nickel chloride also had nanometer size and narrow size distribution. The saturation magnetizations of the NiFe₂O₄ powders changed from 37 to 42 emu/g according to the types of the Fe and Ni precursors. The saturation magnetizations of the NiFe₂O₄ powders increased with increasing the Brunauer-Emmett-Teller (BET) surface areas of the powders.     

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.     

Resistive hysteresis and capacitance effect in NiFe2O4/SrTiO3: Nb(1 wt%) junctions

Epitaxial ultrathin NiFe₂O₄ films were deposited on 1 wt% Nb-doped SrTiO₃ (0 0 1) substrates by reactive cosputtering to form junctions with an area of ∼2 mm², and current-voltage curves show rectifying and asymmetrical hysteresis characteristics. The resistance calculated from the current-voltage curves is strongly voltage dependent, and the hysteretic loops with high and low resistive states were observed. The hysteretic loops are considered to stem from the capacitance effect of the highly resistive NiFe₂O₄ layer, which leads to charge accumulation at the interfaces. The results show that the interfaces of the junctions have a large areal capacitance of ∼100 nF/mm² from 300 to 120 K.     

First-principles study of the electronic and magnetic properties of a Nickel-Zinc ferrite: ZnxNi1−xFe2O4

Using first-principles density functional theory within the generalized gradient approximation method, the effect of Zn doping on electronic and magnetic properties of NiFe₂O₄ ferrite spinel has been studied. The crystal structure of the compounds is assigned to a pseudocubic structure and the lattice constant increases as the Zn concentration increases. Our spin-polarized calculations give a half-metallic state for NiFe₂O₄ and a normal metal state for Zn_xNi_1−xFe₂O₄ (0<x≤0.5). Based on the magnetic properties calculations, it is found that the saturation magnetic moment enhances linearly with increase in the Zn content in NiFe₂O₄. The Zn doping in NiFe₂O₄ also induces strong ferrimagnetism since it decreases the magnetic moment of A-sites.     

Microstructural, dielectric and spectroscopic properties of Li2O-Nb2O5-ZrO2-SiO2 glass system crystallized with V2O5

Li₂O-Nb₂O₅-ZrO₂-SiO₂ glasses mixed with different concentrations of V₂O₅ were crystallized. The samples were characterized by XRD, SEM and DTA techniques. The SEM pictures indicated that the samples contain well defined and randomly distributed crystal grains. The X-ray diffraction studies have revealed the presence of several crystalline phases in these samples. Optical absorption, ESR and photoluminescence spectral studies on these samples have indicated that a considerable proportion of vanadium ions do exist in V⁴⁺ state in addition to V⁵⁺ state and the redox ratio seems to be increasing with increase in the concentration of crystallizing agent V₂O₅. The infrared spectral studies have pointed out the existence of conventional SiO₄, ZrO₄, NbO₆, VO structural units in the glass ceramic network. The study of dielectric properties suggested a decrease in the insulating character of the glass ceramics with increase in the crystallizing agent. A.C. conductivity in the high temperature region seems to be connected mainly with the polarons involved in the process of transfer from V⁴⁺↔V⁵⁺ ions.     

Structural and magnetic properties of NiCuZn ferrite/SiO2 nanocomposites

Ni_0.53Cu_0.12Zn_0.35Fe₂O₄/SiO₂ nanocomposites with different weight percentages of NiCuZn ferrite dispersed in silica matrix were prepared by microwave-hydrothermal method using tetraethylorthosilicate as a precursor of silica, and metal nitrates as precursors of NiCuZn ferrite. The structure and morphology of the composites were studied using X-ray diffraction and scanning electron microscopy. The structural changes in these samples were characterized using Fourier Transform Infrared Spectrometer in the range of 400-1500 cm⁻¹. The bands in the range of 580-880 cm⁻¹ show a slight increase in intensity, which could be ascribed to the enhanced interactions between the NiCuZnFe₂O₄ clusters and silica matrix. The effects of silica content and sintering temperature on the magnetic properties of Ni_0.53Cu_0.12Zn_0.35Fe₂O₄/SiO₂ nanocomposites have been studied using electron spin resonance and vibrating sample magnetometer.     

Fabrication and magnetic properties of Ce1Y2Fe5O12 thin films on GGG and SiO2/Si substrates

Microstructure and magnetic properties of crystalline Ce₁Y₂Fe₅O₁₂ thin films prepared on GGG and on SiO₂/Si substrates by pulsed laser deposition were studied. The results show that highly textured Ce₁Y₂Fe₅O₁₂ film with (4 4 4) preferred orientation prepared on GGG (1 1 1) shows strong paramagnetism superimposed by a weak ferromagnetism. However, polycrystalline Ce₁Y₂Fe₅O₁₂ thin films on SiO₂/Si, which can only be obtained after post-annealing, show strong ferromagnetism with easy axis of magnetization lying in the plane of the film. With post-annealing temperature increasing, CeO₂ segregates from Ce₁Y₂Fe₅O₁₂; then YIG continues to be decomposed, forming Fe₂O₃. Consequently, the saturation magnetization of Ce₁Y₂Fe₅O₁₂ films decreases first and then increases correspondingly, which indicates that the magnetic properties of Ce₁Y₂Fe₅O₁₂ films are mainly related to the microstructure.