Spin-canting and transverse relaxation in maghemite nanoparticles and in tin-doped maghemite

The magnetic properties of maghemite nanoparticles and tin-doped maghemite have been studied by ⁵⁷Fe and ¹¹⁹Sn Mössbauer spectroscopy at temperatures from 6 to 300 K with and without applied magnetic fields. The low-temperature ⁵⁷Fe spectra of both samples, obtained in a field of 4 T, can be described in terms of A-site and B-site components with perfect ferrimagnetic order and a strongly canted component, which seems to have its main contribution from B-site ions. At higher temperatures, the components with strong canting are influenced by transverse relaxation, which results in significant line broadening, a reduction of the magnetic hyperfine splitting and a reduction in the relative areas of lines 2 and 5. The ¹¹⁹Sn spectra show a very broad distribution of magnetic hyperfine fields at low temperatures. When the sample was exposed to applied magnetic fields the distribution became narrower. The spectra show that the direction of the hyperfine field of a large fraction of the tin ions in maghemite is antiparallel to the applied field, but a minor fraction of the tin ions have canted hyperfine fields.     

Synthesis and magnetic properties of platelet γ-Fe2O3 particles for medical applications using hysteresis-loss heating

Platelet γ-Fe₂O₃ particles of particle size less than 100 nm were prepared for medical applications that use the hysteresis-loss heating of ferromagnetic particles. The γ-Fe₂O₃ particles were obtained through the dehydration, reduction, and oxidation of platelet α-FeOOH particles, which were synthesized by the precipitation of ferric ions in an alkaline solution containing ethanolamine, and the crystals grown using a hydrothermal treatment. The γ-Fe₂O₃ particles contained dimples formed by the dehydration of α-FeOOH particles. The coercive force and the saturation magnetization of the γ-Fe₂O₃ particles were in the ranges 11.9 to 12.7 kA/m (150 to 160 Oe), and 70 to 72 Am²/kg (70 to 72 emu/g), respectively. The specific loss power of the γ-Fe₂O₃ particles, estimated from their temperature-raising property measured under a peak magnetic field of 50.9 kA/m (640 Oe) and at a frequency of 117 kHz, was 590 W/g. This value is higher than that of spherical cobalt-containing iron oxide particles having equivalent coercive force and saturation magnetization, reflecting the larger area of the minor hysteresis loop measured under a peak magnetic field of 50.9 kA/m (640 Oe).     

Synthesis of magnetite nanoparticles for AC magnetic heating

Magnetite particles with different average diameter (D_m) suitable for magnetic fluid hyperthermia (MFH) were synthesized by controlled coprecipitation technique. In this method, the reaction pH was stabilized using the pH buffer and the average particle diameter decreased with increasing reaction pH. The size-dependent magnetic behavior of the magnetite nanoparticles was studied and the optimum size range required for magnetic fluid hyperthermia (MFH) has been arrived at. Among the samples studied, the maximum specific absorption rate of 15.7 W/g was recorded for the magnetite sample with D_m of 13 nm, when exposed to an AC magnetic field strength of 3.2 kA/m and a frequency of 600 kHz. The AC magnetic properties suggested that the size distribution of the sample was bimodal with average particle size less than ∼13 nm.     

Enhancement of AC-losses of magnetic nanoparticles for heating applications

Aqueous ferrofluids of maghemite nanoparticles coated with carboxydextran were investigated with respect to their specific loss power (SLP) in dependence on frequency and field amplitude of magnetic AC-fields. In order to elucidate the effect of the size distribution on SLP fluid fractions with different mean particle core size were prepared by a magnetic separation procedure from the original ferrofluid. Structural characterisation by means of TEM and XRD as well as reconstruction of core size distributions from magnetisation curves reveals that the narrow size distributions of the fractions cover a range of mean core sizes from about 8 up to 20 nm. Spectra of the complex susceptibility were measured for a frequency range of 20 Hz to 1 MHz. From the imaginary part of the susceptibility the specific loss power is calculated in dependence on frequency. The results are compared with calorimetrical measurements performed in dependence on field amplitude up to 11 kA/m at 410 kHz. A very high specific loss power in the order of 400 W per gram maghemite was found at 410 kHz and 11 kA/m for the fluid fraction having the largest mean core diameter. A deviation from linear response behaviour is found for this sample showing a power law field dependence of the specific loss power SLPH^2.5. In addition to liquid suspensions measurements were performed with particles immobilised in mannitol or gel in order to elucidate the role of Brownian relaxation. The experimentally found dependence of SLP on the mean particle core diameter may be understood in the frame of the Debye dispersion model. Results are discussed with respect to applications of ferrofluids in RF-magnetic hyperthermia.     

