Polyol synthesis and magnetic study of Mn3O4 nanocrystals of tunable size

Nanosized manganese oxide particles were prepared by the so-called polyol process. The average diameter of the particles was controlled by the growth time. X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photon spectroscopy (XPS) show that the particles are well crystallized, pure, stoichiometric Mn₃O₄ single crystals of uniform size ranging from about 5 to 12 nm. The variation of their dc-magnetization, M, as a function of the magnetic field, H, and temperature, T, clearly corresponds to ferromagnetic ordering at low temperature, with a Curie temperature slightly higher than 40 K. The evidence for superparamagnetism in these particles, due to their very small size, has been discussed in the light of their M(H) and M(T) for zero-field-cooled (ZFC) and field-cooled (FC) plots.     

Structural, microstructural and magnetic properties of NiFe2O4, CoFe2O4 and MnFe2O4 nanoferrite thin films

The structural, microstructural and magnetic properties of nanoferrite NiFe₂O₄ (NF), CoFe₂O₄ (CF) and MnFe₂O₄ (MF) thin films have been studied. The coating solution of these ferrite films was prepared by a chemical synthesis route called sol-gel combined metallo-organic decomposition method. The solution was coated on Si substrate by spin coating and annealed at 700 °C for 3 h. X-ray diffraction pattern has been used to analyze the phase structure and lattice parameters. The scanning electron microscopy (SEM) and atomic force microscopy (AFM) have been used to show the nanostructural behavior of these ferrites. The values of average grain's size from SEM are 44, 60 and 74 nm, and from AFM are 46, 61 and 75 nm, respectively, measured for NF, CF and MF ferrites. At room temperature, the values of saturation magnetization, M_s∼50.60, 33.52 and 5.40 emu/cc, and remanent magnetization, M_r∼14.33, 15.50 and 1.10 emu/cc, respectively, are observed for NF, CF and MF. At low temperature measurements of 10 K, the anisotropy of ferromagnetism is observed in these ferrite films. The superparamagnetic/paramagnetic behavior is also confirmed by χ′(T) curves of AC susceptibility by applying DC magnetizing field of 3 Oe. The temperature dependent magnetization measurements show the magnetic phase transition temperature.     

Fabrication and magnetic properties of Fe3O4 nanowire arrays in different diameters

Fe₃O₄ nanowire arrays with different diameters of D=50, 100, 150 and 200 nm were prepared in anodic aluminum oxide (AAO) templates by an electrodeposition method followed by heat-treating processes. A vibrating sample magnetometer (VSM) and a Quantum Design SQUID MPMS magnetometer were used to investigate the magnetic properties. At room temperature the nanowire arrays change from superparamagnetism to ferromagnetism as the diameter increases from 50 to 200 nm. The zero-field-cooled (ZFC) and field-cooled (FC) magnetization measurements show that the blocking temperature T_B increases with the diameter of nanowire. The ZFC curves of D=50 nm nanowire arrays under different applied fields (H) were measured and a power relationship between T_B and H were found. The temperature dependence of coercivity below T_B was also investigated. Mössbauer spectra and micromagnetic simulation were used to study the micro-magnetic structure of nanowire arrays and the static distribution of magnetic moments of D=200 nm nanowire arrays was investigated. The unique magnetic behaviors were interpreted by the competition of the demagnetization energy of quasi-one-dimensional nanostructures and the magnetocrystalline anisotropy energy of particles in nanowires.     

A study of modified Fe3O4 nanoparticles for the synthesis of ionic ferrofluids

XRD and XPS analyses revealed that a Fe(NO₃)₃·9H₂O layer formed outside γ-Fe₂O₃ particles when Fe₃O₄ nanoparticles were treated with ferric nitrate. The particle density differed for untreated and treated particles and was not uniform for the latter. The specific saturation magnetization of both treated and untreated particles was used to estimate the thickness of the Fe(NO₃)₃·9H₂O layer and the average density of the treated particles. The density of the treated particles was used to calculate the density of ferrofluids of different particle volume fractions. These values are in agreement with measured results. Therefore, the particle volume fraction can be designed to synthesize acid ionic ferrofluids based on Fe₃O₄ nanoparticles using Massart's method.     

