Analysis of oxide layer structure in nitrided grain-oriented silicon steel

The production of low-temperature reheated grain-oriented silicon steel is mainly based on the acquired inhibitor method.Due to the additional nitriding process,a high nitrogen content exists in the oxide layer,which changes the structure of the oxide layer.In this study,the structure of the surface oxide layer after nitriding was analyzed by scanning electron microscopy(SEM),electron back-scattered diffraction(EBSD),glow discharge spectrometry(GDS),and X-ray diffraction(XRD).The size and orientation of ferritic grains in the oxide layer were characterized,and the distribution characteristics of the key elements along the thickness direction were determined.The results show that the oxide layer of the steel sample mainly comprised particles of Fe2SiO4 and spherical and lamellar SiO2,and Fe4N and fcc-Fe phases were also detected.Moreover,the size and orientation of ferritic grains in the oxide layer were different from those of coarse matrix ferritic grains beneath the oxide layer;however,some ferritic grains exhibited same orientations as those in the neighboring matrix.Higher nitrogen content was detected in the oxide layer than that in the matrix beneath the oxide layer.The form of nitrogen enrichment in the oxide layer was analyzed,and the growth mechanism of ferritic grains during the oxide layer formation is proposed.

Model Transformer Evaluation of High-Permeability Grain-Oriented Electrical Steels

The dependence of transformer performance on the material properties was investigated using two laboratory-processed 0.23 mm thick grain-oriented electrical steels domain-refined with elec-trolytically etched grooves having different magnetic properties. The iron loss at 1.7 T, 50 Hz and the flux density at 800 A/m of material A were 0.73 W/kg and 1.89 T, respectively; and those of material B, 0.83 W/kg and 1.88 T. Model stacked and wound transformer core experiments using the tested materials exhibited performance well reflecting the material characteristics. In a three-phase stacked core with step-lap joints excited to 1.7 T, 50 Hz, the core loss, the exciting current and the noise level were 0.86 W/kg, 0.74 A and 52 dB, respectively, with material A; and 0.97 W/kg, 1.0 A and 54 dB with material B. The building factors for the core losses of the two materials were almost the same in both core configurations. The effect of higher harmonics on transformer performance was also investigated.

Simulation of recrystallization based on EBSD data using a modified Monte Carlo model that considers anisotropic effects in cold-rolled ultra-thin grain-oriented silicon steel

A Monte Carlo Potts model was developed to simulate the recrystallization process of a cold-rolled ultra-thin grain-oriented silicon steel.The orientation and image quality data from electron backscatter diffraction measurements were used as input information for simulation.Three types of nucleation mechanisms,namely,random nucleation,high-stored-energy site nucleation(HSEN),and high-angle boundary nucleation(HABN),were considered for simulation.In particular,the nucleation and growth behaviors of Goss-oriented({011}<100>)grains were investigated.Results showed that Goss grains had a nucleation advantage in HSEN and HABN.The amount of Goss grains was the highest according to HABN,and it matched the experimental measurement.However,Goss grains lacked a size advantage across all mechanisms during the recrystallization process.

Fabrication of Grain-oriented (Bi,Pb)_2Sr_2Ca_2Cu_3O_x Superconducting Tapes Using Magnetic Field and Vibration Technique

Highly textured (Bi,Pb)2Sr2Ca2Cu3Ox superconducting tapes have been fabricated by means of magnetic-field and vibration technique. This method is an effective way of improving the degree of grain alignment and density of oxide core in tapes after heat treatment and pressing cycles.Jc of above 20% was increased than that without treatment.

Effect of Ball Scribing on Power Loss Separation of Fe-3%Si Grain-oriented Silicon Steel

Power loss of Fe-3%Sigrain-oriented silicon steelwas measured after ballscribing with different spacing using a self-designed tool.Three different sections of power loss,including hysteresis loss,abnormalloss,and eddy current loss,were measured and calculated,respectively.The loss variation and ratio were analyzed based on the experimentaldata.At 1.0 T,hysteresis loss of tested steelwith scribing spacing of 8 mm descends by 8.2% compared to samples without scribing,which is similar to the totalloss variation,and abnormalloss descends by 16.8%.At 1.0 T,hysteresis loss ratio of the steelwith scribing spacing of 16 mm ascends from 55.7% to 57.9%,and eddy current loss increases from 17.4% to 24.1%,while abnormalloss descends from 26.9% to 23.7%.The experimentalresults show that the reduction of power loss after scribing is mainly due to decreasing of hysteresis loss and abnormalloss.

