Evolution of phase,texture, microstructure and magnetic properties of Fe–Cr–Co–Mo–Ti permanent magnets

Magnetic phase evolution, crystallographic texture, microstructure and magnetic properties of Fe–28Cr–15Co–3.5Mo–1.8Ti alloy have been investigated by X-ray diffractometry, scanning transmission electron microscopy and magnetometry techniques as a function of processing conditions. Heat treatment conditions for obtaining optimum textural, microstructural and magnetic properties have been established by the experimentations. The Goss {110}〈001〉 and cube type {001}〈010〉 textures have been developed in an optimal treated Fe–28Cr–15Co–3.5Mo–1.8Ti magnets. The coercive force in Fe–28Cr–15Co–3.5Mo–1.8Ti magnets depends critically on the shape anisotropy of rod-like Fe Co Ti-rich α₁ particles and remanence on the alignment and elongation of α₁ particles parallel to applied magnetic field 〈100〉 directions. The optimum magnetic properties obtained in Fe–28Cr–15Co–3.5Mo–1.8Ti alloy are intrinsic coercive force, _iH_c, of 78.8 kA/m (990 Oe), remanence, B_r of 1.12 T (11.2 kG) and energy product, (BH)_max of 52.5 kJ/m³ (6.5 MGOe). The development of Fe–28Cr–15Co–3.5Mo–1.8Ti magnets as well as characterization of texture, microstructural and magnetic properties in the current study would be helpful in designing the new Fe–Cr–Co–Mo based magnets suitable for scientific and technological applications.     

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.     

Microstructure and texture evolution of strip casting 3 wt% Si non-oriented silicon steel with columnar structure

An Fe-3 wt%Si strip with columnar structure and pronounced {0 0 1}〈0 v w〉 texture was produced using a twin-roll strip caster. Then the as-cast strip was cold-rolled and annealed. The microstructure and texture evolution along the processing steps was investigated. It is found that inhomogeneous microstructure is produced in both cold-rolled and final annealed samples due to the large initial grains. The cold rolling texture is dominated by pronounced a-fiber texture and relatively strong γ-fiber texture. The final recrystallization texture is characterized by {0 0 1}〈0 1 0〉, {0 0 1}〈2 1 0〉, {1 1 0}〈0 0 1〉 texture and a slightly shifted {1 1 1}〈1 1 2〉 component. The microstructural inhomogeneity plays an important role in the texture evolution.     

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.     

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.     

Developments in the production of grain-oriented electrical steel

The quality and production technology of grain-oriented electrical steel have been improved over the past 70 years. Firstly, through the improvement of {1 1 0} 〈0 0 1〉 alignment, development of thinner-gauge material, and establishment of magnetic domain refining techniques, magnetic properties of the material have been improved dramatically. Secondly, many mechanisms have been proposed for the reason why Goss texture develops selectively during the final annealing stage. Thirdly, to reduce manufacturing costs, many new techniques have been developed. The most advanced in commercial realization is the application of low-temperature slab-reheating techniques. Despite these achievements, the mechanisms of texture selection are not yet clear in all their details. Further improvement of magnetic properties and the application of compact production process for grain-oriented electrical steels in commercial production are needed to be realized.     

The surface blistering kinetics and the H-platelet evolution in H-implanted germanium

The surface blistering phenomenon produced in H-implanted Ge by a series of low temperature annealing processes was investigated. The kinetic plot of the onset of blistering contains a break point that separates the straight-line plot into two parts, with two distinct slopes based on the calculated activation energy from the different temperature regions for 3×10¹⁶ cm⁻² and 5×10¹⁶ cm⁻² H-implanted doses. This plot indicates the existence of distinct, temperature dependent mechanisms, probably caused by the release of different types of H-platelets. The turning direction (from low to high temperature) of the Arrhenius plot with the break point is contrary to that of other known materials. The formation and evolution of the H-platelets under the Ge surface was revealed by TEM (transmission electron microscopy). The TEM results demonstrate that the 〈0 0 1〉 platelets parallel to the sample surface are first produced by a low H implantation dose; however, the vertical 〈0 1 0〉 platelets perpendicular to the sample surface form later as the H implantation dose increases. The H-platelets combine with each other, becoming micro-cracks. The {1 1 1} and {3 1 1} micro-cracks serve as interconnections between the 〈0 0 1〉-oriented micro-cracks below the substrate surface. Finally, the accumulated H₂ pressure in the cracks deforms the surface to generate Ge surface exfoliation.     