Magnetic and transport properties of Cu2MnAl Heusler alloy prepared by rapidly quenched method

The Cu₂MnAl alloy was prepared by rapidly quenched (suction-casting and melt-spinning) methods with various thicknesses of 20, 40 and 1000 μm. The X-ray diffraction (XRD) patterns of the fabricated samples show a single phase of Cu₂MnAl. All the samples reveal soft magnetic behavior with coercivity below 1.6 kA/m and Curie temperature of about 600 K. Resistance of the alloy behaves as a linear function of applied magnetic field. Magnetoresistance (MR) ratio depends on the thickness of the samples and achieves ∼0.8% at the field of 240 kA/m for the sample with thickness of 20 μm. The variation of the properties of the alloy can be interpreted by the difference of energy band structure caused by defects in the alloy.     

Side-hole to anti-hole conversion in time-resolved spectral hole burning of ruby: Long-lived spectral holes due to ground state level population storage

We report time-resolved transient spectral hole burning of Verneuil-grown 20 ppm and ca. 0.6 ppm ruby (Al₂O₃:Cr³⁺) in zero field and low magnetic fields B∥c at 4 K. The hole-burning spectroscopy of the 20 ppm sample implies relatively rapid cross relaxation in the ⁴A₂ ground state on the ∼1 ms timescale both in zero field and in low magnetic fields, B∥c, up to 0.2 T. In the 0.6 ppm sample, side-hole to anti-hole conversion is observed both in zero field and in low magnetic fields. This conversion is caused by population storage in ⁴A₂ ground state levels. Spin-lattice relaxation, on the 200 ms timescale, is directly observed from the time dependence of the resonant hole and anti holes in B∥c, consistent with a very low cross-relaxation rate. However, in zero field cross relaxation in the ⁴A₂ ground state is still a significant relaxation mechanism for the 0.6 ppm sample resulting in hole decay in ∼50 ms.     

The effect of magnetic field heat treatment on magnetostriction of Terfenol-D 2-2 composites

Based on the analysis of the magnetostriction for Terfenol-D composites, Terfenol-D 2-2 magnetostrictive composites have been prepared with laminations perpendicular to [1 1 2] axes. Then one of the samples was annealed in the vacuum at 423 K for 15 min at the magnetic field of 240 kA/m, which is along the direction of laminations and vertical to the [1 1 2] axes of the specimen. The static magnetostriction λ and dynamic magnetostrictive coefficient d₃₃ of samples were measured under the compressive stress of 0, 2, 4, 6 and 8 MPa. Effects of the compressive stress and the magnetic field heat treatment on the magnetostriction λ have been investigated. It is found that the magnetostriction of 2-2 composites can be improved under the compressive stress when the magnetic field is larger than 20 kA/m. The magnetostriction of 2-2 composites with the magnetic field heat treatment increases under compressive stress, and it can reach 1390×10⁻⁶ at the magnetic field of 200 kA/m and under the compressive stress of 4 MPa, much larger than the value of 860×10⁻⁶ without the magnetic field heat treatment. The highest magnetostriction of the 2-2 composite with the magnetic field heat treatment can reach 1530×10⁻⁶. The dynamic magnetostrictive coefficient d₃₃ of 2-2 composites with the magnetic field heat treatment have been improved, compared with that without magnetic field heat treatment. The maximum value of d₃₃ of the sample with magnetic field heat treatment is 71% larger than that without magnetic field heat treatment.     

On the time evolution of transmittivity in magnetic fluids

When a magnetic fluid is subjected to a magnetic field, a part of the magnetic particles in the fluid agglomerates to form chains. Thus, the ferrofluid becomes optically anisotropic. In this work we describe optically observed patterns in some magnetic fluid films in applied parallel magnetic fields and optical effects of these, especially the optical transmittance. The most interesting experimental observation is that concerning the time dependence of relative transmittivity . For kerosene base ferrofluids relax rapidly at coupling and decoupling magnetic field, but for a transformer-oil magnetic fluid the relaxation times can attain (5–10) minutes, depending on the intensity of applied magnetic field.     

FMR studies in the TbFeCo/GdFeCoSi bilayers

Bilayers, TbFeCo/GdFeCoSi, made by sputtering on glass substrate with buffer and capping layers were studied by measuring the hysteresis loop and by ferromagnetic resonance (FMR). When the field H was applied along the film normal, a double H_C hysteresis loop related to the two sublayers was observed. In ferromagnetic resonance measurements, a peculiar out-of-plane angular dependence of FMR spectrum was obtained. When scanning field H was 0-637 kA/m less than the anisotropy field of TbFeCo sublayer, two FMR peaks were observed. One peak was characteristic of uniaxial and unidirectional anisotropy. The anisotropy constants were obtained by fitting the data with the theory of FMR, and this peak was considered to be related to the low anisotropy GdFeCoSi layer. The second peak appeared only when the dc field H was orientated in a limited angular range around 180°. This peak was considered to be related to an uncoupled interfacial GdFeCoSi sublayer near Al capping layer. However, when H was scanned between 0-1114 kA/m, only one peak is observed due to magnetization reversal of TbFeCo layer with uniaxial anisotropy.     