Morphologies and Influential Factors of Forsterite Film in Grain-Oriented Silicon Steel

The product quality of graiworiented silicon steel may be affected by each process because of its complicat- ed production technology. Morphologies, compositions and structures of forsterite film formed in different conditions on the samples subjected to high temperature annealing were measured by using a scanning electron microscope, an energy disperse spectroscope, an X ray diffractometer and Fourier transform infrared technique respectively. The morphologies and influential factors of forsterite film were investigated. The results showed that the major compo- nent of forsterite film composed of light-gray spherical particles was Mg2 SiO4, and the minor was MgAl2O4. If the amount of MgO coated on the surface of the steel was less, bare holes or even large-scale bare grains for forsterite film appeared. The higher temperature of water bath during decarburization annealing led to gaps of strips in forster ite film. Moreover, MgO coating method had great influence on forsterite film. Roller coating method was beneficial to increase compactness and smoothness of forsterite film, but was disadvantageous to its thickness.

Correlation between Primary and Secondary Recrystallization Texture Components in Low-temperature Reheated Grain-oriented Silicon Steel

Low-temperature slab-reheated grain-oriented silicon steel is characterized by a sharp {411}〈148〉 primary recrystallization texture. To date, the influence of this texture on secondary recrystallization is not clear. Microtextures in primary and secondary reerystallized sheets of low-temperature reheated grain-oriented silicon steel were examined using electron backscatter diffraction. By comparing the textures and microstructures of specific primary reerystallized grains neighboring secondary grains with those of other primary grains, the influences of primary re- crystallization textures and microstructures on the orientations of secondary grains were investigated. Results show that for low-temperature reheated graiworiented silicon steel, the primary recrystallization sheet comprises { 411 } 〈148〉, {111}〈112〉, and {001}〈120〉 texture componems. During secondary recrystallization, the {111}〈112〉 primary recrystallized grains were easily consumed by abnormally grown Goss, deviated Goss, Brass, or {210}〈001〉grains ;the { 411 }〈148〉 primary recrystallized grains were more resistant to being swallowed; and the {001} 〈120 grains were the most resistant to being consumed. For a particular primary grain, the distribution of its surrounding grain boundaries determined how easily it is consumed during secondary recrystallization. Primary grains surrounded by 20°- 45° grain boundaries were consumed much earlier than those having grain boundaries above 45°, which is in accordance with high-energy grain boundary theory. In addition, special ∑9 boundaries between {411}〈148〉 and Goss grains move more slowly than ∑9 boundaries between {111 }〈112〉 and Goss grains, which is attributed to the different positions of 〈110〉 rotation axis with respect to the normals of grain boundaries.

Effect of Initial Goss Texture Sharpness on Texture Evolution and Magnetic Properties of Ultra-thin Grain-oriented Electrical Steel

In this study, high- and low-grade grain-oriented electrical steels were used as the initial materials to produce 0.08-mm-thick sheet with one-step cold-rolling method. Electron backscattering diffraction analysis technique and X-ray diffraction texture analysis technique were adopted to investigate the effect of initial Goss texture sharpness on texture evolution and magnetic properties of ultra-thin grain-oriented electrical steel. The results showed that primary recrystal- lization and secondary recrystallization were the main processes that occurred during annealing. The induced factors for secondary recrystallization of two grades samples were not Consistent. The high-grade samples presented texture induction mechanism, while the low-grade samples revealed strong surface-energy induction mechanism. The initial Goss texture sharpness had a great impact on texture evolution and magnetic properties of ultra-thin grain-oriented electrical steel. The Goss texture component formed after primary recrystallization was stronger, and better magnetic properties were obtained at low frequencies. For low-grade samples, secondary recrystallization enhanced the intensity of Goss texture, and both grain size and texture contributed to better high-frequency magnetic properties after secondary recrystallization. By controlling the annealing process, the magnetic properties of low-grade products could be significantly improved, thus achieving conversion from low-grade to high-grade products.