Angular distributions of atoms sputtered from NiAl{1 1 0} and Ni{1 0 0}

Using the laser post-ionization surface analysis technique, I have for the first time studied angular distributions of Ni and Al atoms sputtered from NiAl{1 1 0}. Emission angular distributions from Ni{1 0 0} have also been measured. I have observed preferential emissions of Ni and Al atoms along 〈1 1 1〉 and 〈1 0 0〉crystallographic directions for NiAl{1 1 0} and of Ni atoms along 〈1 1 0〉 and 〈1 0 0〉 directions for Ni{1 0 0}. The observed preferential ejections can be explained in terms of the theory of focusing-collision sequences. Because of the difference in surface binding energy between Al and Ni atoms, preferential ejection angles of Ni atoms are slightly different from those of Al atoms along the 〈1 1 1〉 ejections. For NiAl, the 〈1 1 1〉 preferential ejections were less prominent than the 〈1 0 0〉 preferential ejections and this can be related to the low efficiency of momentum transfer in Ni-Al collision sequences along 〈1 1 1〉 lattice directions. The low efficiency of momentum transfer due to the mass mismatch can also be responsible for the experimental observation that the preferential ejections in the alloy were less prominent than those in the Ni metal.     

Microstructure and magnetic properties studies of SmCo5 thin films grown on MgO and glass substrates

In this work, SmCo₅ thin films are deposited on single crystal MgO (1 0 0) and amorphous glass substrates with a Cr underlayer at 400 °C by sputtering. A comparison study shows that the microstructures and magnetic properties are different in the two SmCo₅ films on the MgO (1 0 0) and glass substrates, respectively. An epitaxial growth of Cr-(2 0 0)〈1 1 0〉/SmCo₅-(1 1 2¯ 0)〈0 0 0 1〉 is achieved on the MgO (1 0 0) single crystal substrate with an average grain size of 20 nm for SmCo₅. On the amorphous glass substrate, no significant crystallographic texture is found in the Cr underlayer. After the deposition of SmCo₅, a weak texture of (1 1 2¯ 0) is observed with an average grain size of 8 nm. High remanence ratio value in this film is probably due to strong exchange coupling. Both SmCo₅ films show high in-plane coercivity, high in-plane anisotropy and remanence enhancement.     

Effect of deformation and annealing on the microstructure and magnetic properties of grain-oriented electrical steels

The effect of plastic deformation and subsequent annealing on the magnetic properties and microstructure of a grain-oriented (GO) electrical steel has been studied. True strain (ε) from 0.002 to 0.23 was applied by rolling in two directions, rolling (RD) and transverse (TD). The deterioration of power losses varies according to the direction of deformation. Annealing the strained material—at 800 °C/2 h—leads to a recrystallization and restored magnetic properties. The main components of annealed-textures are around 15–35° from those of deformed-textures for both RD and TD. Rolling along {1 1 0} 〈0 0 1〉 direction leads to the development of deformation twins.     

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.     

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.     

Effect of isotropic stress on dislocation bias factor in bcc iron: an atomistic study

The effect of externally applied stress on the dislocation bias factor (BF) in bcc iron has been studied using a combination of atomistic static calculations and finite element integration. Three kinds of dislocations were considered, namely, a₀/2〈1 1 1〉{1 1 0} screw, a₀/2〈1 1 1〉{1 1 0} edge and a₀〈1 0 0〉{0 0 1} edge dislocations. The computations reveal that the isotropic crystal expansion leads to an increasing or constant dislocation bias, depending on the Burgers vector and type of dislocation. On the other hand, compressive stress reduces the dislocation bias for all the dislocations studied. Variation of the dislocation BF depending on dislocation type and Burgers vector is discussed by analysing the modification of the interaction energy landscape and the capture efficiency values for the vacancy and self-interstitial atom.     

