Major Loop Research Articles

Structure of Alloys for (Sm,Zr)(Co,Cu,Fe)z Permanent Magnets: III. Matrix and Phases of the High-Coercivity State.

Observations of the surface domain structure (Kerr-effect), optical metallography, scanning electron microscopy (SEM-SE), and electron microprobe analysis (EPMA-SEM), measurements of major and minor magnetic hysteretic loops were used to study pseudo-single-crystal samples of (Sm,Zr)(Co,Cu,Fe)z alloys subjected to heat treatments to the high-coercivity state, which are used in fabricating sintered permanent magnets. Correlations between the chemical composition, hysteretic properties, structural components, domain structure, and phase state were determined for the concentration ranges that ensure wide variations of 4f-/4d-/3d-element ratio in the studied samples. The phase state formed by collinear and coherent phase components determines the high coercive force and ultimate magnetic hysteresis loops of the pseudo-single crystals. It was found that the 1:5 phase with the hexagonal structure (P6/mmm) is the matrix of the alloys for (Sm,Zr)(Co,Cu,Fe)z permanent magnets; the matrix undergoes phase transformations in the course of all heat treatments for the high-coercivity state. The heterogeneity observed with optical magnifications, namely, the observation of main structural components A and B, is due to the alternation, within the common matrix, of regions with modulated quasi-spherical precipitates and regions with hexagonal bipyramids (cellular phase) although, traditionally, many investigators consider the cellular phase as the matrix. It is shown that the relationship of volume fractions of structural components A and B that account for more than 0.9 volume fraction of the total, which is due to the integral chemical composition of the alloys, determines the main hysteretic performances of the samples. The Zr-rich phases, such as 5:19, 2:7, and 6:23, and a structural component with the variable stoichiometry (Sm(Co,Cu,Fe)3.5–5) that is almost free of Zr and contains up to 33 at% Cu, were found only within structural component A in quantities sufficient for EPMA analysis.

A Novel In Situ High‐Temperature Magnetometry Method for Radiofrequency Heating Applications

AbstractRadiofrequency heating of magnetic particles promises highly efficient and direct heating of catalytic reactors for coupling of low carbon electricity with energy intensive chemical transformations. In this work, a novel real‐time and in situ magnetometry method is developed to measure minor and major hysteresis loops of soft magnetic nanopowders. It is applied to measure the magnetic properties and hysteresis power absorption of magnetite and maghemite powders up to 500 °C. An arctangent model for saturation magnetization is adapted for minor hysteresis loops. It produces an excellent fit for hysteresis loop power across field strengths up to 18.5 kA m−1 and allows prediction of heating power, remanence, and susceptibility. Samples of magnetite and maghemite are shown to heat rapidly from room temperature at more than 25 °C s−1, with maghemite giving the strongest heating response. The peak heating power occurs at the transition beyond the ellipsoidal Rayleigh law region. These findings suggest that the properties of magnetic powders, coupled with variable magnetic field strengths and frequencies, can be tuned to optimize the heating power for a variety of applications.

Electric field and frequency dependent scaling behavior of dynamic hysteresis in the epitaxial (Pb0.9La0.1)(Zi0.4Ti0.6)O3 films

Epitaxial (Pb0.9La0.1)(Zi0.4Ti0.6)O3 (PLZT) film was prepared with Pt as the upper electrode and La0.5Sr0.5CoO3(LSCO) as the bottom electrode on (001) STO substrate by radio frequency (RF) magnetron sputtering. The dynamic hysteresis scaling behavior of the film, including the variation of remanent polarization (P r), coercive field (E c), and loop area () with external field (E 0) and frequency (f) , was systematically studied. The evolution of scaling behavior in the PLZT film can be divided into two stages: minor loops and major loops, which are in the low and high E 0 regions, respectively. The scaling relations take form of and in minor loops and major loops, respectively. The results show that the domain structure and domain reversal play an important role in the dynamic hysteresis behavior of ferroelectric materials.

