One-pot low temperature synthesis of MFe2O4 (M=Co,Ni, Zn) superparamagnetic nanocrystals

Magnetic MFe₂O₄ (M=Co, Ni, Zn) nanocrystals with a diameter about 30 nm and a nearly spherical shape were synthesized via a simple hydrothermal approach. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy have been used to investigate the as-prepared magnetic MFe₂O₄ (M=Co, Ni, Zn) nanocrystals. Magnetic properties of the as-prepared samples have been detected by a vibrating sample magnetometer at room temperature and the results show that the as-prepared magnetic MFe₂O₄ nanocrystals are a type characteristic of superparamagnetic materials. These superparamagnetic nanocrystals are believed to be promising for wide engineering applications, such as drug delivery, bioseparation, and magnetic resonance imaging.     

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.     

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.     

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.     

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.     

Synthesis,characterization and magnetic properties of MFe2O4 (M=Co,Mg, Mn,Ni) nanoparticles using ricin oil as capping agent

We focused on obtaining MFe₂O₄ nanoparticles using ricin oil solution as surfactant and on their structural characterization and magnetic properties. The annealed samples at 500 °C in air for 6 h were analyzed for the crystal phase identification by powder X-ray diffraction using CuKα radiation. The particle size, the chemical composition and the morphology of the calcinated powders were characterized by scanning electron microscopy. All sintered samples contain only one phase, which has a cubic structure with crystallite sizes of 12–21 nm. From the infrared spectra of all samples were observed two strong bands around 600 and 400 cm⁻¹, which correspond to the intrinsic lattice vibrations of octahedral and tetrahedral sites of the spinel structure, respectively, and characteristic vibration for capping agent. The magnetic properties of fine powders were investigated at room temperature by using a vibrating sample magnetometer. The room temperature M–H hysteresis loops show ferromagnetic behavior of the calcined samples, with specific saturation magnetization (M_s) values ranging between 11 and 53 emu/g.     

单相Bi0.9Ba0.1Fe0.85Mn0.15O3陶瓷中的多铁性

溶胶-凝胶法制备了Bi_0.9Ba_0.1Fe_0.85Mn_0.15O₃陶瓷样品,XRD分析显示其为单相菱方钙钛矿结构,明显的磁滞回线和电滞回线说明其在室温具有弱铁磁性和铁电性,介电常数随外磁场的变化显示双掺样品具有更大的磁容效应. 关键词： 溶胶-凝胶法 多铁材料 磁容效应     

Exchange coupling behavior in bimagnetic CoFe2O4/CoFe2 nanocomposite

In this work we report a study of the magnetic behavior of ferrimagnetic oxide CoFe₂O₄ and ferrimagnetic oxide/ferromagnetic metal CoFe₂O₄/CoFe₂ nanocomposite. The latter compound is a good system to study hard ferrimagnet/soft ferromagnet exchange coupled. Two steps were followed to synthesize the bimagnetic CoFe₂O₄/CoFe₂ nanocomposite: (i) first, preparation of CoFe₂O₄ nanoparticles using a simple hydrothermal method, and (ii) second, reduction reaction of cobalt ferrite nanoparticles using activated charcoal in inert atmosphere and high temperature. The phase structures, particle sizes, morphology, and magnetic properties of CoFe₂O₄ nanoparticles were investigated by X-Ray diffraction (XRD), Mossbauer spectroscopy (MS), transmission electron microscopy (TEM), and vibrating sample magnetometer (VSM) with applied field up to 3.0 kOe at room temperature and 50 K. The mean diameter of CoFe₂O₄ particles is about 16 nm. Mossbauer spectra revealed two sites for Fe³⁺. One site is related to Fe in an octahedral coordination and the other one to the Fe³⁺ in a tetrahedral coordination, as expected for a spinel crystal structure of CoFe₂O₄. TEM measurements of nanocomposite showed the formation of a thin shell of CoFe₂ on the cobalt ferrite and indicate that the nanoparticles increase to about 100 nm. The magnetization of the nanocomposite showed a hysteresis loop that is characteristic of exchange coupled systems. A maximum energy product (BH)_max of 1.22 MGOe was achieved at room temperature for CoFe₂O₄/CoFe₂ nanocomposites, which is about 115% higher than the value obtained for CoFe₂O₄ precursor. The exchange coupling interaction and the enhancement of product (BH)_max in nanocomposite CoFe₂O₄/CoFe₂ are discussed.     