Cantilevered actuator using magnetostrictive thin film

This paper describes a cantilevered magnetic actuator driven by magnetostriction in a low magnetic field. The dimensions of the two layers actuator were 1×5 mm and amorphous FeSiB was used as the magnetostrictive material. Since the FeSiB has excellent soft magnetic characteristics, the actuator with FeSiB was able to work in magnetic field strength of less than 10 kA/m. The theoretical formulas for the amount of the displacement and the force of the actuator were obtained. The theoretical results agreed with the experimental one. According to the theoretical formula, the displacement was calculated with the parameter of the mechanical properties of the substrate. To obtain the large displacement, the actuator with Co substrate was designed based on the theoretical formula. The displacement of 153 μm was obtained using Cu substrate of 1.1 μm thickness in the magnetic field of 10 kA/m. © 2008 Elsevier B.V. All rights reserved     

Dependence of magnetic characteristics on sputtering-power and substrate-temperature in amorphous Tb40(FeCoV)60 films

The amorphous Tb₄₀(Fe₄₉Co₄₉V₂)₆₀ films were deposited at different sputtering powers and substrate temperatures. The microstructural and magnetic characteristics were investigated by means of field emission scan electron microscope, magnetic force microscope and vibrating sample magnetometer. Our results show that with increasing sputtering power, out-of-plane coercivity decreases monotonically while saturation magnetization has a maximum value of 231 kA/m for the sample prepared at 50 W. The as-deposited alloy films are amorphous, whereas the coercivity and saturation magnetization are strongly dependent on the substrate temperature. An out-of-plane hysteresis loop with coercivity below 22 mT and saturation magnetization over 290 kA/m is obtained combining dc power and substrate temperature. The dominant mechanism of room temperature coercivity appears to be domain wall pinning, rather than nucleation under all conditions measured. The variation of saturation magnetization is similar to that of perpendicular magnetic anisotropy with either sputtering power or substrate temperature according to the difference of magnetic domain structure.     

Effect of poly (ethylene glycol) coating on the magnetic and thermal properties of biocompatible magnetic liquids

The aim of this study was to investigate the influence of poly(ethylene glycol) surface-active coating on the magnetic and thermal properties of biocompatible magnetic liquids. The data were analyzed using the high-temperature approximation model taking into account polydispersity of a system. Heating ability of the PEG-stabilized magnetic fluids was determined by the calorimetric measurement of specific absorption rate (SAR) at a frequency of 750 kHz and a magnetic field of 0-2 kA/m. MF-Oleate/PEG heating properties were found to be comparable to the ones of MF-Oleate. The PEG shell thus does not seem to effect the thermal characteristics and SAR values and might make the magnetic fluid useful for application in hyperthermia treatment.     

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.     

Magnetic resonance in iron oxide nanoparticles: Quantum features and effect of size

In order to better understand the transition from quantum to classical behavior in spin system, electron magnetic resonance (EMR) is studied in suspensions of superparamagnetic magnetite nanoparticles with an average diameter of ∼9 nm and analyzed in comparison with the results obtained in the maghemite particles of smaller size (∼5 nm). It is shown that both types of particles demonstrate common EMR behavior, including special features such as the temperature-dependent narrow spectral component and multiple-quantum transitions. These features are common for small quantum systems and not expected in classical case. The relative intensity of these signals rapidly decreases with cooling or increase of particle size, marking gradual transition to the classical ferromagnetic resonance (FMR) behavior.     

As-NMR/NQR study of pressure-induced superconductivity in CaFe2As2

⁷⁵As-zero-field nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements are performed on CaFe₂As₂ under pressure. At P=4.7 and 10.8 kbar, the temperature dependence of nuclear-spin-lattice relaxation rate (1/T₁) measured at tetragonal phase show no coherence peak just below T_c and decrease with decreasing temperature. The superconductivity is of gapless at P=4.7 kbar but evolves to multiple gaps at P=10.8 kbar. We find that the superconductivity appears near a quantum critical point. Both electron correlation and superconductivity disappear in the collapsed tetragonal phase. A systematic study under pressure indicates that electron correlations play a vital role in forming Cooper pairs in this compound.     