Critical curves in NiFe/FeMn bilayers with varying antiferromagnetic layer thickness

The effect of antiferromagnetic (AF) layer thickness on exchange bias was studied in a series of NiFe(50 nm)/FeMn(t) bilayers through both irreversible and reversible experiments at room temperature. The exchange bias was evaluated in the sample plane both through measurement of the major hysteresis loops and probing the reversible susceptibility. The critical curve was constructed to map the angular dependence of the magnetization switching and exchange bias, which is found to evolve as a function of AF layer thickness. Ferromagnetic resonance absorption was measured at several frequencies and angles, and angular-dependent absorption curves were plotted. A comparison is made between the recorded exchange bias using the three methods. The measurements reported are supported by simulations under a generalized Stoner–Wohlfarth model, and general limitations of the experiment are discussed.

Thermal Stability, Blocking Regime and Superparamagnetic Behavior in Mn-Al-C Melt Spun Ribbons.

Alloys possessing nominal compositions Mn53Al45C2 and Mn52Al46C2 were prepared by the melt spinning method and were subjected to complex structural, morphological and magnetic investigations. As these alloys can exhibit tetragonal L10-type and τ phase, they have good potential as rare earth (RE)—free magnets. It is, therefore, important to monitor the ε–τ phase transformation and the stability and the magnetic features of the tetragonal phase in an entire temperature interval. By using synchrotron X-ray diffraction, it has been proven that the ε–τ phase transformation occurs gradually, with the τ phase becoming predominant only after 450 °C. Moreover, this phase has been proven to be quite stable without any grain growth even at the highest temperature investigated at 800 °C. Low temperature behavior was thoroughly investigated by using a complex combination of major and minor hysteresis loops combined with the zero field cooled-field cooled magnetization protocols (ZFC-FC). Two different regimes, blocking and superparamagnetic, were documented. A spin reorientation transition was proven to occur at 55 K while a maximum magnetization observed in ZFC-FC curves proved that at about 75 K, a transition from ferro to superparamagnetic state occurs. The existence of a blocking regime below 55 K that is characteristic to nanogranular systems with superparamagnetic behavior has shown further development towards obtaining RE-free magnets.

Improved Preisach Model for the Vector Hysteresis Property of Soft Magnetic Composite Materials Based on the Hybrid Technique of SA-NMS

The two-dimensional hysteresis property of the soft magnetic composite (SMC) material under circular rotational excitation was measured by the experimental platform. The first-order reversal curves and the corresponding scalar Everett functions can be numerically generated by the measured major hysteresis loops along the orthogonal easy axis and hard axis. Different from the classical model, an improved vector Preisach hysteresis model that considers the anisotropic property of the SMC materials under vector magnetic excitation was put forward by introducing two parameters w and z. The two parameters were used to identify the vector Everett functions and adjust the shape of hysteresis curves under different magnitudes of the magnetic flux density. Furthermore, an efficient hybrid algorithm that combines simulated annealing with Nelder-Mead simplex technique was proposed for the accurate extraction of optimal parameters. The simulated results based on the improved model agree well with the measured ones; thus, the effectiveness and accuracy of the proposed method were verified.

Observation of recoil magnetization curves outside the major loop in Co, Fe, and Ni films

We report a peculiar magnetization reversal observed in magnetron-sputtered Co, Fe, and Ni films. We found that some recoil (minor) magnetization curves lie entirely and way outside the major loop, a phenomenon referred to here as a recoil-curve overshoot. The greatly enhanced recoil curve's remanence and coercivity result in an up to 2.5-fold increase of loop's area. The model of pairs of exchange-coupled grains with misaligned anisotropy axes reproduces, in a very good agreement with the experiment, all key features of the recoil-curve overshoot as well as the kink that some major loops present before saturation. The disclosed features of the ferromagnetic hysteresis provide further insights into this important classical phenomenon.

