Overview of Microstructure and Microtexture Development in Grain-oriented Silicon Steel

This paper outlines the development of the microstructure and microtexture of grain-oriented silicon steel during the industrial production process. In particular the evolution of the Goss orientation was studied in industrial material as well as in single crystal experiments.     

Effect of nitriding on grain oriented silicon steel bearing aluminum (the second study)

All kinds of high-permeability GO are manufactured using AlN as the main inhibitor. From a purely metallurgical viewpoint, three types of inhibitor preparation for high-permeability GO have been shown. They include a complete solution without nitriding, a complete precipitation with nitriding and a partial precipitation with nitriding. In this study, another possibility, i.e., a complete solution method with nitriding, was investigated to avoid the extra high-temperature slab reheating and to examine the effect of nitriding on GO bearing Al. This method can also provide the sharp Goss texture, and nitriding is shown to be very useful for changing the inhibitor intensity, depending on the primary grain size.     

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.     

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.     

Effect of stress relief annealing temperature and atmosphere on the magnetic properties of silicon steel

Fully processed non-oriented silicon steel samples 0.50 mm thick were sheared and submitted to stress relief annealing under different conditions of temperature and atmosphere to investigate the effect of this treatment on the recovery of magnetic properties. Two different compositions were used, with different Si and Al contents. Temperature was varied in the range of 600–900 °C and four atmospheres were used: N₂ and N₂+10%H₂ combined with dew points of −10 and 15 °C. The results showed that annealing atmosphere has very important effect on the magnetic properties and that the beneficial effect of stress relief annealing can be overcome by the detrimental effect of the atmosphere under certain conditions, due to oxidation and nitration.     

Iron disilicide formation by Au-Si eutectic reaction on Si substrate

We have investigated the growth of iron disilicide on Au-coated Si(0 0 1) substrates and its photoluminescence behaviour. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy observations revealed that the Si surface above 380 °C was melted as a result of the Au-Si eutectic reaction and that coarse island disilicide grains with sizes of several micrometres were formed on the Si surface. The full width at half maximum of 0.056° on the rocking curve of α-FeSi₂004 was observed on the sample deposited at 800 °C, and indicated the high crystal quality in perfection of orientation. The photoluminescence spectrum of β-FeSi₂ grains, which were deposited at 750 °C, was observed. The melted Si surface contributed to the improved crystallinity of α-FeSi₂ and β-FeSi₂.     

Novel approaches to high-density perpendicular recording media

Two different approaches to reduce the intermediate layer (IL) thickness in perpendicular recording media are proposed. Such a reduction in IL thickness could lead to improvement in writability and recording performance. The first approach involved the introduction of a magnetic intermediate layer (MIL), to obtain C-axis growth. Media with CoCr alloy layer as the MIL were studied. Reasonably good C-axis growth with a Δθ₅₀ of about 3.8° could be obtained for MIL thickness of about 10 nm. Noise could be controlled by introducing exchange-breaking layers. The other approach involved the use of crystalline soft underlayers (SUL) to obtain suitable growth conditions for the recording layers. For this purpose, CoFeTaCr alloys with a FCC(1 1 1) texture were prepared. A good C-axis dispersion in the recording layer with a Δθ₅₀ of about 3.1° could be obtained for IL thickness of about 5 nm. The present study indicates that the recording medium deposited on crystalline SUL is relatively noisier than that deposited on amorphous SUL. Reducing the noise of the crystalline SUL is a way towards higher areal densities.     

Production for high thermal stability NdFeB magnets

To improve sintered NdFeB magnets’ thermal stability and magnetic properties, combined addition of elements Cu and Gd was investigated. It was found that with Gd addition increase to 1.0%, the temperature coefficient α improved from −0.15 to −0.05%/°C (maximum working temperature 120 °C), but the remanence and the maximum energy product linearly decreased. With addition of Cu in Gd-containing magnets the intrinsic coercivity increased greatly, and the remanence increased also because of their density improvement, and optimum Cu content was achieved at 0.2%. Microstructure analysis showed that most of the Cu distributed at grain boundaries and led to clear and smooth morphologies. Magnets with high thermal stability α=−0.05%/°C and magnetic properties were obtained with addition of Gd=0.8% and Cu=0.2%.     