Investigating the influence of Cr-Zn substitution on magnetic and structural properties of M-type SrBaSm hexaferrites Sr0.6Ba0.1Sm0.3Fe12.0-x(Cr0.6Zn0.4)xO19

The Cr-Zn substituted M-type SrBaSm hexaferrites Sr_0.6Ba_0.1Sm_0.3Fe_12.0-x(Cr_0.6Zn_0.4)_xO₁₉ (0.00?≤?x?≤?0.75) were synthesized by the conventional ceramic route. The crystal structures were identified by X-ray diffraction. XRD analysis showed that the magnetic powders with CrZn content (x) from 0.00 to 0.30 had M-type as major phase and α-Fe₂O₃ as impurity phase, while the magnetic powders with CrZn content (x)?≥?0.45 exhibited a single M-type phase. The grain morphology of the magnets was observed by a field emission scanning electron microscopy (FE-SEM). The FE-SEM images show that all grains were distributed homogeneously and had regular hexagonal platelet-like shape. The magnetic properties of the magnets were derived from the demagnetizing curves. The remanence (B_r) and maximum energy product [(BH)_max] first increased with increasing CrZn content (x) from 0.00 to 0.30, and then decreased when CrZn content (x)?≥?0.30. The intrinsic coercivity (H_cj) and magnetic induction coercivity (H_cb) first decreased with increasing CrZn content (x) from 0.00 to 0.30, and then slightly fluctuated and basically remained unchanged when CrZn content (x) ≥ 0.30.     

Influence of pH on characteristics of BaFe12O19 powder prepared by sol–gel auto-combustion

BaFe₁₂O₁₉ powders with nanocrystalline sizes were produced by sol–gel auto-combustion. Fe³⁺ and Ba²⁺, in a molar ratio of 11.5, were chelated by citric acid ions at different pH. After dehydration, auto-combustion and calcinations, BaFe₁₂O₁₉ powders were formed. TG/DSC indicated the action to form BaFe₁₂O₁₉ first occurred at about 800. XRD patterns of the annealed powders showed that the well-crystalline powder was produced when pH=10. In addition, the data from XRD showed the lattice parameters a and c, and the unit-cell volume V had a little decrease and the density went up with the increasing pH. The data from PPMS exhibited that pH in the starting solution had an important influence on magnetic properties. In this case, BaFe₁₂O₁₉ powder, of maximum magnetization M(3 T)≈60 A m²/kg, the remanent magnetization M_r≈33 A m²/kg and the intrinsic coercive H_c≈432 kA/m, was produced under the molar ratio of citric acid to the metal nitrate of 1.5 when pH=10.     

Magnetic properties and magneto electric effect in ferroelectric rich Ni0.5Zn0.5Fe2O4+BPZT ME composites

Magneto electric composites with composition (x) Ni_0.5Zn_0.5Fe₂O₄+(1-x) Ba_0.8Pb_0.2Zr_0.8Ti_0.2O₃ (BPZT—barium lead zirconate titanate) in which x varies as 0.0, 0.15, 0.30, 0.45 and 1.0 mol% were prepared by standard double sintering ceramic method. The presence of constituent phases such as ferrite and ferroelectric was confirmed by X-ray diffraction. The structural analyses were carried out by using X-ray diffraction pattern. Scanning electron micrographs (SEM) were taken to understand the microstructure of the samples. The calculated values of the porosity of the samples lie between 4.5% and 16.2%. The hysteresis measurements were made to determine saturation magnetization (M_s), magnetic moment (μ_B) and coercivity (H_c). From the AC susceptibility measurements the contribution of both the single domain (SD) particles of the ferrite phase and mixed domain (SD+MD) particles of the composites in ME output were explained. The static magneto electric voltage coefficients (dE/dH)_H were measured as a function of intensity of magnetic field and the maximum ME coefficient were observed for the composites with 30% of ferrite+70% of ferroelectric phase.     