Exchange bias training in La0.7Sr0.3FeO3/Ni79Fe21 films with native surface oxide: First-order reversal curve analysis

In conventional magnetometry, exchange bias training (EBT) is mostly evaluated through the major magnetization hysteresis loops (MHLs). We here report a study of EBT by using the first-order reversal curves (FORCs) in the heterostructures of ${\mathrm{SrTiO}}_{3}(001)/{\mathrm{La}}_{0.7}{\mathrm{Sr}}_{0.3}{\mathrm{FeO}}_{3}(\mathrm{LSFO})/{\mathrm{Ni}}_{79}{\mathrm{Fe}}_{21}(\mathrm{Py})/{\mathrm{PyO}}_{x}$. It was unraveled that the training effect occurs once after exceeding the left coercivity of the first MHL, while the magnetic coupling from the ultrathin native oxide (${\mathrm{PyO}}_{x}$) mainly contributes to an exchange springlike behavior. Besides for the first MHL, the FORCs corresponding to the second MHL and the quasiequilibrium stage were collected, respectively, which provide a detailed picture of how the magnetization reversal evolves in the training process.

A rate-dependent constitutive model incorporated in two-dimensional PolyFEM for Galfenol sensors

A micromechanical model with rate effects is developed to constitute the nonlinear hysteresis sensor behaviour of Galfenol and embedded into a numerical framework, the polygonal finite element method. The model stems from the domain rotation events taking place at microlevel in response to the external magnetomechanical loads. The internal variables of the model to represent the material state at any instant are the volume fraction of the domains, and their evolution equations are derived using thermodynamic principles. Inter-domain effects within each grain are accounted in the form of back fields that act as hardening or softening parameters. The constitutive model is extended further to include the rate effects and then incorporated into a hybrid-magnetomechanical-formulation with Voronoi-based-discretization to study the behaviour of Galfenol. The Voronoi discretizations closely resemble the microstructure of Galfenol with each finite element specifying a random grain in the polycrystalline Galfenol. The developed framework is shown to simulate the major and minor loop sensor responses of the material with rate effects under complex loading conditions.

The Relaxation Effects in the Preisach - Néel Model of Patterned Media

Abstract In this paper, we present the calculation of thermal magnetic viscosity based on numerical simulations of relaxation isotherms curves for a Stoner–Wohlfarth ensemble. The Stoner–Wohlfarth particles is described by two equilibrium states and thermal activation is done by overcoming the energy barrier. For simulations we have used a new Preisach type model for Patterned Media, which takes into account the effects of time and temperature. The magnetization of the system is treated using the Preisach Model for Patterned Media with bimodal interactions field distributions. We have simulated relaxation curves starting from different points on the negative region of the descending branch of the major hysteresis loop and from the obtained data we evaluated the thermal fluctuation field. The results obtained for the linear energy barrier were compared with the non-linear energy barrier.

Precise appraisement of the harmonic loads impact on hysteresis losses in a 3-phase HTS transformer

Nowadays, the application of non-linear loads such as, rectifiers, electronic phase control, PWM drives, gives rise to a vastly increased level of harmonics in the power network. As such, the transport currents of transformers are non-sinusoidal alternating currents. On the other hand, AC losses are one of the most critical characteristics for the design and operation of high-temperature superconducting (HTS) transformers. The amount of hysteresis losses is a key parameter for the design of HTS windings affecting equipment, cooling cost, efficiency, and transformer economic feasibility. The computation of AC losses by traditional techniques, is suitable for the sinusoidal current condition. While, non-linear loads brings about different number of peaks and amplitudes in the current waveform passing through the HTS transformer windings. So that, in addition to the major hysteresis loop, a number of minor hysteresis loops are also formed changing the hysterical nature of the AC losses.Hence, this paper proposes an accurate, yet efficient analytical algorithm, for calculating hysteresis losses in a three-phase HTS transformer's windings in the presence of the harmonic loads accounting for the AC losses estimation. This is accomplished by performing a numerical Finite Element Method to verify the analytical results. The analysis of the hysteresis losses in an exemplary 315 kVA three-phase HTS distribution transformer for different harmonic loads, is another object of this paper.

