Development of a new generation of high permeability non-oriented silicon steels

The paper describes a new generation of the high permeability fully processed silicon steel grades developed by Acesita, with core loss (W_1.5/60) in range of 3.10–4.20 W/kg and polarisation (J₅₀) from 1.71 to 1.75 T, respectively. The new grades have lower (Si+Al) content and a better crystallographic texture, with lower fractions of [1 1 1]||ND fibre and higher fractions of [0 0 1]||RD fibre. The new grades have better mechanical and magnetic properties than conventional grades.     

The influence of shear bands on final structure and magnetic properties of 3% Si non-oriented silicon steel

The presence of shear bands in the deformed material before final annealing is very important for Goss and Cube textures formation in silicon steel [S.C. Paolinelli, M.A. Cunha, J. Magn. Magn. Mater. 255 (2003) pp. 379. [1]; J.T. Park, J.A. Szpunar, Acta Mater., 51 (2003) 3037. [2]]. The increase of the hot-band grain size can increase the number of shear bands, which favor the nucleation of these orientations. In this work, the effect of the hot band grain size variation, promoted by varying the hot rolling finishing temperature, on final structure and magnetic properties was investigated for 3% Si alloy. It was found that the increase of the hot-band grain size increases the occurrence of shear bands and promotes an increase of η fiber fraction and a reduction of γ fiber fraction, improving the magnetic induction. On the other hand, the final grain size is reduced when the hot-band grain size is larger than 190 μm, deteriorating the core loss values in spite of the texture benefits. The reduction of final grain size was explained by the increase of the number of nuclei at the beginning of the recrystallization caused by the increase of shear bands in the deformed material.     

Influence of thermomechanical processing on shear bands formation and magnetic properties of a 3% Si non-oriented electrical steel

The effect of thermomechanical processing on the formation of shear bands and on the magnetic properties of a 3.0 wt% silicon non-oriented steel was investigated by hot rolling samples with different thicknesses at different temperatures, in order to obtain a variation in hot band grain size and cold strain. All the samples were processed in a single-stage cold rolling and finally annealed at 1020 °C. It was found that the increase of the hot band grain size decreases the γ fiber volume fraction and increases the η fiber volume fraction after the final annealing. The increase of the cold strain strongly contributed to this result. A good combination of intense generation of shear bands, and proper crystallographic texture, due to higher nucleation of grains with favorable orientations to magnetization in these bands, can be obtained for the samples hot rolled at 1000 and 1120 °C and submitted to cold strain of 64.3% and 72.2% respectively. However the best combination of B₅₀, W_15/60 and μ_r can be obtained by hot rolling the samples at 1000 °C to the thickness of 1.4 mm, corresponding to 64.3% of cold strain.     

Effect of annealing prior to cold rolling on magnetic and mechanical properties of low carbon non-oriented electrical steels

The effects of annealing prior to cold rolling on the microstructure, magnetic and mechanical properties of low-C grain non-oriented (GNO) electrical steels have been investigated. The grain structure of hot-rolled electrical steel strips is modified by annealing at temperatures between 700 and 1050 °C. Annealing at temperatures less than the ferrite to austenite+ferrite transformation temperature on heating (Ac₁) causes a marginal effect on the grain size. However, annealing in the intercritical region at temperatures between Ac₁ and Ac₃ (the ferrite+austenite to austenite transformation temperature on heating) causes rapid decarburization and development of large columnar ferrite grains free of carbide particles. This microstructure leads, after cold rolling and a fast annealing treatment, to carbide free, large ferrite grain microstructures with magnetic and mechanical properties superior to those observed typically in the same steel in the industrially fully processed condition. These results are attributed to the increment in grain size and to the {1 0 0} fiber texture developed during the final annealing at temperatures up to 850 °C. Annealing at higher temperatures, T>Ac₃, results in a strong {1 1 1} fiber texture and an increase of the quantity of second phase particles present in the microstructure, which lead to a negative effect on the final properties. The results suggest that annealing prior to cold rolling offers an attractive alternative processing route for the manufacture of fully processed low C GNO electrical steels strips.     

