Magnetoelectric characterization of xNi0.75Co0.25Fe2O4-(1−x)BiFeO3 nanocomposites

Magnetoelectric (ME) nanocomposites containing Ni_0.75Co_0.25Fe₂O₄-BiFeO₃ phases were prepared by citrate sol-gel process. X-ray diffraction (XRD) analysis showed phase formation of xNi_0.75Co_0.25Fe₂O₄-(1−x)BiFeO₃ (x=0.1, 0.2, 0.3 and 0.4) composites on heating at 700 °C. Transmission electron microscopy revealed the formation of powders of nano order size and the crystal size was found to vary from 30 to 85 nm. Dispersion in dielectric constant (ε) and dielectric loss (tan δ) in the low-frequency range have been observed. It is seen that nanocomposites exhibit strong magnetic properties and a large ME effect. On increasing Ni_0.75Co_0.25Fe₂O₄ contents in the nanocomposites, the saturation magnetization (M_S) and coercivity (H_C) increased after annealing at 700 °C. The large ME output in the nanocomposites exhibits strong dependence on magnetic bias and magnetic field frequency. The large value of ME output can be attributed to small grain size of ferrite phase of nanocomposite being prepared by citrate precursor process.     

Mossbauer, infrared and magnetic susceptibility studies of iron sodium borate glasses doped by sulphur

The affect of sulphur on the structural properties of iron sodium diborate glasses having the composition {(100−x)Na₂B₄O₇+xFe₂O₃}+yS, where x=0.05, 0.15 and 0.25 mol% and Y=0, 2.5 and 5 wt% was studied by infrared, Mossbauer spectroscopy and magnetic susceptibility measurements. It was found that, for samples having 5 mol% Fe₂O₃ and free from sulphur, the iron ions are present in both Fe²⁺ and Fe³⁺ states and also 92% of the total iron enters the glass network as a glass former. The ratio of Fe³⁺/Fe²⁺ increases with increasing the iron content for sulphur-free samples and others containing sulphur. This ratio also decreases with increasing the sulphur content. The magnetic susceptibility was found to decrease with increasing the sulphur content. Also, the increase of Fe₂O₃ content led to a less symmetrical environment of Fe³⁺ ions and vice versa for the Fe²⁺ environment.     

Phase formation, grain growth and magnetic properties of NiCuZn ferrites

We studied the effects of iron-deficient, stoichiometric and iron-excessive compositions on the phase formation, crystal structure, grain growth and magnetic property of NiCuZn ferrites. As the Fe₂O₃ ratio increased from iron-deficiency 47.0 mol% to iron-excess 54.0 mol%, the X-ray diffraction peaks initially shifted towards lower angle and then moved to higher angle. Correspondingly, an initial increase in lattice parameter followed by a subsequent decrease was observed. The lattice parameter showed a maximum 8.396 Å when the Fe₂O₃ ratio was 49.0 mol%. When the system was iron-deficient, ZnO phase was detected in addition to the spinel phase. However, equimolar and iron-excessive compositions exhibited a single spinel phase. As the content of Fe₂O₃ increased, the grain size, density, saturation induction and initial permeability first increased and then decreased. Core losses at 50 kHz and 150 mT, however, changed in the opposite way. Finally, NiCuZn ferrite with an equimolar composition (50.0 mol%) showed the highest initial permeability (1467), highest saturation induction (361 mT) and lowest core losses (234 kW/m³).     

Microwave synthesis of magnetic Fe3O4 nanoparticles used as a precursor of nanocomposites and ferrofluids