Influence of substrate temperature on the optical and piezoelectric properties of ZnO thin films deposited by rf magnetron sputtering

In this study, ZnO thin films were fabricated using the rf magnetron sputtering method and their piezoelectrical and optical characteristics were investigated for various substrate temperatures. The ZnO thin film has the largest crystallization orientation for the (0 0 2) peak and the smallest FWHM value of 0.56° at a substrate temperature of 200 °C. The surface morphology shows a relatively dense surface structure at 200 °C compared to the other substrate temperatures. The surface roughness shows the smallest of 1.6 nm at a substrate temperature of 200 °C. The piezoelectric constant of the ZnO thin film measured using the pneumatic loading method (PLM) has a maximum value of 11.9 pC/N at a substrate temperature of 200 °C. The transmittance of the ZnO thin film measured using spectrophotometry with various substrate temperatures ranged from 75 to 93% in the visible light region. By fitting the refractive index from the transmittance to the Sellmeir dispersion relation, we can predict the refractive index of the ZnO thin film according to the wavelength. In the visible light range, the refraction index of the ZnO thin film deposited at a substrate temperature of 200 °C is the range of 1.88-2.08.     

On the thermal stability of Co2Z hexagonal ferrites for low-temperature ceramic cofiring technologies

Co₂Z hexaferrite Ba₃Co₂Fe₂₄O₄₁ was prepared by a mixed oxalate co-precipitation route and the standard ceramic technology. XRD studies show that at T<1300 °C different ferrite phases coexist with the M-type hexaferrite as majority phase between 1000 and 1100 °C and the Y-type ferrite at 1230 °C. The Z-type material has its stability interval between 1300 and 1350 °C. Both synthesis routes result in almost single-phase Z-type ferrites after calcination at 1330 °C, intermediate grinding and sintering at 1330 °C. The permeability of Co₂Z-type ferrite of about μ=20 is stable up to several 100 MHz, with maximum losses μ′′ around 700 MHz. Addition of 3 wt% Bi₂O₃ as sintering aid shifts the temperature of maximum shrinkage down to 950 °C and enables sintering of Z-type ferrite powders at 950 °C. However, the permeability is reduced to μ=3. It is shown here for the first time that Co₂Z ferrite is not stable under these conditions; partial thermal decomposition into other hexagonal ferrites is found by XRD studies. This is accompanied by a significant decrease of permeability. This shows that Co₂Z hexagonal ferrite is not suitable for the fabrication of multilayer inductors for high-frequency applications via the low-temperature ceramic cofiring technology since the material is not compatible with the typical process cofiring temperature of 950 °C.     

Influence of cold-rolling texture and heating rate on {1 1 0}〈0 0 1〉 development in inhibitor-free 3%Si–Fe sheets

This paper presents cold-rolling and annealing methods to obtain a high-magnetic induction in inhibitor-free 0.1-mm-thick 3% silicon–iron sheets containing 18 or 150 ppm sulfur. In case of the two-step cold-rolling, the sheets containing 150 ppm sulfur showed a strong {1 0 0} final texture at 400 °C/h, and some fraction of {1 1 0} component was observed at 25 °C/h. However, three-step cold-rolling resulted in a sharp {1 1 0}〈0 0 1〉 final texture at 25 °C/h. This is due to the difference in intensity ratio of {1 0 0}〈0 1 1〉 to {1 1 1}〈1 1 2〉 in the cold-rolling texture which influences the nucleation of {1 1 0}〈0 0 1〉 component and the selective growth kinetics of various grains. In case of 18 ppm sulfur, the final texture was mainly composed of a sharp {1 1 0}〈0 0 1〉 component even at 400 °C/h, due to the relatively low segregation concentration.     

Structural and optical characterization of Ce-doped Gd2SiO5 films by sol-gel technique

Cerium-doped Gd₂SiO₅ (GSO:Ce) films have been prepared on (1 1 1) silicon substrates by the sol-gel technique. Annealing was performed in the temperature range from 400 to 1000 °C. X-ray diffraction (XRD), and atomic force microscopy (AFM) were used to investigate the structure and morphology of GSO:Ce films. Results showed that GSO:Ce film starts to crystallize at about 600 °C, GSO:Ce films have a preferential (0 2 1) orientation, as the annealing temperature increase, the (0 2 1) peak intensity increases, the full width of half maximum (FWHM) decreases, and the grain size of GSO:Ce films increases. Emission spectra of GSO:Ce films were measured, results exhibit the characteristic blue emission peak at 427 nm.     

Effect of substrate temperature on the growth of ITO thin films

Indium tin oxide (ITO) thin films were deposited onto glass substrates by rf magnetron sputtering of ITO target and the influence of substrate temperature on the properties of the films were investigated. The structural characteristics showed a dependence on the oxygen partial pressure during sputtering. Oxygen deficient films showed (4 0 0) plane texturing while oxygen-incorporated films were preferentially oriented in the [1 1 1] direction. ITO films with low resistivity of 2.05 × 10⁻³ Ω cm were deposited at relatively low substrate temperature (150 °C) which shows highest figure of merit of 2.84 × 10⁻³ square/Ω⋅     

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.     