Modelling magnetic polarisation J50 by different methods

Two different methods for modelling the angular behaviour of magnetic polarisation at 5000 A/m (J₅₀) of electrical steels were evaluated and compared. Both methods are based upon crystallographic texture data. The texture of non-oriented electrical steels with silicon content ranging from 0.11 to 3%Si was determined by X-ray diffraction. In the first method, J₅₀ was correlated to the calculated value of the average anisotropy energy in each direction, using texture data. In the second method, the first three coefficients of the spherical harmonic series of the ODF and two experimental points were used to estimate the angular variation of J₅₀. The first method allows the estimation of J₅₀ for samples with different textures and Si contents using only the texture data, with no need of magnetic measurement, and this is advantageous, because texture data can be acquired with less than 2 g of material. The second method may give better adjust in some situations but besides the texture data, it requests magnetic measurements in at least two directions, for example, rolling and transverse directions.     

Preparation of non-oriented silicon steel with high magnetic induction using columnar grains

Columnar grains can lead to detrimental surface ridging and an inhomogeneous microstructure, although their {1 0 0}〈0 v w〉 texture is considered desirable due to their good magnetic properties in non-oriented silicon steel. Based on the hereditary tendency of {1 0 0}〈0 v w〉 texture, the effects of lubrication and heating rate on texture and on final magnetic properties were investigated using a cast slab containing 100% columnar grains. Hot rolling with lubrication, normalization at low heating rate, two-stage cold rolling, and final annealing at 1000 °C helped achieve high performance. As a result, a new non-oriented silicon steel with high magnetic induction (B₅₀=1.82 T) and low core loss (P_1.5=2.35 W/kg) was prepared. The possibility of further performance optimization was also discussed.     

Pre-annealing and magnetic induction in inhibitor-free 3% Si–Fe strips

Effects of pre-annealing and hydrogen flow rate on final texture and magnetic induction have been investigated in inhibitor-free 100 μm thick 3% Si–Fe strips containing 18 ppm sulfur. Without any pre-annealing, the strip showed a low magnetic induction, due to various {1 1 0}, {1 0 0} and {1 1 1} final texture components. The number and the area fraction of {1 1 0} grains increased with increasing pre-annealing temperature and hydrogen flow rate. A pre-annealing temperature range that results in the sharp {1 1 0} 〈0 0 1〉 texture is observed, depending on the hydrogen flow rate.     

Effects of sulfur content and slab reheating temperature on the magnetic properties of fully processed nonoriented electrical steels

The effects of sulfur content and slab reheating temperature on the magnetic properties of four fully processed nonoriented electrical steels have been investigated. Four slabs of nonoriented electrical steels with sulfur content in the range of 0.0006–0.0126 wt% were reheated to 1100, 1200, and 1300 °C, respectively. Then, they were hot rolled and annealed at 700 °C, cold rolled at the same condition and annealed at 820 °C in the salt bath furnace for 1 min to simulate continuous annealing. The ac core loss, dc hysteresis loss, and ac and dc permeability were measured at 15 kG inductions. It was found that the amount of inclusions in the hot-rolled bands increased with increasing slab reheating temperature and increasing sulfur content in steels. After final annealing, grain sizes of cold-rolled steel sheets decreased with increasing sulfur content and increasing slab reheating temperature. The main preferred orientations in the final annealed steel sheets were (0 1 1) 〈1 0 0〉 and (1 1 1) 〈u v w〉 γ fiber texture. Steel sheets containing 0.0032 and 0.0060 wt% sulfur developed a more stronger (0 1 1)〈1 0 0〉 texture than other steel sheets. However, steel sheets containing 0.0126 wt% sulfur had the weakest (1 1 1)〈u v w〉 texture during slab reheating at temperatures higher than 1200 °C. Both ac core loss and dc hysteresis loss increased with increasing slab reheating temperature and increasing sulfur content in steel sheets. Both ac and dc permeability decreased with increasing slab reheating temperature and increasing sulfur content in steel sheets. If sulfur content decreased from 0.0060 to 0.0032 wt%, there were great improvements in ac core loss, dc hysteresis loss, and ac and dc permeability. However, eddy current loss was almost independent of the sulfur content and slab reheating temperature.     