Enhanced magnetization in Co and Ta-substituted BiFeO3 ceramics

Cobalt (Co) and tantalum (Ta) co-substituted BiFeO₃ polycrystalline ceramics were prepared by a solid-state reaction and their magnetic and dielectric properties were investigated. Magnetic hysteresis loops were clearly observed in co-substituted specimens and magnetization was greatly improved. The co-substitution decreased the electrical conductivity by six orders of magnitude along with the reduction of grain size. The magnetoelectric coupling was estimated in co-substituted BiFeO₃ by determining the changes of the dielectric constant with an external magnetic field.     

Synthesis and magnetic properties of hard magnetic (CoFe2O4)-soft magnetic (Fe3O4) nano-composite ceramics by SPS technology

CoFe₂O₄/Fe₃O₄ nano-composite ceramics were synthesized by Spark Plasma Sintering. The X-ray diffraction patterns show that all samples are composed of CoFe₂O₄ and Fe₃O₄ phases when the sintering temperature is below 900 °C. It is found that the magnetic properties strongly depend on the sintering temperature. The two-step hysteresis loops for samples sintered below 500 °C are observed, but when sintering temperature reaches 500 °C, the step disappears, which indicates that the CoFe₂O₄ and Fe₃O₄ are well exchange coupled. As the sintering temperature increases from 500 to 800 °C, the results of X-ray diffractometer indicate the constriction of crystalline regions due to the ion diffusion at the interfaces of CoFe₂O₄/Fe₃O₄ phases, which have great impact on the magnetic properties.     

The effect of B2O3 addition to the microstructure and magnetic properties of Ni0.4Zn0.6Fe2O4 ferrite

The effects of 0.01 and 0.1 mol B₂O₃ addition to the microstructure and magnetic properties of a Ni–Zn ferrite composition expressed by a molecular formula of Ni_0.4Zn_0.6Fe₂O₄ were investigated. The toroid-shaped samples prepared by pressing the milled raw materials used in the preparation of the composition were sintered in the range of 1000–1300 °C. The addition of 0.01 mol B₂O₃ increased the grain growth and densification giving rise to reduced intergranular and intragranular porosity due to liquid-phase sintering. The sintered toroid sample at 1300 °C gave the optimum magnetic properties of B_r=170 mT, H_c=0.025 kA/m and a high initial permeability value of μ_i=4000. The increment of the B₂O₃ content to 0.1 mol resulted in a pronounced grain growth and also gave rise to large porosity due to the evaporation of B₂O₃ at higher sintering temperatures. Hence, it resulted in an air-gap effect in the hysteresis curves of these samples.     

Preparation and characterization of polyaniline (PANI)-Mn3O4 nanocomposite

Polyaniline (PANI)-Mn₃O₄ nanocomposite was synthesized by a combination of sonochemical synthesis of Mn₃O₄ NP's and in-situ polymerization of aniline. Structural characteristics were evaluated by XRD, FT-IR, TGA, VSM, TEM and SEM analysis, and conduction characteristics were evaluated by total conductivity measurements in the temperature range of 20-100 °C and frequency range of 0.1 Hz-1 MHz. Our findings show that PANI is successfully coated on nanoparticles surface and overall conductivity of nanocomposite is approximately 50-1000 times higher than that of uncapped Mn₃O₄ or PANI base with increase in temperature. Morphology of the synthesized powder was observed to be thin nanosheets with a thickness of 2-3 nm based on SEM analysis. Room temperature magnetization curves for nanocomposite show no hysteresis, indicating the super-paramagnetic character of the sample in the region of measured field strength. σ_AC increased after polyaniline coating.     