High resistive ferrite films by a solution process for electromagnetic compatible (EMC) devices

Mn-Zn ferrite films with high resistivity and good noise suppressing ability for use as ‘coupling-type noise suppressors’ have been prepared by the spin-spray ferrite plating. The as-prepared films were crystalline and exhibited single-phase spinel structure. The films had an ‘integrated nano-columnar’ morphology that resulted in a very high resistivity. Further, by varying the chemical composition, films with varying resistivity were prepared and then heat treated at 260 °C for 3 min, similar to that of the reflow soldering process. The reflection and transmission coefficients, S₁₁ and S₂₁ parameters, on coplanar micro-strip line (50 Ω) were measured for the as-prepared and heat-treated films in order to study the effect of heat treatment. When the resistivity was above 2×10⁵ Ω/sq, S₁₁ and S₂₁ exhibited uniform profiles throughout the measurement frequency (50 MHz-10 GHz), which is ideal for the ‘coupling-type’ noise suppressor. These films retain a moderately high resistivity and hence do not show the downshift in the stopband frequency even after the heat treatment (reflow soldering process).     

On the Steinmetz hysteresis law

The behavior of the Steinmetz coefficient has been described for several different materials: steels with 3.2% Si and 6.5% Si, MnZn ferrite and Ni–Fe alloys. It is shown that, for steels, the Steinmetz law achieves R²>0.999 only between 0.3 and 1.2 T, which is the interval where domain wall movement dominates. The anisotropy of Steinmetz coefficient for non-oriented (NO) steel is also discussed. It is shown that for a NO 3.2% Si steel with a strong Goss component in texture, the power law coefficient and remanence decreases monotonically with the direction of measurement going from rolling direction (RD) to transverse direction (TD), although coercive field increased. The remanence behavior can be related to the minimization of demagnetizing field at the surface grains. The data appear to indicate that the Steinmetz coefficient increases as magnetocrystalline anisotropy constant decreases.     

Amorphous to crystalline phase transition in pulsed laser deposited silicon carbide

SiC thin films were grown on Si (1 0 0) substrates by excimer laser ablation of a SiC target in vacuum. The effect of deposition temperature (up to 950 °C), post-deposition annealing and laser energy on the nanostructure, bonding and crystalline properties of the films was studied, in order to elucidate their transition from an amorphous to a crystalline phase. Infra-red spectroscopy shows that growth at temperatures greater than 600 °C produces layers with increasingly uniform environment of the Si-C bonds, while the appearance of large crystallites is detected, by X-ray diffraction, at 800 °C. Electron paramagnetic resonance confirms the presence of clustered paramagnetic centers within the sp² carbon domains. Increasing deposition temperature leads to a decrease of the spin density and to a temperature-dependent component of the EPR linewidth induced by spin hopping. For films grown below 650 °C, post-deposition annealing at 1100 °C reduces the spin density as a result of a more uniform Si-C nanostructure, though large scale crystallization is not observed. For greater deposition temperatures, annealing leads to little changes in the bonding properties, but suppresses the temperature dependent component of the EPR linewidth. These findings are explained by a relaxation of the stress in the layers, through the annealing of the bond angle disorder that inhibits spin hopping processes.     

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.     

A three-phase single sheet tester with digital control of flux loci based on the contraction mapping principle

Tight control of flux loci in 2D testing of soft magnetic laminations is realized by a method based on the principle of contraction mapping. It is implemented through digital control of the currents supplying a three-phase yoke magnetizer and the use of circular samples. Faithful realization of the prescribed loci and good measuring accuracy are demonstrated in grain-oriented and non-oriented Fe–Si laminations.     

Magnetic properties of the ferrimagnetic glass-ceramics for hyperthermia

Magnetic materials play a key-role in magnetic induction hyperthermia for the treatment of cancer. In this paper, we analyse the magnetic properties of ferrimagnetic glass-ceramics with the composition in the system SiO₂–Na₂O–CaO–P₂O₅–FeO–Fe₂O₃, as a function of the melting temperature. These materials were obtained by melting of commercial reagents in the temperature range of 1400–1550 °C. Room-temperature magnetic measurements were performed by means of a vibrating sample magnetometer at room temperature. The power loss was determined from calorimetric measurements, using a magnetic induction furnace. The highest power loss (61 W/g) has been obtained for samples melted at 1500 °C. The heat generation of the ferrimagnetic glass-ceramics prepared by two different synthesis methods (traditional melting and coprecipitation-derived) will be compared. These materials are expected to be useful in the localised treatment of cancer.