Tubule-specific protein nanocages potentiate targeted renal fibrosis therapy

BackgroundDespite the dramatic advances in modern medicine, efficient therapeutic measures for renal fibrosis remain limited. Celastrol (CLT) is effective in treating renal fibrosis in rat models, while causing severe systemic toxicity. Thus, we designed a tubule-specific nanocage (K3-HBc NCs) that effectively deliver CLT to tubular epithelial cell in a virus-like manner. The targeting ligand (K3) to tubular epithelial cells was displayed on the surface of Hepatitis B core protein (HBc) NCs by genetic fusion to the major immunodominant loop region. Ultra-small CLT nanodots were subtly encapsulated into the cavity through electrostatic interaction with the disassembly and reassembly of K3-HBc NCs, to yield K3-HBc/CLT complex. The efficacy of K3-HBc/CLT NCs were demonstrated in Unilateral ureteral obstruction (UUO)-induced renal fibrosis.ResultsThe self-assembled K3-HBc/CLT could specifically target tubular epithelial cells via affinity with K3 ligand binding to the megalin receptor, significantly attenuating renal fibrosis. Remarkably, K3-HBc/CLT NCs significantly increased therapeutic efficacy and reduced the systemic toxicity in comparison with free CLT in UUO-induced mouse renal fibrosis model. Importantly, analysis of RNA sequencing data suggested that the anti-fibrotic effect of K3-HBc/CLT could be attributed to suppression of premature senescence in tubular epithelial cells via p21Cip1 and p16Ink4a pathway.ConclusionThe tubule-specific K3-HBc/CLT represented a promising option to realize precise treatment for renal fibrosis.

Paramount Importance of Core Conformational Changes for Heparin Allosteric Activation of Antithrombin.

Antithrombin is unique among serpin family protein protease inhibitors with respect to the major reactive center loop (RCL) and core conformational changes that mediate allosteric activation of its anticoagulant function by heparin. A critical role for expulsion of the RCL hinge from a native stabilizing interaction with the hydrophobic core in the activation mechanism has been proposed from reports that antithrombin variants that block this change through engineered disulfide bonds block activation. However, the sufficiency of core conformational changes for activation without expulsion of the RCL from the core is suggested by variants that are activated without the need for heparin and retain the native RCL-core interaction. To resolve these apparently conflicting findings, we engineered variants in which disulfides designed to block the RCL conformational change were combined with constitutively activating mutations. Our findings demonstrate that while a reversible constitutive activation can be engineered in variants that retain the native RCL-core interaction, engineered disulfides that lock the RCL native conformation can also block heparin allosteric activation. Such findings support a three-state allosteric activation model in which constitutive activating mutations stabilize an intermediate-activated state wherein core conformational changes and a major activation have occurred without the release of the RCL from the core but with a necessary repositioning of the RCL to allow productive engagement with an exosite. Rigid disulfide bonds that lock the RCL native conformation block heparin activation by preventing both RCL repositioning in the intermediate-activated state and the release of the RCL from the core in the fully activated state.

Magnetic investigations on irradiation-induced nanoscale precipitation in reactor pressure vessel steels: A first-order reversal curve study

We have investigated magnetic properties for reactor pressure vessel model alloys with variable Cu contents, subjected to neutron irradiation up to a fluence of 9 × 10 19 n cm − 2 . Unlike a monotonic increase of microhardness with neutron fluence, the major-loop coercivity decreases at a higher fluence and the decrease becomes larger for the alloy containing a higher amount of Cu. The measurements of first-order reversal curves (FORCs) for the high-Cu alloy show that the position of the FORC distribution peak shifts toward a lower coercivity just after neutron irradiation, followed by a slight increase, associated with the broadening along both the coercivity and interaction field axes. The results can be explained by the enhancement of magnetic inhomogeneity in a matrix due to Cu precipitation and an increasing magnetostatic interaction between local magnetic regions with different coercivity. The magnetic method using FORCs can be a possible technique which provides in-depth information on microstructural changes due to neutron irradiation, which is not obtained by measurements of a conventional major hysteresis loop.