Synthesis and anomalous magnetic properties of CoCr2O4 nanocrystallites with lattice distortion

Nanocrystalline Cobalt chromite (CoCr₂O₄) ceramic has been synthesized under a mild condition, rather than by a high-temperature sintering (e.g. >1673 K, in general). A shifted hysteresis loop with an exchange-bias field of 35.7 kA/m and a high coercivity of 627.9 kA/m at 4.2 K was achieved under the cooling field of 2.39×10⁶ A/m. X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) results reveal that a strong lattice distortion and a large amount of surface defects exist in CoCr₂O₄ nanocrystallites (NCs). The anomalous magnetic properties, such as bias field and large coercivity, are attributed not only to the nanosize effect but also to the lattice distortion and crystal defects.     

Magnetic properties of nanoscale crystalline maghemite obtained by a new synthetic route

In this work we describe the synthesis and characterization of maghemite nanoparticles obtained by a new synthetic route. The material was synthesized using triethylamine as a coprecipitation agent in the presence of the organic ligand N,N′-bis(3,5-di-tert-butyl-catechol)-2,4-diaminotoluene (LCH₃). Mössbauer spectrum at 4 K shows typical hyperfine parameters of maghemite and Transmission Electron Microscopy images reveal that the nanoparticles have a mean diameter of 3.9 nm and a narrow size distribution. AC magnetic susceptibility in zero field presents an Arrhenius behavior with unreasonable relaxation parameters due to the strong influence of dipolar interaction. In contrast when the measurements are performed in a 1 kOe field, the effect of dipolar interactions becomes negligible and the obtained parameters are in good agreement with the static magnetic properties. The dynamic energy barrier obtained from the AC susceptibility results is larger than the expected from the average size observed by HRTEM results, evidencing the strong influence of the surface contribution to the anisotropy.     

Mechanism of chain formation in nanofluid based MR fluids

Mechanism of structure formation in bidispersed colloids is important for its physical and optical properties. It is microscopically observed that the mechanism of chain formation in magnetic nanofluid based magnetorheological (MR) fluid is quite different from that in the conventional MR fluid. Under the application of magnetic field the magnetic nanoparticles are filled inside the structural microcavities formed due to the association of large magnetic particles, and some of the magnetic nanoparticles are attached at the end of the chains formed by the large particles. The dipolar energy of the large particles in a magnetic nanofluid matrix becomes effective magnetic permeability (μ_eff) times smaller than that of the neutral medium. Inclusion of magnetic nanoparticles (∼10 nm) with large magnetic particles (∼3-5 μm) restricts the aggregation of large particles, which causes the field induced phase separation in MR fluids. Hence, nanofluid based MR fluids are more stable than conventional MR fluids, which subsequently increase their application potentiality.     

Preparation and chemical stability of iron-nitride-coated iron microparticles

Iron-nitride-coated iron microparticles were prepared by nitridation of the surface of iron microparticles with ammonia gas at a temperature of 510 °C. The phases, composition, morphology, magnetic properties, and chemical stability of the particles were studied. The phases were α-Fe, ε-Fe₃N, and γ-Fe₄N. The composition varied from the core to the surface, with 99.8 wt% Fe in the core, and 93.8 wt% Fe and 6 wt% N in the iron-nitride coating. The thickness of the iron-nitride coating was about 0.28 μm. The chemical stability of the microparticles was greatly improved, especially the corrosion resistance in corrosive aqueous media. The saturation magnetization and the coercive force were 17.1×10³ and 68 kA/m, respectively. It can be concluded that iron-nitride-coated iron microparticles will be very useful in many fields, such as water-based magnetorheological fluids and polishing fluids.     

Influence of complexing agent on the electrodeposited Co-Pt-W magnetic thin films

Complexing agents are often used to improve the quality of electrodeposited alloys. Influence of different complexing agents with hydroxycarboxylic acid group on the electrodeposited Co-Pt-W thin films has been investigated. Cathodic polarization curves show that the polarization behaviors of electroplating bath with different complexing agents are very different. Surface morphology, phase composition and magnetic properties are observed by means of FESEM, XRD and vibrating sample magnetometer (VSM), respectively. It has been found out that, if citrate was used as complexing agent, the Co-Pt-W thin films were homogeneous and the granular crystals with the average grain size of 2 μm have been observed. Co-Pt-W thin films exhibited hexagonal close packed (hcp) lattice and strong perpendicular anisotropic magnetic behavior (H_c⊥ = 215.5 kA/m; H_c∥ = 55.4 kA/m). In the presence of gluconate, needle-like deposits were obtained and a strong face centered cubic (fcc(1 1 1)) texture was measured. The Co-Pt-W thin films showed isotropic magnetic behavior. In the case of tartate and malate, the coexistence of needle-like deposits and cellular deposits appeared. The XRD patterns showed that the mixed fcc and hcp phase formed. Perpendicular anisotropic magnetic behaviors of thin films, from malate or tartate baths, were not obvious.