Enhancement of low-field magnetoresistance in Fe3O4 particles induced by ball milling

A series of Fe₃O₄ particles with different size have been obtained by mechanical ball milling from t=0-450 h. Crystal structure and microstructure of the samples are analyzed by XRD and SEM. An emphasis has been placed on magnetic and transport properties. The experimental results indicate that the sample t=350 exhibits an enhancement of magnetoresistance (MR) comparing with initial powder compress sample (t=0). The low-field magnetoresistance reaches MR=−6.04% at Verwey temperature 120 K and MR=−2.54% at 290 K. Thermal behavior TGA analysis and investigation of magnetic properties have revealed that there is an oxide layer on surface of Fe₃O₄ particles. It is considered that the enhanced magnetoresistance can be taken into account in terms of spin-dependent tunneling effect between Fe₃O₄ particles.Temperature dependence of magnetization and resistivity are measured in order to study electrical and magnetic behavior near Verwey transition. In addition, we also discuss ball milling time dependence of coercivity H_c and specific magnetization M_s of these samples.     

Microwave-assisted synthesis of SrFe12O19 hexaferrites

Ultra-fine and homogeneous SrFe₁₂O₁₉ hexaferrites were synthesized by a microwave-assisted calcination route. The calcined precursors were prepared by a sol-gel auto-combustion method using Fe(NO₃)₃·9H₂O, Sr(NO₃)₂ and citric acid as starting materials. The structures, powder morphology and magnetic properties of the products were characterized by X-ray diffraction, scanning electron microscope and vibrating sample magnetometer. The results showed that microwaves are helpful to reduce the calcination temperature and shorten the calcination time. The ferrites with saturation magnetization, remanence and intrinsic coercivity of 54.80 emu/g, 29.52 emu/g and 5261 Oe, respectively, were obtained in samples calcined at 800 °C for 80 min.     

Synthesis and magnetic properties of Au-coated amorphous Fe20Ni80 nanoparticles

Gold-coated nanoparticles of Fe₂₀Ni₈₀ (permalloy) have been synthesized by a microemulsion process. The as-prepared samples consist of ∼5 nm diameter particles of amorphous Fe₂₀Ni₈₀ that are likely encapsulated in B₂O₃. One or more Fe₂₀Ni₈₀@B₂O₃ particles are subsequently encapsulated in 8-20 nm gold nanospheres, as determined by TEM and X-ray powder diffraction (XRD) line broadening. The gold shells were found to be under expansive strain. Magnetic data confirm the existence of a superparamagnetic phase with a blocking temperature, T_B, of ∼33 K. The saturation magnetization, M_S, of the as-prepared, Au-coated sample is ∼65 emu g⁻¹ at 5 K and ∼16 emu g⁻¹ at 300 K. The coercivity, H_C, is ∼280 Oe at 5 K.     

The properties of acicular particles of (γ-Fe2O3)x(Fe3O4)1-x

It is known that acicular particles, initially of Fe₃O₄, which have been partially oxidised, show anomalous properties e.g. in the variation of H_c with composition. It is shown that these can be explained by considering the particles to comprise an inner core of Fe₃O₄ with an outer layer of γ-Fe₂O₃. Owing to the large change in volume which occurs on oxidation, these mutually stress each other. Over a certain range of composition, the stress field interacts with the magnetization to increase H_c, and it is also responsible for H_c increasing with time after the oxidation process. A similar situation applies to partially reduced γ-Fe₂O₃.     

The magnetic properties of diluted CoFe2O4 nanomaterials

The magnetic properties of （Cox Fe1-x）A （Zn1-x Fe1＋x）B O4 are studied using mean-field theory and the probability distribution law to obtain the saturation magnetization, the coercive field, the critical temperature, and the exchange interactions with different values of D （nm） and x. High-temperature series expansions （HTSEs） combined with the Pade approximant are used to calculate the critical temperature of （CoxFe1-x）A（Znl-xFe1＋x）BO4, and the critical exponent associated with magnetic susceptibility is obtained.     

