Texture measurement of grain-oriented electrical steels after secondary recrystallization

The measurement of the final Goss texture sharpness in grain-oriented electrical steels is a challenging task due to the immense grain size ranging from millimeters to centimeters. Although, it is widely claimed in the literature that the orientation deviations from the ideal Goss orientation lie in the range of about 7° for conventional grain-oriented steel and in the range of about 3° for high permeability grades, no precise investigation with an appropriate statistical relevance is known to the authors.     

Effects of SnO2 addition on the magnetic properties of manganese zinc ferrites

SnO₂ was added to high-permeability MnZn ferrites and MnZn ferrites for high-frequency power supplies. The effects of the SnO₂ addition were studied. Sn⁴⁺ ions can dissolve into the spinel lattice and form stable Fe²⁺–Sn⁴⁺ pairs and hence can compensate the magneto-crystalline anisotropy constant K₁ and improve the initial permeability effectively. The initial permeability of ferrites is also improved as abnormal grain growth caused by ion vacancy is controlled with SnO₂ doping. In addition, the SnO₂ doping also leads to a decrease in the relative loss factor and an increase in density. The power loss and minimum power loss temperature decrease with SnO₂ doping.     

Ferromagnetic CrSb film fabricated by pulse-laser deposition and rapidly annealing

CrSb film was fabricated by pulse laser deposition (PLD) on Si (1 0 0) wafer. Strong ferromagnetism was observed in the CrSb film annealed at a high heating/cooling rate of 200 K/s, which can be attributed to the presence of ferromagnetic zinc blende (ZB) CrSb phase. The appearance of metastable ZB-CrSb results from the strong inner stress due to the precipitation of the monoclinic Sb.     

Surface modification and properties of Bombyx mori silk fibroin films by antimicrobial peptide

The Bombyx mori silk fibroin films (SFFs) were modified by a Cecropin B (CB) antimicrobial peptide, (NH₂)-NGIVKAGPAIAVLGEAAL-CONH₂, using the carbodiimide chemistry method. In order to avoid the dissolution of films during the modification procedure, the SFFs were first treated with 60% (v/v) ethanol aqueous solution, resulting a structural transition from unstable silk I to silk II. The investigation of modification conditions showed that the surface-modified SFFs had the satisfied antimicrobial activity and durability when they were activated by EDC·HCl/NHS solution followed by a treatment in CB peptide/PBS buffer (pH 6.5 or 8) solution at ambient temperature for 2 h. Moreover, the surface-modified SFFs showed the smaller contact angle due to the hydrophilic antimicrobial peptides coupled on the film surface, which is essential for the cell adhesion and proliferation. AFM results indicated that the surface roughness of SFFs was considerably increased after the modification by the peptides. The elemental composition analysis results also suggested that the peptides were tightly coupled to the surface of SFFs. This approach may provide a new option to engineer the surface-modified implanted materials preventing the biomaterial-centered infection (BCI).     

On the understanding of the microscopic origin of the properties of diluted magnetic semiconductors by atom probe tomography

Spintronics, in which both the spin and charge of electrons are used for logic and memory operations, promises to revolutionize the current information technology. Just as silicon supports microelectronics, diluted magnetic semiconductors (DMSs) will be the platform of spintronics. Ideal DMSs should maintain ferromagnetic and semiconducting properties at operating temperatures to realize the spintronic functions. Although many high-temperature Curie temperature DMSs have been reported, the origin of ferromagnetism remains controversial. Currently, this is a major obstacle to the development of spintronic devices. The solution to this problem depends on a more complete understanding of DMS microstructure, especially the distribution of doped magnetic ions at atomic resolution and any defects introduced. Therefore, an analysis technique is required, possessing both high spatial and elemental resolutions, which is beyond the capability of conventional techniques, such as electron microscopy. However, atom probe tomography (APT), which recently has been successfully applied to nanoscale characterization of structural materials, has the potential to provide the unique combination of near atomic spatial and elemental resolutions needed for such an investigation.     