Methods to synthesize magnetic Fe₃O₄ nanoparticles and to modify the surface of particles are presented in the present investigation. Fe₃O₄ magnetic nanoparticles were prepared by the co-precipitation of Fe³⁺ and Fe²⁺, NH₃·H₂O was used as the precipitating agent to adjust the pH value, and the aging of Fe₃O₄ magnetic nanoparticles was accelerated by microwave (MW) irradiation. The obtained Fe₃O₄ magnetic nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and vibrating sample magnetometer (VSM). The average size of Fe₃O₄ crystallites was found to be around 8–9 nm. Thereafter, the surface of Fe₃O₄ magnetic nanoparticles was modified by stearic acid. The resultant sample was characterized by FT-IR, scanning electron microscopy (SEM), XRD, lipophilic degree (LD) and sedimentation test. The FT-IR results indicated that a covalent bond was formed by chemical reaction between the hydroxyl groups on the surface of Fe₃O₄ nanoparticles and carboxyl groups of stearic acid, which changed the polarity of Fe₃O₄ nanoparticles. The dispersion of Fe₃O₄ in organic solvent was greatly improved. Effects of reaction time, reaction temperature and concentration of stearic acid on particle surface modification were investigated. In addition, Fe₃O₄/polystyrene (PS) nanocomposite was synthesized by adding surface modified Fe₃O₄ magnetic nanoparticles into styrene monomer, followed by the radical polymerization. The obtained nanocomposite was tested by thermogravimetry (TG), differential scanning calorimetry (DSC) and XRD. Results revealed that the thermal stability of PS was not significantly changed after adding Fe₃O₄ nanoparticles. The Fe₃O₄ magnetic fluid was characterized using UV–vis spectrophotometer, Gouy magnetic balance and laser particle-size analyzer. The testing results showed that the magnetic fluid had excellent stability, and had susceptibility of 4.46×10⁻⁸ and saturated magnetization of 6.56 emu/g. In addition, the mean size d (0.99) of magnetic Fe₃O₄ nanoparticles in the fluid was 36.19 nm.     

Interactions of ferrimagnetic glass/glass-ceramics with bovine serum albumin

Glasses/glass-ceramics with nominal composition 34 SiO₂-(45 − x)CaO-16P₂O₅-4.5MgO-0.5CaF₂ − xFe₂O₃ (where x = 10, 15, 20 wt%) have been prepared by melt quenching technique. These are characterized for structural and micro structural properties by using XRD and Raman spectroscopy. Interaction of glass-ceramics samples with bovine serum albumin (BSA) has been studied using SEM and TOF-SIMS. The formation of magnetite, apatite and wollastonite phases are observed. Typical sizes of crystallites as seen from SEM measurement are 30-50 nm. The progressive addition of iron oxide to glass leads to increase in number of non-bridging oxygen, which in turn affects the response of glass-ceramics when immersed in BSA. The samples with 15 and 20 wt% Fe₂O₃ have shown nearly full surface coverage with BSA, while the sample with 10 wt% Fe₂O₃ shows poor adhesion.     

Study on dielectric and magnetic properties of Ho3Fe5O12 ceramics

Ho₃Fe₅O₁₂ ceramics with garnet structure were prepared by the solid-state reaction method. The results revealed the existence of Fe²⁺ ions have intensive influence on dielectric and magnetic properties of Ho₃Fe₅O₁₂ ceramics, which could be further confirmed by oxygen treatment. With a magnetic field lower than 10 kOe, the ME coefficient reaches 33 ps m⁻¹ at room temperature. And the ME coupling was further verified by dielectric anomaly near Néel temperature.     

Superparamagnetic silica nanoparticles with immobilized metal affinity ligands for protein adsorption

Superparamagnetic silica-coated magnetite (Fe₃O₄) nanoparticles with immobilized metal affinity ligands were prepared for protein adsorption. First, magnetite nanoparticles were synthesized by co-precipitating Fe²⁺ and Fe³⁺ in an ammonia solution. Then silica was coated on the Fe₃O₄ nanoparticles using a sol–gel method to obtain magnetic silica nanoparticles. The condensation product of 3-Glycidoxypropyltrimethoxysilane (GLYMO) and iminodiacetic acid (IDA) was immobilized on them and after charged with Cu²⁺, the magnetic silica nanoparticles with immobilized Cu²⁺ were applied for the adsorption of bovine serum albumin (BSA). Scanning electron micrograph showed that the magnetic silica nanoparticles with an average size of 190 nm were well dispersed without aggregation. X-ray diffraction showed the spinel structure for the magnetite particles coated with silica. Magnetic measurement revealed the magnetic silica nanoparticles were superparamagnetic and the saturation magnetization was about 15.0 emu/g. Protein adsorption results showed that the nanoparticles had high adsorption capacity for BSA (73 mg/g) and low nonspecific adsorption. The regeneration of these nanoparticles was also studied.     

A facile method to synthesize magnetic polymer nanospheres with multifunctional groups

Magnetic poly(styrene methyl methacrylate)/Fe₃O₄ nanospheres with ester groups were prepared by a modified one-step mini-emulsion polymerization in the presence of Fe₃O₄ ferrofluids. The effects of monomer dose, surfactant content, ferrofluid concentration and initiator content on the particle characteristics such as the size, morphology and magnetic properties were investigated by Fourier-transform infrared spectroscopy, transmission electron microscopy, thermogravimetric analysis and vibrating sample magnetometer. The results indicated that magnetic nanospheres were superparamagnetic with high saturation magnetization of 51.0 emu/g and corresponding magnetite content of 61.5 wt%. Subsequently, magnetic nanospheres with carboxyl and amino groups were also obtained by hydrolysis and ammonolysis reaction. These magnetic nanospheres with multifunctional groups have biomedical applications.     