Study of cerium doped magnetite (Fe3O4:Ce)/PMMA nanocomposites

The paper presents the synthesis and properties of polymer nanocomposite material based on cerium doped magnetite (Fe₃O₄) as filler material and poly methyl methacrylate (PMMA) as host matrix. The magnetite (Fe₃O₄) particles were synthesized by co-precipitation route using stable ferrous and ferric salts with ammonium hydroxide as precipitating agent. Further, they doped by cerium oxide (CeO₂) non-stoichiometrically. The composite material was fabricated by solvent evaporation method. Here 2.4 GHz microwaves were used to study the effect of microwaves heating on polymerization. The phase and crystal structure is determined by X-ray diffraction (XRD). The average crystallite size of the composites varies from 28 to 35 nm. The chemical structure is confirmed by Fourier transform infrared (FTIR) spectroscopy. The magnetic and thermal properties are investigated by vibrating sample magnetometer (VSM) and differential scanning calorimetry (DSC). The thermal study shows that the microwave heated samples possess higher glass transition temperature (T_g). The magnetic results suggest that coercivity (H_C) and squareness (M_r/M_s) of the loop increases with increasing doping percent of cerium.     

Magneto-transport and magnetic properties of (1-x)La0.7Ca0.3MnO3+xAl2O3 composites

We report magneto-transport and magnetic properties of (1-x)La_0.7Ca_0.3MnO₃+xAl₂O₃ composites synthesized through a solid-state reaction method combined with a high energy milling method. Most interestingly, the effective magnetic anisotropy is found to decrease with increase in the non-magnetic insulating Al₂O₃ phase fraction in the composites. In addition, we observed that the magnitude of low-field magnetoresistance arising from spin-polarized tunneling of conduction electrons, as well as that of high-field magnetoresistance, displays a Curie-Weiss law-like behavior. Finally, we found that the temperature dependence of low and high-field magnetoresistance is controlled predominantly by the nature of temperature response of surface magnetization of the particles.     

Structural and magnetic properties of Co1−xZnxFe2O4 nanoparticles by co-precipitation method

Co_1−xZn_xFe₂O₄ nanoparticles were prepared by co-precipitation method with x varying from 0 to 1.0. The powder samples were characterized by X-ray diffraction (XRD), vibrating sample magnetometer (VSM) and Fourier transform infrared spectroscopy (FTIR). The average crystallite sizes of the particles were determined from XRD. X-ray analysis showed that the samples were cubic spinel. The average crystallite size (D_aveXR) of the particles precipitated was found to vary from 6.92 to 12.02 nm decreasing with the increase in zinc substitution. The lattice constant (a_o) increased with the increase in zinc substitution. The specific saturation magnetization (M_S) of the particles was measured at room temperature. The magnetic parameters such as M_S, H_c, and M_r were found to decrease with the increase in zinc substitution. FTIR spectra of the Co_1−xZn_xFe₂O₄ with x varying from 0 to 1.0 in the range 400–4000 cm⁻¹ were reported. The spinel structure and the crystalline water adsorption of Co_1−xZn_xFe₂O₄ nanoparticles were studied by using FTIR.     

Synthesis and characterization of Co3O4 nanorods by thermal decomposition of cobalt oxalate

Cobalt oxalate was used as a precursor to prepare Co₃O₄ nanorods by thermal decomposition. The combinations of triphenylphosphine and oleylamine were added as surfactants to control the morphology of the particles. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The diameters of Co₃O₄ nanorods are 20 nm and the average lengths are around 500 nm. The hysteresis loops of the obtained samples reveal the ferromagnetic behaviors, the enhanced coercivity (H_c) and decreased saturation magnetization (M_s) in contrast to their respective bulk materials. The study provides a simple and efficient route to synthesize Co₃O₄ nanorods at low temperature.     

Exchange interactions and magnetization reversal of nanocrystalline (NdDyTb)12.3(FeZrNbCu)81.7B6.0 ribbons with Co substitution

Alloys of composition Nd_10.8Dy_0.75Tb_0.75Fe_79.7−xCo_xZr_0.8Nb_0.8Cu_0.4B_6.0 (x=0, 3, 6, 9, 12, 15) were prepared by melt spinning at 22 m/s and subsequent annealing. Phase analysis revealed single-phase materials. Magnetic structure and remanence analysis indicated strong exchange coupling between neighboring grains in all samples. The remanence polarization J_r and maximum energy product (BH)_max increased first and then decreased with further increasing Co content x although the intrinsic coercivity H_ci decreased with increasing x. The increase in remanence polarization J_r by the substitution of Co for Fe is mainly caused by the increase in the saturation polarization J_s rather than by the improvement of exchange-coupling interactions. Optimum magnetic properties with J_r=1.041 T, H_ci=944.9 kA/m and (BH)_max=155.1 kJ/m³ were achieved for x=12 ribbons. The mechanism of magnetic hardening in all samples was of pinning type by analyzing initial magnetization and the dependence on applied magnetizing field of the coercivity and remanence.     