Effective biaxial modulus and strain energy density of ideally (h k l)-fiber-textured cubic polycrystalline films

The effective biaxial modulus (M_eff) and strain energy density (W) of cubic polycrystalline films with ideally (h k l) fiber textures are estimated using Vook-Witt (VW) grain interaction model and the data are compared with those derived from Voigt, Reuss and Voigt-Reuss-Hill (VRH) models. Numerical results show that the VW average of M_eff for ideally (1 0 0)- or (1 1 1)-fiber-textured films is identical to the VRH average of M_eff. For (1 1 0) and (1 1 2) planes, however, the VW average of M_eff for (1 1 0)-fiber-textured film is larger than that of (1 1 2)-fiber-textured film when the Zener anisotropic factor (A_R) is not equal to 1. Furthermore, M_eff and W exhibit incremental tendencies with the increase of the orientation factor (Γ_h k l) for the [h k l] axis when A_R > 1, implying that M_eff and W have the minimums on the (1 0 0) plane. Reversely, M_eff and W decrease with the increasing Γ_h k l when A_R < 1. This means that M_eff and W on (1 1 1) plane have the minimums.     

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.     

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.     

Magnetic properties of spray-formed Fe–6.5%Si and Fe–6.5%Si–1.0%Al after rolling and heat treatment

The maximum silicon content in commercial Fe–Si steels is limited to about 3.5 wt%Si, since the ductility declines sharply as this maximum is exceeded, hindering the production of thin sheets by cold/hot rolling. However, the best magnetic properties are attained at about 6.5 wt%Si, a silicon content that renders magnetostriction practically null and minimizes magnetic losses. Using spray-forming, our research group has successfully produced this type of high silicon alloy in thin sheet form by carefully controlling the many variables of the process and subsequent rolling operations. In the present study, we investigated the magnetic properties and the microstructure of spray-formed Fe–6.5 wt%Si and Fe–6.5 wt%Si–1.0 wt%Al alloys after warm rolling and heat treatment. The main cause for the brittleness of Fe–6.5 wt%Si alloy has been attributed to the B2 phase long-range ordering, which leads to premature fractures. The presence of aluminum could avoid B2 formation and improve the alloy's ductility. The binary Fe–6.5 wt% Si alloy showed the best magnetic properties, which were ascribed to a recrystallized, coarse grain size (∼500 μm; and 340 μm for the Al-containing alloy). TEM analysis showed that a well-developed B2 domain structure (about 50–300 nm in size) was formed in the binary alloy when low cooling rates are prevailing after heat treatment. This structure contributed to improve additionally the magnetic properties, but its effect was not so strong as that of the grain size. The addition of Al to the binary alloy suppressed B2 formation, as indicated by Mossbauer spectroscopy, and apparently hindered excessive grain growth, which may explain the slightly poorer magnetic properties when compared with the binary alloy.     

The effect of growth ambient on the structural and optical properties of MgxZn1−xO thin films

Mg_xZn_1−xO (x = 0.0-0.20) thin films have been deposited by sol-gel technique on glass substrates and the effect of growth ambient (air and oxygen) on the structural, and optical properties have been investigated. The films synthesized in both ambient have hexagonal wurtzite structure. The c-axis lattice constant decreases linearly with the Mg content (x) up to x = 0.05, and 0.10 respectively for air- and oxygen-treated films, above which up to x = 0.20, the values vary irregularly with x. The change in the optical band gap values and the ultraviolet (UV) peak positions of Mg_xZn_1−xO films show the similar change with x. These results suggest that the formation of solid solution and thus the structural and optical properties of Mg_xZn_1−xO thin films are affected by the growth ambient.     

Strain-induced grain growth in non-oriented electrical steels

The present work considers a method of columnar microstructure development in vacuum-degassed non-oriented electrical steels. Samples after temper rolling were annealed under special heat treatment conditions. The influence of the applied thermo-mechanical treatments on microstructure progress in the investigated non-oriented steels is studied. Columnar microstructure is obtained after combining the temper rolling and appropriate annealing conditions. The dependence of texture on the applied conditions was studied by EBSD facilities in the investigated material. It was confirmed that the obtained columnar microstructure possesses pronounced cube texture components.     