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.     

Study of magnetic properties and magnetoelectric effect in (x) Ni0.5Zn0.5Fe2O4+(1−x)PZT composites

Magnetoelectric (ME) composites consisting of ferrite phase (x) Ni_0.5Zn_0.5Fe₂O₄+ferroelectric phase (1−x)Pb Zr_0.8Ti_0.2O₃ (Lead Zirconate Titanate—PZT) in which x (mol%) varies between 0 and 1 (0.0≤x≤1.0) was synthesized by double sintering ceramic method. The presence of constituent phases of ferrite, ferroelectric and their composites was confirmed by X-ray diffraction studies. The hysteresis measurement was used to study magnetic properties such as saturation magnetization (M_S) and magnetic moment (μ_B). The existence of single domain (SD) particle in the ferrite phase and mixed (SD+MD) particle in the composites was studied from AC susceptibility measurements. ME voltage coefficient for each mol% of ferrite phase was measured as a function of applied DC magnetic field and at the same time influence of magnetic field on ME response and resistivity of composites was studied. The maximum ME voltage coefficient of 0.84 mV/cm Oe was observed for 15% of ferrite phase and 85% of ferroelectric phase in the composites.     

The surface structure of Fe3O4(1 1 1) films as studied by CO adsorption

We have studied adsorption of CO on Fe₃O₄(1 1 1) films grown on a Pt(1 1 1) substrate by temperature programmed desorption (TPD), infrared reflection absorption spectroscopy (IRAS) and high resolution electron energy loss spectroscopy (HREELS). Three adsorption states are observed, from which CO desorbs at ∼110, 180, and 230 K. CO adsorbed in these states exhibits stretching frequencies at ∼2115-2140, 2080 and 2207 cm⁻¹, respectively. The adsorption results are discussed in terms of different structural models previously reported. We suggest that the Fe₃O₄(1 1 1) surface is terminated by 1/2 ML of iron, with an outermost 1/4 ML consisting of octahedral Fe²⁺ cations situated above an 1/4 ML of tetrahedral Fe³⁺ ions, in agreement with previous theoretical calculations. The most strongly bound CO is assigned to adsorption to Fe³⁺ cations present on the step edges.     

Preparation of pyrrole with iron oxide precipitated on the surface of graphite nanosheet

Fe₃O₄/NanoG was firstly prepared by precipitation reaction of iron oxide (Fe₃O₄) on the surface of graphite nanosheet (NanoG). Then composites PPy/NanoG, PPy/Fe₃O₄ and PPy/Fe₃O₄/NanoG were prepared by in-situ polymerization of the monomer pyrrole polymerized on the surface of NanoG, Fe₃O₄ and Fe₃O₄/NanoG. The structures of Fe₃O₄/NanoG, PPy, PPy/NanoG, PPy/Fe₃O₄ and PPy/Fe₃O₄/NanoG were characterized by scanning electron microscopy, energy dispersive spectroscopy, fourier transmission infrared spectroscopy and X-ray diffraction . Results show that NanoG and Fe₃O₄/NanoG are encapsulated by PPy for the layered structure and their high aspect ratio (300–500). From the thermogravimetric analysis it can be seen that the introductions of NanoG, Fe₃O₄ and Fe₃O₄/NanoG into PPy based composites lead them to exhibit better thermal stabilities than pure PPy. The measurements of electromagnetic parameters show that the reflection loss of PPy/Fe₃O₄/NanoG is below −15 dB at the X band (8.2–12.4 GHz) and the minimum loss value is −18.30 dB at 9.84 GHz, while the reflection loss of PPy/Fe₃O₄ is below −10 dB at 8.2–12.4 GHz and the minimum loss value is −14.02 dB at 10.26 GHz. The reflection loss of PPy/NanoG is below −10 dB at 8.2–12.4 GHz and the minimum loss value is −13.44 dB at 10.28 GHz. The microwave absorbing properties of PPy/Fe₃O₄/NanoG, PPy/Fe₃O₄ and PPy/NanoG are superior to that of PPy.     