Consideration of Magnetic Measurements for Characterisation of Ferrite–Martensite Commercial Dual-Phase (DP) Steel and Basis for Optimisation of the Operating Magnetic Field for Open Loop Deployable Sensors

The magnetic properties of commercial dual-phase (DP) steels (DP600, DP800 and DP1000 grades) were evaluated using initial permeability, incremental permeability and coercivity and correlated with the key microstructural differences between the grades. The ferrite grain sizes and ferrite fractions have been compared with the magnetic parameters obtained from minor and major magnetisation loops within each DP grade. It has been revealed that the incremental permeability increases with the applied magnetic field amplitude to reach a peak and then drops at a higher magnetic field, with the values being different for the three DP grades at a lower field and converging to a similar permeability value at the high field. The effects of ferrite grain size and phase fraction on the incremental permeability are considered, and it has been shown that the influence of ferrite grain boundaries on magnetic permeability is more dominant than the effect of ferrite fraction in commercial DP steel samples. An analysis of the correlation between coercivity and initial permeability with tensile strength shows that the initial permeability provides a slightly better prediction of strength for the steels examined, which is believed to be due to the fact that a combination of reversible and irreversible domain components affect the coercivity value, while the initial permeability is predominantly affected by reversible domain movements. Based on the trend between incremental permeability and applied magnetic field and the commercial EM sensor (EMspec) operating parameters, the effect of lift-off and hence magnetic field strength on the sensitivity to DP steel properties can be assessed.

Sleep-related hypermotor epilepsy associated mutations uncover important kinetic roles of α4β2- nicotinic acetylcholine receptor intracellular structures.

Sleep-related hypermotor epilepsy (SHE) is a group of seizure disorders prominently associated with mutations in nicotinic acetylcholine receptors (nAChR). The most prevalent central nervous system nAChR subtype contains α4 and β2 subunits, in two ratios. (α4β2)2β2-nAChR have high agonist sensitivity (HS-isoform), whereas (α4β2)2α4-nAChR agonist responses exhibit a small high-sensitivity, and a predominant low-sensitivity, phase of function (LS-isoform). Multiple non-synonymous mutations in the second and third transmembrane domains of α4 and β2 subunits are associated with SHE. We recently demonstrated that two additional, SHE-associated, missense mutations in the major cytoplasmic loops of these subunits [α4(R336H) and β2(V337G)] cause increased macroscopic function-per receptor. Here, we use single-channel patch-clamp electrophysiology to show that these mutations influence single-channel amplitudes and open- and closed-state kinetics. Pure populations of HS- or LS-isoform α4β2-nAChR were expressed by injecting either 1:10 or 30:1 α4:β2 cRNA ratios, respectively, into Xenopus laevis oocytes. Functional properties of the resulting mutant α4β2-nAChR isoforms were compared to their wildtype counterparts. α4(R336H) subunit incorporation minimally affected single-channel amplitudes, whereas β2(V337G) subunit incorporation reduced them significantly in both isoforms. However, for both mutant subunits, increased function-per-receptor was predominantly caused by altered single channel kinetics. The α4(R336H) mutation primarily destabilizes desensitized states between openings. By contrast, the β2(V337G) mutation principally stabilizes receptor open states. The use of naturally-occurring and physiologically-impactful mutations has allowed us to define valuable new insights regarding the functional roles of nAChR intracellular domains. Further mechanistic context is provided by intracellular-domain structures recently published for other members of the Cys-loop receptor superfamily (α3β4-nAChR and 5-HT3AR).