Ensemble inequivalence in random graphs

We present a complete analytical solution of a system of Potts spins on a random k-regular graph in both the canonical and microcanonical ensembles, using the Large Deviation Cavity Method (LDCM). The solution is shown to be composed of three different branches, resulting in a non-concave entropy function. The analytical solution is confirmed with numerical Metropolis and Creutz simulations and our results clearly demonstrate the presence of a region with negative specific heat and, consequently, ensemble inequivalence between the canonical and microcanonical ensembles.     

Electron beam treatments of electrophoretic ceramic coatings

In this work a method to densify ceramic coating obtained by electrophoresis and to improve its adhesion to the substrate is proposed. It consists in irradiating the coating surface by electron beam (EB). Alumina and alumina-zirconia coatings were deposited on stainless steel substrates and treated by low power EB. SEM, XRD and TEM characterizations demonstrated that the sintering occurred. Moreover, it is shown that on alumina-zirconia coating the EB irradiation produced a composite material consisting principally of tetragonal zirconia particles immersed in an amorphous alumina matrix. The adhesion stress of EB treated coating was estimated by stud pull test and it was found to be comparable to that of plasma-sprayed coatings.     

Effect of initial grain size on texture evolution and magnetic properties in nonoriented electrical steels

The magnetic properties of nonoriented electrical steels are influenced by the grain size and crystallographic texture. The technologies used to control the grain size in nonoriented electrical steels are approaching their limits. However, there is still some room for improvement of the magnetic properties through texture control. Hot-band annealing is known to be one of the most effective processing stages for texture modification. In this study, two types of initial grain sizes prior to cold rolling are obtained by different hot-band annealing. The effect of initial grain size on texture evolution and magnetic properties in nonoriented electrical steels containing 2% Si is examined. The specimens having different initial grain sizes have significantly different textures in the cold-rolled state and the annealed state. During the recrystallization stage, new grains formed in the coarse-grained specimens have stronger Goss but weaker γ-fibre texture than those in the fine-grained specimens. During the grain growth after complete recrystallization, the coarse-grained specimens still have weaker γ-fibre texture than the fine-grained specimens. The magnetic induction of the coarse-grained specimens is always higher at the same temperature than that of the fine-grained specimens. The core loss of the coarse-grained specimens is lower at the same temperature than that of fine-grained specimens. However, the improvement of the core loss becomes less pronounced as the annealing temperature increases.     

Curie temperatures and crystallization behavior of amorphous Fe81−xNixZr7B12 (x=10, 20, 30, 40, 50, 60) alloys

Curie temperature, crystal structure and crystallization behavior of amorphous alloys with the stoichiometry Fe_81−xNi_xZr₇B₁₂ (x=10–60) have been studied by X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and AC-magnetization (TMAG) measurements as functions of temperature. The thermal stability of long-range magnetic order, T_C vs. Ni content in as-quenched amorphous alloys exhibits maximum at 352 °C for x=40. The primary crystallization has been detected during annealing at the first crystallization stage of all ribbons investigated.     

The effect of solution temperature on crystallite size and magnetic properties of Zn substituted Co ferrite nanoparticles

In this work zinc substituted cobalt ferrite nanoparticles (Co_0.5Zn_0.5Fe₂O₄) have been synthesized by the coprecipitation method, using stable ferric, zinc and cobalt salts with sodium hydroxide, at different solution temperatures, from room temperature to 363 K. The cobalt-zinc ferrite crystalline phase, the particle size and the morphology of the resulting nanoparticles were studied by X-ray diffraction and transmission electron microscopy. The average crystallite size of each sample was calculated from the broadening of the most intense peak (3 1 1), using Scherrer's formula and the results show crystallite sizes increased from 6 to 8 nm by increasing the solution temperature from room temperature to 363 K respectively. Room temperature VSM measurements show that the prepared nanoparticles have superparamagnetic behavior and did not saturate at maximum field of 800 kA/m. The variation of AC-susceptibility of the samples with respect to temperature was measured and it was found that the blocking temperature increased from 198 to 270 K by increasing the solution temperature from room temperature to 363 K respectively. FTIR spectra of the samples have been analyzed in the frequency range 400-4000 cm⁻¹, which also confirms the results of XRD.     