Deformation-induced texture in nanocrystalline 2:17, 1:5 and 2:7 Sm-Co magnets

The effect of crystal structures on texture induced by hot plastic deformation was studied for Sm-Co, Sm-Zr-Co, Sm-Zr-Co-Fe and Sm-Co-Fe-Mn nanocrystalline alloys with 9-22 at% Sm. Nanocrystalline precursors were obtained via high-energy ball milling and subsequent hot consolidation; deformation was carried out at 800-1150 °C. The analysis of X-ray diffraction and magnetic measurements showed that the degree of the axial [0 0 1] texture after deformation was negligible for the ordered 2:17 structure, but became increasingly noticeable for the disordered 2:17 (“1:7”), 1:5 and 2:7 structures. Because of interplay of several factors including the [0 0 1] texture, saturation magnetization and magnetocrystalline anisotropy, there was no universal trend in the hard magnetic properties with the Sm content. Optimum compositions for the maximum energy product varied from Sm₁₁(Co, Fe, Mn)₈₉ in the Sm-Co-Fe-Mn series to Sm₁₁Zr₂(Co, Fe)₈₇ in the Sm-Zr-Co-Fe series to Sm₁₇(Co, Fe)₈₃ in the Sm-Co-(Fe) series. Iron substitution for cobalt strongly suppresses the 1:5 structure, whereas the Fe-free magnets based on the SmCo₅ compound showed by far the highest room-temperature coercivity.     

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.     

Interactive contribution of grain size and grain orientation to coercivity of melt spun ribbons

During melt spinning process, the improvement of certain grain orientation and the refinement of grain size with surface velocity have interactive and contradictory effects on the magnetic properties. The contributions of these effects have seldom been taken into account and they were discussed in this paper via Fe-2, 4, 6.5 wt% Si alloys. Heat treatment at 1173 K for 1 h was performed to show the annealing impact. The X-ray diffraction patterns show that the high surface velocity and heat treatment increase the intensity ratio of line (2 0 0) to (1 1 0) of A2 phase. The (2 0 0) line corresponds to (2 0 0) plane in 〈0 0 1〉 direction, easy magnetization direction of α-Fe phase in Fe-Si alloy. The improvement of this grain orientation with the surface velocity decreases the coercivity, which should increase due to the grain refinement. It is revealed that the 〈0 0 1〉 texture promoted by the anisotropic heat release during melt spinning process is one factor to improve the magnetic properties and should be considered when preparing soft magnetic materials.     

Structural and photo-luminescence properties of nanocrystalline silicon films deposited at low temperature by plasma-enhanced chemical vapor deposition

Nanocrystalline silicon (nc-Si) films were prepared by a plasma-enhanced chemical vapor deposition method at a deposition temperature below 220 °C with different dynamic pressures (P_g), hydrogen flow rates ([H₂]), and RF powers, using SiH₄/H₂/SiF₄ mixtures. We examined the photo-luminescence (PL) spectra and the structural properties. We observed two stronger and weaker PL spectra with a peak energies around E_PL = 1.8 and 2.2-2.3 eV, respectively, suggesting that the first band was related to nanostructure in the films, and another band was associated with SiO-related bonds. The nc-Si films with rather large PL intensity was obtained for high [H₂] and/or low pressure values, However, effects of [H₂] are likely to be different from those of P_g. The average grain size (δ) and the crystalline volume fraction (ρ) at first rapidly increase, and then slowly increase, with increasing P_g. Other parameters exhibited opposite behaviors from those of δ or ρ. These results were discussed in connection with the changes in the PL properties with varying the deposition conditions.     

Fiber laser annealing of nanocrystalline PZT thick film prepared by aerosol deposition

Nanocrystalline PZT thick films (1 mm square and over 10 μm thick) directly deposited onto stainless-steel substrates (PZT/SUS) by aerosol deposition (AD) technique and then annealed using focused laser beam with a fiber laser to suppress thermal damage to the back sides of the PZT/SUS and substrate near the film edge and to retain the dielectric and/or ferroelectric properties of the PZT/SUS. Compared with CO₂ laser annealing, fiber laser annealing suppressed thermal damage to the substrate. Compared with PZT/SUS annealed at 600 °C using an electric furnace, PZT/SUS annealed at 600 °C using a fiber laser showed superior properties, namely, dielectric constant ? > 1200 at a frequency of 100 Hz, remanent polarization P_r > 30 μC/cm², and coercive field strength E_c < 50 kV/cm at a frequency of 10 Hz. Furthermore, the grain growth for the PZT/SUS formed by AD technique and annealed by fiber laser irradiation was occurred within the laser spot size.     

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.