Effects of Normalizing Annealing on Grain-oriented Silicon Steel

The grain-oriented silicon steel is a kind of important magnetic materials with low iron loss and high induc tion. Hot hand normalizing annealing is an important process which influences the microstructure and the development of the inhibitors. The effects of different annealing temperatures and cooling conditions on the inhibitors and microstructures of normalizing annealing band were investigated. The microstructure and different kinds of the inhibitors, i. e. , A1N, AIN＋Cu, S＋MnS, and TiN, were discovered. The result shows that a suitable cooling condition leads to more nano scale inhibitors and uniform microstructure of the normalizing annealing band and consequently results in better magnetic properties.

Microstructure,texture and precipitates of grain-oriented silicon steel produced by thin slab casting and rolling process

A grain-oriented silicon steel strip with AlN as main inhibitor was produced by thin slab casting and rolling（TSCR）process.The microstructure,texture and precipitates of the hot-rolled strip were investigated by use of optical microscope（OM）,X-ray diffractometer,transmission electron microscope（TEM）and energy dispersive spectroscope（EDS）.The result shows that the microstructure and texture exhibit a through-thickness gradient similar to that of the hot-rolled strip produced by conventional high-temperature slab-reheating process;the preferred orientation varies from {110}〈001〉in the surface layer to{001}〈110〉in the center layer,and the Goss texture with a maximum intensity mainly concentrates on the surface layer.In addition,some other texture components,for example rotated Goss texture,form in the 1/4thickness layer,which are not observed in the hotrolled strip produced by conventional high-temperature slab-reheating process.The precipitates in the hot-rolled strip are mainly（Mn,Cu）S and AlN compound particles with dimension of 100-200 nm,and the fine precipitates are significantly less than that in the hot-rolled strip produced by conventional high-temperature slab-reheating process.Moreover,the areal density of the fine precipitates in the center layer is more than that in the surface layer.

Formation mechanism of surface oxide layer of grain-oriented silicon steel

The surface oxide layer of grain-oriented electrical steels was investigated by scanning electron microscopy.The formation mechanism and the influence on the glass film of the surface oxide layer were analyzed by the calculation of thermodynamics and kinetics.The surface oxide layer with 2.3μm in thickness is mainly composed of SiO_(2),a small amount of FeO and Fe_(2)SiO_(4).During the formation of surface oxide layer,the restriction factor was the diffusion of O in the oxide layer.At the initial stage of the decarburization annealing,FeO would be formed on the surface layer.SiO_(2) and silicate particles rapidly nucleated,grew and formed a granular oxide layer in the subsurface.As the oxidation layer thickens,the nucleation of new particles decreases,and the growth of oxide particles would be dominant.A lamellar oxide layer was formed between the surface oxide layer and the steel matrix,and eventually formed a typical three-layer structure.During the high temperature annealing,MgO mainly reacted with SiO_(2) and Fe_(2)SiO_(4) in the surface oxide layer to form Mg2SiO_(4) and Fe_(2)SiO_(4) would respond first,thus forming the glass film with average thickness of 4.87μm.

Effect of Ball Scribing on Magnetic Barkhausen Noise of Grain-oriented Electrical Steel

Effect of ball scribing on magnetic Barkhausen noise （MBN） of conventional grain-oriented （CGO） and high- permeability grain-oriented （HGO） electrical steel was investigated. The results showed that after ball scribing, root mean square of MBN （MBNrms） of CGO electrical steel increased 9.8% with 4 mm scribing spacing at 1.2 T, and that of HGO electrical steel apparently decreased 17.3% with 16 mm scribing spacing at 1.2 T. Through the formation and development of free magnetic poles and secondary magnetic domains due to compressive stress, primary magnetic domain space of grain-oriented electrical steel becomes smaller, which reflects as a variation of MBN in the macroscopic magnetic properties. Through correlation formula derivation of MBNrms and equilibrium distance between domain walls, effect of domain refinement on grain-oriented electrical steel was also interpreted, and optimum equilibrium distance between domain walls was determined.

Abnormal Growth of Goss Grains in Grain-oriented Electrical Steels

With the help of electron back scattering diffraction techniques and field emission microscope, the misorienta- tion and the precipitation environment of Goss grains in conventional grain-oriented steel were observed and investigated at the initial stage of secondary recrystallization. It reveals that the abnormal Goss grains have a high fraction of high angle boundaries ranging from 25 to 40 deg. The most important observation is that some of {110}〈001〉 grains in matrix indicated higher particle density than their neighbor grains during final annealing at 875℃ before secondary recrystallization, which could create a favorable environment for their abnormal grain growth. Based on misorientation and precipitation results, the abnormal growth mechanism of Goss grains was sketched.