Magnetization of sol-gel prepared zinc ferrite nanoparticles: Effects of inversion and particle size

Nanoparticles of ZnFe₂O₄ have been prepared by using sol-gel method in two different mediums (acidic and basic) in order to observe the influence of the medium on the magnetic properties of the obtained nanoparticles. X-ray diffraction and Mössbauer studies of these samples show the presence of single-phase spinel structure. The average size of the particles as determined by X-ray diffraction increases with the annealing temperature from 18 to 52 nm. With the increase in particle size, magnetization decreases while the magnetization blocking temperature increases. Magnetization studies show that the samples prepared in basic medium have more ferrimagnetic nature as compared to those prepared in acidic medium. We understand this increase in magnetization as reflective of the increased degree of inversion (transfer of Fe³⁺ ions from octahedral to tetrahedral sites) in the particles of smaller size unit cells. From lattice parameter calculations on different particles it is determined that inversion is more favorable in the particles prepared in a basic medium than in the acidic medium due to the smaller cell size in the former.     

Electrochemical formation of intermediate layer for Co/Pd multilayered media

Pd nanocluster seeds were formed on a soft magnetic underlayer (SUL) using an electrochemical substitution reaction, and were utilized as an intermediate layer for a Co/Pd multilayered ([Co/Pd]_n) perpendicular magnetic recording medium. A CoNiFeB film prepared with electroless deposition was used as SUL, which was immersed into a PdCl₂ solution for the formation of Pd seeds. The Pd seeds were found to effectively reduce the size of magnetic domains in the [Co/Pd]_n film deposited on them. The optimization of the concentration of the PdCl₂ solution and the use of the pretreatment process with a SnCl₂ solution were effective to obtain the smooth SUL surface with fine Pd seeds as small as 5 nm. The 20 nm-thick [Co/Pd]_n film deposited on the optimized Pd seeds/CoNiFeB SUL exhibited a high coercivity of 7.8 kOe and a small magnetic domain size of 69 nm. These results indicated that the combination of the Pd seeds and the electroless-deposited SUL was desirable in terms of the improvement not only in the magnetic properties of [Co/Pd]_n media but also in the mass productivity of the underlayer.     

Study of domain structure of magnetic powder particles by Mössbauer spectroscopy

The determination technique of monodomain state of the magnetic powder particles using the Mössbauer spectroscopy is described. The method was verified on the particles of gadolinium iron garnet near the compensation temperature. It has also shown that using the Mössbauer spectroscopy we can evaluate the domain wall energy in ferrites possessing the compensation point.     

Photoluminescence enhancement and stabilisation of porous silicon passivated by iron

Iron is incorporated in porous silicon (PS) by impregnation method using Fe(NO₃)₃ aqueous solution. The presence of iron in PS matrix is shown from energy-dispersive X-ray (EDX) analysis and Fourier transform infrared (FTIR) measurements. The optical properties of PS and PS-doped iron are studied by photoluminescence (PL). The iron deposited in PS quenched the silicon dangling bonds then increased the PL intensity. The PL peak intensity of impregnated PS is seven times stronger than that in normal PS. Upon exposing iron-PS sample to ambient air, there is no significant change in peak position but the PL intensity increases during the first 3 weeks and then stabilises. The stability is attributed to passivation of the Si nanocrystallites by iron.     

Demineralisation of semi-anthracite char with molten salts/HCl: Effects on the porous texture and reactivity in air

The effects of chemical heat treatments of a semi-anthracite char (AC) on textural properties and reactivity in air of the material are investigated. The starting char was first treated with a mixture of LiCl/KCl or LiCl/KCl/CaO at 743, 873 or 1173 K and the products obtained were then washed thoroughly with distilled water. A small fraction of these samples were treated with 10⁻³ M HCl solution. Valuable information on textural modifications produced in the material was derived from the adsorption isotherms for CO₂ at 273 K. The reactivity tests were carried out at 808, 823 and 823 K. The microporosity developed and the reactivity in air increased in the partially demineralised products. The former effect was stronger for the LiCl/KCl/CaO-treated samples and the latter for a larger number of the LiCl/KCl-treated samples.     