Synthesis and characterization of Ni1−xCoxFe2O4 nanoparticles

Ni_1−xCo_xFe₂O₄ (x=0.6, 0.8 and 0.9) nanoparticles have been synthesized with various crystallite sizes depending on the thermal treatments and composition (cobalt content) using the sol-gel combustion method. The size of nanoparticles has been controlled by thermal treatment. On the other hand, the magnetic property of the ferrite has been controlled by changing the heat treatment. Morphology and particle sizes of Ni_1−xCo_xFe₂O₄ have been studied using atomic force microscopy (AFM) and transmission electron microscopy (TEM). The presence of functional group has been identified by Fourier Transform Infrared (FTIR) spectra. From TGA-DTA studies, the weight gains of Ni_1−xCo_xFe₂O₄ nanoparticles have been observed and it might be due to capping organic molecules with oxygen at temperatures above 200 °C. Magnetic properties of Ni_1−xCo_xFe₂O₄ particles have been analysed using VSM and it is found that saturation magnetization (M_s) has increased with particle size and has coercivity (H_c) increased initially and then decreased. The M_s and H_c values decreased with the increase of content of cobalt in Ni_1−xCo_xFe₂O₄.     

Synthesis and ion conductivity of (Bi2O3)0.75(Dy2O3)0.25 ceramics with grain sizes from the nano to the micro scale

Using (Bi₂O₃)_0.75(Dy₂O₃)_0.25 nano-powder synthesized by reverse titration co-precipitation method as raw material, dense ceramics were sintered by both Spark Plasma Sintering (SPS) and pressureless sintering. According to the predominance area diagram of Bi-O binary system, the sintering conditions under SPS were optimized. (Bi₂O₃)_0.75(Dy₂O₃)_0.25 ceramics with relative density higher than 95% and an average grain size of 20 nm were sintered in only 10 min up to 500 °C. During the pressureless sintering process, the grain growth behavior of (Bi₂O₃)_0.75(Dy₂O₃)_0.25 followed a parabolic trend, expressed as D² − D₀² = Kt, and the apparent activation energy of grain growth was found to be 284 kJ mol^− 1. Dense (Bi₂O₃)_0.75(Dy₂O₃)_0.25 ceramics with different grain sizes were obtained, and the effect of grain size on ion conductivity was investigated by impedance spectroscopy. It was shown that the total ion conductivity was not affected by the grain size down to 100 nm, however lower conductivity was measured for the sample with the smallest grain size (20 nm). But, although only the δ phase was evidenced by X-ray diffraction for this sample, a closer inspection by Raman spectroscopy revealed traces of α-Bi₂O₃.     

Synthesis and characterization of room-temperature ferromagnetism in Fe- and Ni-co-doped In2O3

Observation of room-temperature ferromagnetism in Fe- and Ni-co-doped In₂O₃ samples (In_0.9Fe_0.1−xNi_x)₂O₃ (0?x?0.1) prepared by citric acid sol-gel auto-igniting method is reported. All of the samples with intermediate x values are ferromagnetic at room-temperature. The highest saturation magnetization (0.453 μ_B/Fe+Ni ions) moment is reached in the sample with x=0.04. The highest solubility of Fe and Ni ions in the In₂O₃ lattice is around 10 and 4 at%, respectively. The 10 at% Fe-doped sample is found to be weakly ferromagnetic, while the 10 at% Ni-doped sample is paramagnetic. Extensive structure including Extended X-ray absorption fine structure (EXAFS), magnetic and magneto-transport including Hall effects studies on the samples indicate the observed ferromagnetism is intrinsic rather than from the secondary impurity phases.