Evolution of modulated structure in Fe–Cr–Co alloy during isothermal ageing with different external magnetic field conditions

The evolution of modulated structure in Fe–Cr–Co alloy during isothermal ageing with and without external magnetic field was investigated by using transmission electron microscopy (TEM) and phase-field simulation. The isotropic modulated structure in Fe–Cr–Co alloy formed during isothermal ageing without external magnetic field could be converted to be anisotropy during further isothermal ageing under an 8 kOe external magnetic (thermo-magnetic treatment), and the formation of anisotropy was slower than the direct formation from spinodal decomposition under external magnetic field and is time dependent. The anisotropy characteristic of modulated structure in Fe–Cr–Co alloy subjected to thermo-magnetic treatment for 1 h remained during further isothermal ageing without external magnetic field for up to 20 h. Novel modulated structure could be obtained through specific thermo-magnetic treatment processes, which was confirmed by phase-field simulation.     

A combined ab initio and atomistic simulation study of the surface and interfacial structures and energies of hydrated scheelite: introducing a CaWO4 potential model

Density functional theory (DFT) calculations of the calcium tungstate material scheelite CaWO₄ have shown that water introduced into the bulk material remains undissociated and leads to swelling and layering of the structure, a behaviour which may resemble silicate clays more than three-dimensional poly-anionic materials, but which results in a structure that is even more similar to a rare hydrous calcium carbonate phase--a finding which suggests the existence of semi-crystalline hydrous pre-cursor phases to the dehydrated scheelite material. An interatomic potential model was derived for CaWO₄ which adequately reproduces structural and physical properties of the material and is in good agreement with the DFT calculations in respect of the structure and energy of hydration (DFT: 85 kJ mol⁻¹, atomistic: 105 kJ mol⁻¹). Atomistic simulations of a range of scheelite surfaces confirm the dominance of the experimental {1 0 1} and {0 0 1} cleavage planes in the morphology of the dry crystal and the presence of the experimentally found {1 0 3} and {1 0 1} surfaces in the hydrated morphology. Hydration of the surfaces shows non-Langmuir behaviour, where the interactions between surface calciums and oxygen atoms of the water molecules outweigh hydrogen-bonding to the surface oxygen atoms or intermolecularly within the water layer. The hydration energies indicate physisorption of water, ranging from 22 kJ mol⁻¹ on the {0 0 1} surface to 78 kJ mol⁻¹ on the more reactive {1 0 3} surface.     

Magnetocaloric effect in high-energy ball-milled Gd5Si2Ge2 and Gd5Si2Ge2/Fe nanopowders

Evolution of structure and magnetocaloric properties in ball-milled Gd₅Si₂Ge₂ and Gd₅Si₂Ge₂/0.1 wt% Fe nanostructured powders were investigated. The high-energy ball-milled powders were composed of very fine grains (70–80 nm). Magnetization decreased with milling time due to decrease in the grain size and randomization of the magnetic moments at the surface. The magnetic entropy change (ΔS_M) was calculated from the isothermal magnetization curves and a maximum value of 0.45 J/kg K was obtained for 32 h milled Gd₅Si₂Ge₂ alloy powder for a magnetic field change of 2 T while it was still low in Fe-contained alloy powders. The thermo-magnetic measurements revealed that the milled powders display distribution of magnetic transitions, which is desirable for practical magnetic refrigerant to cover a wide temperature span.     

Effects of layering and magnetic annealing on the texture of CoPt films

The effect of magnetic field annealing of magnetron sputtered CoPt alloy films and Co/Pt bilayers on the crystallographic texture of the obtained chemically ordered (L1₀) CoPt films is presented. In CoPt alloy films the main effect of the magnetic field is to suppress (1 1 1) growth in the early stages of L1₀ formation whereas the development of (0 0 1) versus (1 0 0) texture is related to chemical ordering strain. A higher degree of (0 0 1) texture is obtained by magnetically annealing Co/Pt bilayers since the initial (1 1 1) texture in the as-sputtered films is avoided and Co-Pt alloying occurs in the presence of the magnetic field.     