Electronic structure and ferromagnetism of polycrystalline Zn1−xCoxO (0≤x≤0.15)

The electronic structure of polycrystalline ferromagnetic Zn_1−xCo_xO (0.05≤x≤0.15) and the oxidation state of Co in it, have been investigated. The Co-doped polycrystalline samples are synthesized by a combustion method and are ferromagnetic at room temperature. XPS and optical absorption studies show evidence for Co²⁺ ions in the tetrahedral symmetry, indicating substitution of Co²⁺ in the ZnO lattice. However, powder XRD and electron diffraction data show the presence of Co metal in the samples. This give evidence to the fact that some Co²⁺ ion are incorporated in the ZnO lattice which gives changes in the electronic structure whereas ferromagnetism comes from the Co metal impurities present in the samples.     

A novel technique for measurement of core loss in low permeability materials

A survey of existing techniques for measuring core loss in magnetic materials is presented. It is shown that the most challenging combination is a low permeability material at low measurement frequency. Such materials have application in components of power converters, and thus are of considerable technological significance. Measurement difficulties stem from losses in the windings employed, which are difficult to disentangle from loss in the core, as well as the stringent requirements on phase accuracy of measurement instruments. Another practical problem is the large power capacity required of the drive source to achieve significant induction levels. A new resonant measurement setup, which we call the “virtual impedance” technique, is proposed as a solution to these problems. Its utility is demonstrated with measurements of a commercial composite core with permeability 14μ₀ whose low-core loss defeats conventional methods of measurement.     

Precipitates in electrical steels

Precipitates heavily influence the magnetic properties of electrical steels, either as a key controlled requirement as part of the manufacturing process or as an unwanted harmful residual in the final product. In this current work copper-manganese sulphides precipitates are the primary inhibitor species in the conventional grain-oriented (CGO) steels examined and grain boundary pinning is effective at a mean precipitate size of 30–70 nm. The growth of CuMnS has been studied and the results show that a precipitate size above ∼100 nm allows the onset of secondary recrystallisation in the heating conditions applied.     

A comparative study of the physical properties of Sb2S3 thin films treated with N2 AC plasma and thermal annealing in N2

As-deposited antimony sulfide thin films prepared by chemical bath deposition were treated with nitrogen AC plasma and thermal annealing in nitrogen atmosphere. The as-deposited, plasma treated, and thermally annealed antimony sulfide thin films have been characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy, scanning electron microscopy, atomic force microscopy, UV-vis spectroscopy, and electrical measurements. The results have shown that post-deposition treatments modify the crystalline structure, the morphology, and the optoelectronic properties of Sb₂S₃ thin films. X-ray diffraction studies showed that the crystallinity of the films was improved in both cases. Atomic force microscopy studies showed that the change in the film morphology depends on the post-deposition treatment used. Optical emission spectroscopy (OES) analysis revealed the plasma etching on the surface of the film, this fact was corroborated by the energy dispersive X-ray spectroscopy analysis. The optical band gap of the films (E_g) decreased after post-deposition treatments (from 2.36 to 1.75 eV) due to the improvement in the grain sizes. The electrical resistivity of the Sb₂S₃ thin films decreased from 10⁸ to 10⁶ Ω-cm after plasma treatments.     

Magnetic losses evolution of a semi-processed steel during forced aging treatments

An ultra-low carbon steel (30 ppm after decarburization) containing Al and Si was aged for distinct soaking times at 210 °C. The core loss increased continuously until around 24 h. After that, only slight changes were verified. It was found that only the hysteresis loss component changed during the aging treatment. By internal friction test and transmission electron microscopy it was seen that carbon precipitation caused the magnetic aging. By scanning electron microscopy it could be concluded that the increase of aging index was attributed to the high number of carbides larger than 0.1 μm.