Sol–gel derived nanocrystalline multiferroic BiFeO3 and R (R=Er and Tm) doped therein: Magnetic phase transitions and enhancement of magnetic properties

Nanocrystalline BiFeO₃ and rare earth ion doped BiFeO₃ (Bi_0.9R_0.1FeO₃, R=Er and Tm) were prepared by sol–gel method. Rietveld analysis of the X-ray diffractograms of the samples revealed that small amount of impurity phase of Bi₂Fe₄O₉ was formed together with the desired phase. In the thermal variation of magnetic mass susceptibility (χ_m) of the samples, one sharp transition below T_M (T_M∼100 K, 50 K and 30 K for BiFeO₃, Bi_0.9Er_0.1FeO₃ and Bi_0.9Tm_0.1FeO₃, respectively) was observed, which clearly hint the change of the domination of the ferromagnetic exchange interaction over the usual antiferromagnetic exchange interaction. Also, static magnetization (M) and susceptibility of each doped sample have been drastically enhanced compared to that of BiFeO₃. The values of χ_m and M measured at different temperatures confirmed that the magnetic behavior of the doped systems has been dominated by the paramagnetic/ferromagnetic clusters below ∼T_M. Another phase transition were observed in the χ_m vs. T curve of the samples at relatively higher temperature T_B (∼260 K for BiFeO₃, ∼220 K for Bi_0.9Er_0.1FeO₃ and ∼180 K for Bi_0.9Tm_0.1FeO₃), which may be attributed to the charge ordering transition. Ferroelectric hysteresis loops of the samples observed at 100 Hz confirmed the presence of ferroelectric ordering of the samples. Measured values of dielectric constants at 1 kHz of each sample in presence and absence of magnetic field confirmed a substantial magnetoelectric coupling of all the samples.     

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.     

Effect of magnetic annealing on magnetization of BiFeO3 ceramics

The effect of magnetic annealing treatment on the magnetization of multiferroic BiFeO₃ was studied systematically. A series of pelletized nano-sized BiFeO₃ powders were annealed at high temperature under different magnetic fields. Typical ferromagnetic hysteresis loops were obtained at room temperature of the ceramics which were derived from ferromagnetic BiFeO₃ precursors. On the other hand, antiferromagnetic behaviors were observed in other samples synthesized from nonmagnetic precursors. The enhanced magnetic properties were ascribed to the magnetic anisotropy which was induced by the strong magnetic fields. This work indicates that the strong magnetic annealing method is an alternative approach to tuning the magnetic properties of high performance multiferroic materials with canted antiferromagnetic ordering.     

Ion dependence of magnetic anisotropy in MFe2O4 (MFe,Co, Mn) nanoparticles synthesized by high-temperature reaction

The influence of different M²⁺ cations on the effective magnetic anisotropy of systems composed of MFe₂O₄ (M=Fe, Co and Mn) nanoparticles was investigated. Samples were prepared by the high-temperature (538 K) solution phase reaction of Fe (acac)₃, Co (acac)₂ and Mn (acac)₂ with 1,2 octanodiol in the presence of oleic acid and oleylamine. The final particles are coated by an organic layer of oleic acid that prevents agglomeration. Transmission electron microscopy (TEM) images show that particles present near spherical form and a narrow grain size distribution, with mean diameters in the range of 4.5–7.6 nm. Powder samples were analyzed by ac susceptibility and Mössbauer measurements, and K_eff for all samples was evaluated using both techniques, showing a strong dependence on the nature of the divalent cation.     