Synthesis and characterization of a novel magnetic carrier with its composition of Fe3O4/carbon using hydrothermal reaction

In this study, a simple method to prepare a novel magnetic carrier based on carbon matrix has been built by heating the aqueous solution of glucose and oleic acid-stabilized Fe₃O₄ nanoparticle at 170 °C for 3 h. The results show that the surface hydrophobic modification of Fe₃O₄ nanoparticle is necessary for the successful synthesis of Fe₃O₄/C nanocomposition, and a possible formation mechanism of Fe₃O₄/C nanocomposition was presented. The influence of the reaction parameters such as the concentration of oleic acid-stabilized Fe₃O₄ nanoparticle, the reaction time, etc. on the product was also investigated. In the typical reaction (2.5 g/L of oleic acid-stabilized Fe₃O₄ nanoparticle, 0.5 M of glucose), Fe₃O₄/C nanocompositions with the average diameter in the range 100–200 nm were obtained and its saturation is 12.4 emu/g. In order to characterize Fe₃O₄/C nanocompositions, XPS, XRD, FT–IR, and Mössbauer spectra were employed.     

Ionic conductivity and electrochemical stability of poly(methylmethacrylate)-poly(ethylene oxide) blend-ceramic fillers composites

The role of inorganic ceramic fillers namely nanosized Al₂O₃ (15-25 nm) and TiO₂ (10-14 nm) and ferroelectric filler SrBi₄Ti₄O₁₅ (SBT CIT) (0.5 μm) synthesized by citrate gel technique (CIT) on the ionic conductivity and electrochemical properties of polymer blend 15 wt% PMMA+PEO₈:LiClO₄+2 wt% EC/PC electrolytes were investigated. Enhancement in conductivity was obtained with a maximum of 0.72×10⁻⁵ S cm⁻¹ at 21 °C for 2 wt% of SrBi₄Ti₄O₁₅ (SBT CIT) composite polymer electrolyte. The lithium-ion transport number and the electrochemical stability of the composite polymer electrolytes at ambient temperature were analyzed. An enhancement in electrochemical stability was observed for polymer composites containing 2 wt% of SrBi₄Ti₄O₁₅ (SBT CIT) as fillers.     

Study of polydiethylsiloxane-based ferrofluid with excellent frost resistance property

The polydiethylsiloxane-based ferrofluid was prepared by dispersing finely divided magnetic Fe₃O₄ particles which are modified with oleoyl sarcosine and lauroyl sarcosine. The optimized experiment parameters including molar ratio of surfactant to Fe₃O₄ (1:5), temperature (80 °C), stirring rate (300 RPM), the surfactant content of lauroyl sarcosine (0 to 33 mol%) and the modification time (25 min) were obtained by the orthogonal test. The magnetic liquid was characterized by a transmission electron microscope (TEM), infrared (IR) spectrometer, X-ray diffractometer (XRD), thermogravimetry (TG), vibrating sample magnetometer (VSM) and differential scanning calorimetry (DSC). It is indicated that the surfactant is mainly bonded to the surface of Fe₃O₄ nanoparticles through covalent bond between carboxylate (COO⁻) and Fe atom. The modified magnetic particles are equally dispersed into the carrier and remain stable below −12 °C over 4 months. The ferrofluids exhibit excellent frost resistance property and distinctly reduced temperature coefficient of viscosity compared with polydimethylsiloxane-based ferrofluids and hydrocarbon-based ferrofluids, respectively. The saturation magnetization could reach up to 27.7 emu/g.     

Point defects and orientation-dependent transport of matter and charge in iron-containing olivines

The variation of the oxygen content, x_O, of synthetic fayalite (Fe₂SiO₄) single crystals was investigated thermogravimetrically at 1130 °C as a function of the oxygen activity, a_O2 (= P_O2/P_O2° ≈ f_O2/f_O2° with P_O2° ≈ f_O2° = 1 bar ≈ 1 atm). It was found that x_O varies less in fayalite single crystals than in polycrystalline Fe₂SiO₄ studied earlier. The majority defects are most likely cation vacancies, (V_Me²⁺)″, ferric ions on M-sites, (Fe³⁺_Me²⁺), and ferric ions on Si-sites, (Fe³⁺_Si⁴⁺)′. Furthermore, the diffusion of iron in synthetic olivine single crystals ((Fe_xMg_1 − x)₂SiO₄) was studied at 1130 °C as a function of orientation, oxygen activity, and cationic composition. The observed oxygen activity dependencies suggest that cations move via different types of cation vacancies, most likely isolated vacancies, (V_Fe²⁺)″, and possibly neutral associates, {2(Fe³⁺_Me²⁺) ⋅ (V_Me²⁺)^′ ? ′}^x, the latter being minority defects. In addition, the electrical conductivity, σ, of fayalite single crystals was investigated as a function of orientation and oxygen activity within the stability field of fayalite at 1130 °C. The observed oxygen activity dependencies are compatible with (V_Me²⁺)^′ ? ′, (Fe³⁺_Me²⁺), and (Fe³⁺_Si⁴⁺)′ being the majority point defects at high a_O2 and with h^⋅ and e′ as the majority defects at low a_O2. The electrical conduction in fayalite is governed by contributions of electrons and holes. This extended point defect model for fayalite is also compatible with data for the variation of the oxygen content and for the iron tracer diffusion.     