Characterization of Microstructure and Texture in Grain-Oriented High Silicon Steel by Strip Casting

Grain-oriented 4.5 wt% Si and 6.5 wt% Si steels were produced by strip casting, warm rolling, cold rolling, primary annealing, and secondary annealing. Goss grains were sufficiently developed and covered the entire surface of the secondary recrystallized sheets. The microstructure and texture was characterized by OM, EBSD, TEM, and XRD. It was observed that after rolling at 700 ℃, the 6.5 wt% Si steel exhibited a considerable degree of shear bands, whereas the 4.5 wt% Si steel indicated their rare presence. After primary annealing, completely equiaxed grains showing strong y-fiber texture were presented in both alloys. By comparison, the 6.5 wt% Si steel showed smaller grain size and few favorable Goss grains. Additionally, a higher density of fine precipitates were exhibited in the 6.5 wt% Si steel, leading to a ~ 30-s delay in primary recrystallization. During secondary annealing, abnormal grain growth of the 6.5 wt% Si steel occurred at higher temperature compared to the 4.5 wt% Si steel, and the final grain size of the 6.5 wt% Si steel was greater. The magnetic induction B8 of the 4.5 wt% Si and the 6.5 wt% Si steels was 1.75 and 1.76 T, respectively, and the high- frequency core losses were significantly improved in comparison with the non-oriented high silicon steel.

Efect of Ball Scribing on Relative Permeability of Grain-oriented Electrical Steel

Efect of ball scribing on relative permeability of conventional grain-oriented（CGO） and high permeability grain-oriented（HGO） electrical steel was investigated. The samples were scribed with spacing of 2 mm, 4 mm, 8 mm and 16 mm. The results show that after ball scribing with 16 mm width at 1.0 T, relative permeability of both℃GO and HGO steels was increased by 109% and 80%, respectively. Relative permeability rises as the scribing space increases, with the movement of the peak value of relative permeability to a higher flux density. Relational models describing relative permeability and flux density were constructed with high accuracy based on experimental data. The experimental data curves were analyzed during the magnetizing process.

Texture and inhibitor features of grain-oriented pure iron produced by different cold-rolling processes

To promote the manufacture of grain-oriented pure iron, the texture and inhibitor features of two samples A and B produced by different cold-rolling processes were studied by optical microscopy, X-ray diffraction, and transmission electron microscopy. The results showed that a higher content of inhibitor elements directly resulted in a greater number of fine inhibitors, which exhibited strong inhibitory ability, leading to more fine precipitates of appropriate size effectively inhibiting the growth of primary grains in decarburized bands （sheets） during the single-stage cold-rolling process. The formation of the component with { 110}〈001〉 Goss orientation was greatly suppressed in the stage of primary recrystallization, and this component could hardly be observed in the decarburized band; by contrast, the {411 }〈148〉-oriented grains grew. During the process of high-temperature annealing, abnormal growth occurred and secondary recrystallized grains （Goss orientation） merged with other matrix grains such as { 111 }〈112〉 and {411 }〈148〉. The magnetic induction of samples A and B at 800 Aim was 1.939 T and 1.996 T, respectively.

Effect of Ball Scribing on Magnetic Shielding Efficiency of Grain-oriented Silicon Steel

Magnetic shielding of grain-oriented silicon steel was investigated. Ball scribing with spacing of 2 to 16 mm was performed at peak flux densities of 8.0 mT to 1.3 T. Magnetic shielding efficiency was calculated, including absorption, reflection and inner multi-reflection shielding efficiencies. Magnetic shielding efficiency （MSE） increase ratios after different scribing spacing were compared, and thickness requirement to achieve absorption shielding of 50 dB was also calculated. The results show that magnetic shielding efficiencies of C711 and H668 silicon steels increase by 4.79 and 3.15 dB respectively after scribing of 16 mm. Before scribing, shielding efficiency of H668 steel was higher than that of C711 steel, while after scribing, both absorption and shielding efficiency gaps were largely abridged between C711 and H668 steels. Plate thickness of C711 steel could be reduced from 3.18 mm without scribing to 2. 20 mm after scribing of 16 mm. There is no apparent thickness reduction at lower flux densities; while the peak flux density is above 0.3 T, the shielding effect becomes apparent, and the thickness could be reduced from 2.28 mm without scribing to 1.70 mm with scribing spacing of 16 ram. Magnetizing process and its effect on variation of magnetic shielding were also analyzed.