Sol-gel derived nanoparticles of Zn substituted lithium ferrite (Li0.32Zn0.36Fe2.32O4): magnetic and Mössbauer effect measurements and their theoretical analysis

Nanoparticles of Zn substituted lithium ferrite (Li_0.32Zn_0.36Fe_2.32O₄) have been prepared by a sol-gel method where the ultra-sonication technique has been adopted to reduce the agglomeration effect among the nanoparticles. The samples were heat-treated at three different temperatures and the formation of the nanocrystalline phase was confirmed by X-ray diffractograms (XRD). The average particle size of each sample has been estimated from the (311) peak of the XRD pattern using the Debye-Scherrer formula and the average sizes are in the range of 10-21 nm. The average particle size, crystallographic phase, etc. of some selected samples obtained from the high-resolution transmission electron microscopy are in agreement with those estimated from the XRD patterns. Static magnetic measurements viz., hysteresis loops, field cooled and zero field cooled magnetization versus temperature curves of some samples carried out by SQUID in the temperature range of 300 to 5 K clearly indicate the presence of superparamagnetic (SPM) relaxation of the nanoparticles in the samples. The maximum magnetization of the SPM sample annealed at 500 °C is quite high (68 Am²/Kg) and the hysteresis loops are almost square shaped with very low value of coercive field at room temperature (827.8 A/m). The particle size, magneto-crystalline anisotropy, etc. have been estimated from the detailed theoretical analysis of the static magnetic data. The dynamic magnetic behavior of the samples was also investigated by observing the ac hysteresis loops and magnetization versus field curves with different time windows at room temperatures. The different soft magnetic quantities viz., coercive field, magnetization, remanance, hysteresis losses, etc. were extracted from dynamic measurements. Dynamic measurements confirmed that the samples are in their mixed state of SPM and ordered ferrimagnetic particles, which is in good agreement with the results of static magnetic measurements. Mössbauer spectra of the samples recorded at room temperature (300 K) and at different temperatures down to 20 K confirmed the presence of the SPM relaxation of the nanoparticles of the samples.     

Reflux synthesis of Co3O4 nanoparticles and its magnetic characterization

Co₃O₄ nanoparticles have been prepared for the first time via reflux method, as an alternative low-temperature high-yield process, starting from one single precursor. A plausible mechanism is suggested for the synthetic process. XRD, TEM, FTIR and VSM were used for the structural, morphological, spectroscopic, and magnetic characterization of the product respectively. X-ray diffraction line profile fitting showed that average particle size of the sample is 28 nm. Morphology of the synthesized powder was observed to be thin nanosheets with a thickness of 2-3 nm based on SEM and TEM analyses. Magnetic measurements showed a deviation of the Neel temperature from the bulk value which is attributed to the finite size effects. A loop shift with an enhanced coercivity is observed in the field-cooled hysteresis loops. The opening of the hysteresis loop reveals the existence of the spin-glass like surface spins of the Co₃O₄ nanoparticles.     

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.     

Nd28Fe66B6/Fe50Co50双层纳米复合膜的结构和磁性

利用磁控溅射法制备了Nd₂₈Fe₆₆B₆/Fe_{50Co50 双层纳米复合磁性薄膜，研究了其结构和磁性.经873K退火处理15min 后，利用x射线衍射仪测定薄膜晶体结构，采用俄歇电子能谱仪估算薄膜厚度和超导量子干 涉仪测量其磁性.磁性测量表明，1)该系列薄膜具有垂直于膜面的磁各向异性.从起始磁化曲 线和小回线的形状特征可知，矫顽力机制主要是由畴壁钉扎控制.2)对于固定厚度（10nm） 层的硬磁相Nd-Fe-B和不同厚度（dFeCo=1—100nm）层软磁相FeCo双层纳米复合 膜,剩磁随软磁相FeCo 厚度的增加快速增加，而矫顽力则减少.当dFeCo=5nm 时 ，最大磁能积达到160×１０^３A/m.磁滞回线的单一硬磁相特征说明，硬磁相Nd -Fe-B层和软磁相FeCo层之间的相互作用使两相很好地耦合在一起.剩磁和磁能积的提高是由 于两相磁性交换耦合所致. 关键词： Nd-Fe-B/FeCo双层纳米复合膜 交换耦合 磁性增强}