Observation of regular defects formed on the surface of PbTe thin films grown by molecular beam epitaxy

Regular shape defects on the surface of PbTe thin films grown by molecular beam epitaxy (MBE) were studied by scanning electron microscope (SEM). Two types of regular shape defects were observed on Te-rich PbTe films grown at substrate temperature T ≥ 235 °C with a beam flux ratio of Te to PbTe (R_f) to be 0.5 and at 280 °C with a R_f ≥ 0.4, which include cuboids and triangular pyramids. The formation mechanism of the observed regular shape defects is interpreted as following: They are the outcome of fast growth rate along {1 0 0} crystal planes that have the lowest surface energy and the enclosure of the {1 0 0} crystal planes. The formation of the regular shape defects in the growth of PbTe needs appropriate substrate temperature and Te-rich ambience. However, when R_f is decreased low enough to make the films slightly Pb-rich, triangular pits that originate from the insufficient glide of the threading dislocations along the main 〈1 1 0〉 {1 0 0} glide system of PbTe in Cottrell atmosphere, will be the main feature on the film surface.     

The formation model of Ni-Cr oxides on NiCoCrAlY-sprayed coating

The atomic arrangement and distribution of oxides (Cr₂O₃, NiCr₂O₄ and NiO) on the sprayed-NiCoCrAlY coating after oxidation are analyzed. The formation and the growth model of Ni-Cr oxide phases are discussed according to the matching relationship between atoms. The outline character and a scale of spinel NiCr₂O₄ are discussed. The results show that Cr atoms can form two close-packed arrangements in the crystal plane of Cr₂O₃ perpendicular to 〈0 0 1〉 orientation. The atomic spacing in the first arrangement corresponds to double that of Ni/Ni₃Al in {1 1 1} crystal face. This suggests that Ni/Ni₃Al is the substrate for Cr₂O₃ to grow along 〈0 0 1〉 direction. The lattice mismatch between Cr₂O₃ and Ni/Ni₃Al is less than that of Al₂O₃, which indicates that Cr₂O₃ is easier to form than Al₂O₃ during the oxidation process. The atomic spacing in another close-packed arrangement of Cr₂O₃ perpendicular to 〈0 0 1〉 orientation is approximately equal to that of Ni or Cr in the plane of NiCr₂O₄ and NiO perpendicular to 〈1 1 1〉 orientation. So Cr₂O₃ can be the substrate for NiCr₂O₄ and NiO to grow in the 〈0 0 1〉 direction. NiCr₂O₄ and NiO can grow directly along the 〈1 1 1〉 orientation on each other. NiCr₂O₄ can grow outward in the planes of Cr₂O₃ perpendicular to 〈0 0 1〉 and grow inward along 〈1 1 1〉 orientation of NiO.     

Texture development during cold rolling of Fe–Cr–Ni alloy-experiments and simulations

Abstract

In the present work, evolution of microstructure and crystallographic texture during cold rolling of two phase Fe–Cr–Ni alloy was investigated. Fe–Cr–Ni alloy (in initially solution annealed condition) was uni-directionally cold rolled in a laboratory rolling mill to different thickness reductions. Scanning electron microscopy was used to observe the changes in microstructure, while X-ray diffraction was used to investigate changes in crystallographic texture of austenite and ferrite (through changes in orientation distribution function). Crystallographic texture was also simulated using different crystal plasticity models (Full constraint Taylor, relaxed constraint Taylor (lath and pancake) and co-deformation Visco Plastic Self Consistent (VPSC)). With the increase in plastic deformation, there were morphological as well as crystallographic changes in the microstructure. Strong α-fibre (RD//〈1?1?0〉) texture was developed in ferrite, while brass ({1?1?0}〈1?1?2〉) and Goss ({1?1?0}〈0?0?1〉) was dominant in austenite after 80% cold rolling. The formation of brass type texture after deformation has been attributed to the formation of shear bands and presence of strong crystallographic texture in the initial solution annealed material. Both Taylor as well as VPSC models could not capture the changes in texture with deformation accurately. For ferrite: γ-fibre (ND//〈1?1?1〉) and for austenite: Cu ({1?1?2}〈1?1?1〉) component was always present in the simulated textures. Possible reason for this could be the pining effect of interface boundaries and non-incorporation of non-crystallographic shear banding in the Taylor and VPSC models.