{411}<148> Texture in Thin-Gauge Grain-Oriented Silicon Steel

The significant occupancy of {411}〈148〉texture exists in the thin-gauge grain-oriented silicon steel（TGCRGO is defined that thickness of the sheet is〈0.25 mm and the reduction in cold rolling is more than 90%） which has been considered to have obviously effects on the abnormal growth of Goss-oriented grains during the secondary recrystallization process. The microstructures of the TG-CRGO were investigated by X-ray diffraction and electron back-scattered diffraction in this study. It was found that {411}〈148〉〉texture mainly exists in the center layer of hot-rolled as well as normalized plates.With the increase in cold rolling reduction, {411}〈148〉 orientation gradually rotates to a-fiber texture（〈110〉//RD）.Finally, few {411}〈148〉would retain at the boundaries of deformed a-fiber grains（〈110〉//RD） as the reduction in cold rolling reaches 90%. After annealing treatment, a small amount of c-fiber textures（〈111〉//ND） preferably nucleates and recrystallizes between the DBs（deformation bands） at first; then, the {411}〈148〉 recrystallization texture occurs and mainly nucleates at the grains boundaries of the deformed a-fiber grains, and also quite a few {411}〈148〉orientation grains nucleate in the inner of {112}〈110〉grains. But this phenomenon was not observed in the {100}〈011〉deformation grains.With respect to the occurrence of {411}〈148〉recrystallization texture, it is mainly induced by strong a-fiber as well as weak c-fiber textures formed during cold rolling other than originating from {411}〈148〉 regions in hot bands.

Effect of aluminum on secondary recrystallization texture and magnetic properties of grain-oriented silicon steel

The slab low-temperature reheating grain-oriented silicon steel was prepared in the laboratory,and the high-temperature annealing interruption tests were carried out.The effects of aluminum(which meant acid-soluble aluminum)on the grain size texture,precipitate,magnetic properties and their correlations were studied.The results showed that with the increase in aluminum element,the grain size decreased,while the intensity of{114}<481>and{111}<112>textures increased in the primary recrystallization structure.Meanwhile,the pinning force during the secondary recrystallization and the onset secondary recrystallization temperature were increased.The precipitates were concluded to have a more important role on determining the onset secondary recrystallization temperature than the primary grain size.The higher onset temperature resulted in sharper Goss texture and the better magnetic properties,but when the aluminum content came up to a certain extent,a fine-grain structure was developed.The most suitable aluminum content for present study was 0.025 wt.%,while the onset secondary recrystallization temperature and the primary texture were considered to be conducive to the sharpness of Goss texture.

Secondary Recrystallization Behaviors of Grain-Oriented 6.5 wt% Silicon Steel Sheets Produced by Rolling and Nitriding Processes

By rolling and nitriding processes, 0.23- to 0.3-mm-thick grain-oriented 6.5 wt% silicon steel sheets were produced. The core losses of grain-oriented 6.5 wt% silicon steel at frequencies ranging from 400 Hz to 20 kHz were lower than that of the grain-oriented 3 wt% silicon steel with the same thickness by 16.6-35.8%. The secondary recrystallization behavior was investigated by scanning electron microscopy, energy-dispersive spectroscopy, and electron backscattered diffraction. The results show that the secondary recrystallization in high-silicon steel sheets develops more completely as the nitrogen content increases after nitriding, secondary recrystallized grain sizes become larger, and the sharpness of Goss texture increases. Because more { 110} （116） grains in the subsurface and the central layer of the sheets have a lot of 20°-45° high-energy boundaries in addition to Goss grains, {110} （116） can be the main component through selective growth during secondary recrystallization when the inhibitor quantity is not enough and inhibitor intensity is weaker. The increases in nitrogen content can increase the inhibitor intensity and hinder abnormal growth of a mount of {110} （116） grains and therefore enhance the sharpness of Goss texture.