A novel approach to preparing magnetic protein microspheres with core-shell structure

Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe₃O₄ cores and coated with globular bovine serum albumin (BSA). Under an optimized condition, up to 57.8 wt% of approximately 10 nm superparamagnetic Fe₃O₄ nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides of the abundant functional groups. The possible formation mechanism of magnetic microspheres was discussed in detail.     

The colloidal stability and core-shell structure of magnetite nanoparticles coated with alginate

The adsorption of alginate (Alg) onto the surface of in water dispersed Fe₃O₄ nanoparticles and zeta potential of alginate-coated Fe₃O₄ nanoparticles have been investigated to optimize the colloidal stability of Alg-coated Fe₃O₄ nanoparticles. The adsorption amount of Alg increased with the decrease of adsorption pH. The zeta potential of Fe₃O₄ nanoparticles shifted to a lower value after adsorption of Alg. The lower adsorption pH was the lower zeta potential of Fe₃O₄ nanoparticles became. The Alg-coated Fe₃O₄ nanoparticles were found to be stabilized by steric and electrostatic repulsions. Those prepared at pH 6 were not stable around pH 5, and those prepared at pH 4 became unstable at pH below 3.5. Alg of M_w 45 kDa was a little bit more adsorbed onto nanoparticles surface than that of M_w 24 kDa. An average Fe₃O₄ core size of 9.3 ± 1.7 nm was found by transmission electronic microscopy. An average hydrodynamic diameter of 30-150 nm was measured by photon correlation spectroscopy. However, an average core size of 10 nm and an average hydrodynamic diameter of 38 nm were estimated from the magnetization curve of the concentrated magnetic fluids (MFs). The maximum available saturation magnetization of MFs was about 3.5 kA/m.     

Biosynthesis and magnetic properties of mesoporous Fe3O4 composites

Magnetic Fe₃O₄ materials with mesoporous structure are synthesized by co-precipitation method using yeast cells as a template. The X-ray diffraction (XRD) pattern indicates that the as-synthesized mesoporous hybrid Fe₃O₄ is well crystallized. The Barrett-Joyner-Halenda (BJH) models reveal the existence of mesostructure in the dried sample which has a specific surface area of 96.31 m²/g and a pore size distribution of 8-14 nm. Transmission electron microscopy (TEM) measurements confirm the wormhole-like structure of the resulting samples. The composition and chemical bonds of the Fe₃O₄/cells composites are studied by Fourier transform infrared (FT-IR) spectroscopy. Preliminary magnetic properties of the mesoporous hybrid Fe₃O₄ are characterized by a vibrating sample magnetometer (VSM). The magnetic Fe₃O₄/cells composites with mesoporous structure have potential applications in biomedical areas, such as drug delivery.     

Thermal and irradiation induced interdiffusion in magnetite thin films grown on magnesium oxide (0 0 1) substrates

Epitaxial Fe₃O₄(0 0 1) thin films (with a thickness in the range of 10-20 nm) grown on MgO substrates were characterized using low-energy electron diffraction (LEED), conversion electron Mössbauer spectroscopy (CEMS) and investigated using Rutherford backscattering spectrometry (RBS), channeling (RBS-C) experiments and X-ray reflectometry (XRR). The Mg out-diffusion from the MgO substrate into the film was observed for the directly-deposited Fe₃O₄/MgO(0 0 1) films. For the Fe₃O₄/Fe/MgO(0 0 1) films, the Mg diffusion was prevented by the Fe layer and the surface layer is always a pure Fe₃O₄ layer. Annealing and ion beam mixing induced a very large interface zone having a spinel and/or wustite formula in the Fe₃O₄-on-Fe film system.