Reconstructing phase-resolved hysteresis loops from first-order reversal curves

The first order reversal curve (FORC) method is a magnetometry based technique used to capture nanoscale magnetic phase separation and interactions with macroscopic measurements using minor hysteresis loop analysis. This makes the FORC technique a powerful tool in the analysis of complex systems which cannot be effectively probed using localized techniques. However, recovering quantitative details about the identified phases which can be compared to traditionally measured metrics remains an enigmatic challenge. We demonstrate a technique to reconstruct phase-resolved magnetic hysteresis loops by selectively integrating the measured FORC distribution. From these minor loops, the traditional metrics—including the coercivity and saturation field, and the remanent and saturation magnetization—can be determined. In order to perform this analysis, special consideration must be paid to the accurate quantitative management of the so-called reversible features. This technique is demonstrated on three representative materials systems, high anisotropy FeCuPt thin-films, Fe nanodots, and SmCo/Fe exchange spring magnet films, and shows excellent agreement with the direct measured major loop, as well as the phase separated loops.

Pressure gradient effect on spin-crossover materials: Experiment vs theory

We studied the effect of non-hydrostatic pressure on the hysteretic spin crossover in coordination complexes. By introducing into an Ising-like model a double distribution of the interactions and gap energy, respectively, we were able to generate the major hysteresis loop and the first-order reversal curve (FORC) diagram for spin-crossover systems of 106 hysterons (like-spin domains). We show that, for high pressure gradients around the spin-crossover system, the thermal hysteresis loop takes an asymmetric shape, in good agreement with the experimental data on pressure effect recorded at low temperatures, below the solidification of the pressure transmitting medium. Interestingly, the FORC diagram method seems to be much more sensitive to local changes than the “bulk” parameters, which characterize the major hysteresis loop.

Temperature Dependence and Microstructure Effects on Magnetic Properties of FePt(B, Ag, C) Film.

A FePt(B, Ag, C) granular film was formed from post-annealed B4C(1.0 nm)/FePt(Ag, C) layers at a substrate temperature of 470 °C for 2 min. The 6 nm thick FePt(B, Ag, C) film demonstrates high perpendicular magnetic anisotropy (Ku = 2.83 × 107 erg/cm3 at 100 K) and out-of-plane coercivity (Hc = 38.0 kOe at 100 K). The Ku and out-of-plane Hc are respectively increased from 38% and 46% between 350 K and 50 K. The sample with a thickness of 8 nm also shows a similar trend for magnetic properties; however, the tiny magnetization kink which may come from rare Fe-B or disordered FePt grains was observed in the easy axis loop. The intrinsic (ΔHint = 12.6 kOe) and extrinsic switching field distribution (ΔHext = 1.62 kOe) were characterized by major and minor loops to correlate the microstructural grains. The coupled FePt grains grown on a single MgTiON grain were observed in a high-resolution transmission electron microstructure (HRTEM) image. This small intergranular exchange coupling was defined by estimating the magnetic cluster size (46.6 nm) from ΔHext and the average grains size (28.2 nm) from TEM images. The temperature dependence of coercivity was fitted to further understand the magnetization reversal process. The lower microstructural parameter was evidenced in the imperfect grain morphology.

Modified Preisach Model of Hysteresis in Multi Air Gap Ferrite Core Medium Frequency Transformer

This article presents the modified Preisach model of hysteresis for a 3-phase medium frequency transformer in a 100 kW dual active bridge converter. The transformer magnetic core is assembled out of ferrite I-cores, which results in multiple parasitic air gaps. For this transformer, the hysteresis loops were measured and parameters of the Preisach model were determined. The Preisach distribution function is approximated with a two-dimensional Gauss function series and the feedback function is a 3rd-degree polynomial. The optimized identification of Preisach distribution function parameters was prepared. Two sets of parameters were determined based on the analysis of major and minor hysteresis loop. The developed model is used to analyze the transformer core power loss. A new set of Steinmetz equation parameters for multi air gap ferrite core MFT is proposed.