Effect of Thickness and Annealing Temperature on Magnetic Properties of Ultrathin γ-Fe2O3 Films Grown on Silicon Substrate

The effect of thickness and annealing temperature on magnetic properties of ultrathin γ-Fe₂O₃ films with MgO buffer layer grown on silicon substrate is investigated. The saturation magnetization and coercive force of samples at room temperature increase with increasing of annealing temperature, and decrease as annealing temperature is above 873 K (600 °C). The saturation magnetization of samples decreases with increasing of the thickness of γ-Fe₂O₃ at room temperature. The samples with 3 to 4 nm thick γ-Fe₂O₃ annealed at 873 K (600 °C) show saturation magnetization of about 400 emu/cm³, which is close to the bulk value of ~390 emu/cm³ within the error range.     

Design of strong tough Fe/Mo/C martensitic steels and the effects of cobalt

The microstructures and mechanical properties of a series of vacuum melted Fe/(2 to 4) Mo/(0.2 to 0.4) C steels with and without cobalt have been investigated in the as-quenched fully martensitic condition and after quenching and tempering for 1 h at 673 K (400°C) and 873 K (600°C); austenitizing was done at 1473 K (1200°C) in argon. Very good strength and toughness properties were obtained with the Fe/2 Mo/0.4 C alloy in the as-quenched martensitic condition and this is attributed mainly to the absence of internal twinning. The slightly inferior toughness properties compared to Fe/Cr/C steels is attributed to the absence of interlath retained austenite. The two 0.4 pct carbon steels having low Mo contents had approximately one-half the amount of transformation twinning associated with the two 0.4 pct carbon steels having high Mo contents. The plane strain fracture toughness of the steels with less twinning was markedly superior to the toughness of those steels with similar alloy chemistry which had more heavily twinned microstructures. Experiments showed that additions of Co to a given Fe/Mo/C steel raised M_s but did not decrease twinning nor improve toughness. Molybdenum carbide particles were found in all specimens tempered at 673 K (400°C). The Fe/Mo/C system exhibits secondary hardening after tempering at 873 K (600°C). The precipitate is probably Mo₂C. This secondary hardening is associated with a reduction in toughness. Additions of Co to Fe/Mo/C steels inhibited or eliminated the secondary hardening effect normally observed. Toughness, however, did not improve and in fact decreased with Co additions.     

Ferrite recrystallization and austenite formation in cold-rolled intercritically annealed steel

The recrystallization of ferrite and austenite formation during intercritical annealing were studied in a 0.08C-1.45Mn-0.21Si steel by light and transmission electron microscopy. Normalized specimens were cold rolled 25 and 50 pct and annealed between 650 °C and 760 °C. Recrystallization of the 50 pct deformed ferrite was complete within 30 seconds at 760 °C. Austenite formation initiated concurrently with the ferrite recrystallization and continued beyond complete recrystallization of the ferrite matrix. The recrystallization of the deformed ferrite and the spheroidization of the cementite in the deformed pearlite strongly influence the formation and distribution of austenite produced by intercritical annealing. Austenite forms first at the grain boundaries of unrecrystallized and elongated ferrite grains and the spheroidized cementite colonies associated with ferrite grain boundaries. Spheroidized cementite particles dispersed within recrystallized ferrite grains by deformation and annealing phenomena were the sites for later austenite formation.     

High Strength and High Ductility of Ultrafine-Grained,Interstitial-Free Steel Produced by ECAE and Annealing

Interstitial-free steel (IF steel) underwent severe plastic deformation by equal-channel angular extrusion/pressing (ECAE/P) to improve its strength, and then it was annealed to achieve a good strength-ductility balance. The coarse-grained microstructure of IF steel was refined down to the submicron level after eight-pass ECAE. The ultrafine-grained (UFG) microstructure with high dislocation density brought about substantially improved strength but limited tensile ductility. The limited ductility was attributed to the small, uniform elongation caused by early plastic instability. The annealing at temperatures below 723 K (450 °C) for 1 hour did not lead to remarkable softening, whereas annealing at temperatures up to 923 K (650 °C) resulted in complete softening depending on the development of recrystallization. Therefore, the temperature of approximately 923 K (650 °C) can be considered as a critical recrystallization temperature for UFG IF steel. The annealing at 873 K (600 °C) for different time intervals resulted in different stress–strain response. Uniform tensile elongation increased at the expense of strength with annealing time intervals. After annealing at 873 K (600 °C) for 60 minutes, the yield strength, tensile strength, uniform elongation, and total elongation were found to be 320 MPa, 485 MPa, 15.1 pct, and 33.7 pct, respectively, showing the better combination of strength and ductility compared with cold-rolled samples.     

Design of strong tough Fe/Mo/C martensitic steels and the effects of cobalt

The microstructures and mechanical properties of a series of vacuum melted Fe/(2 to 4) Mo/(0.2 to 0.4) C steels with and without cobalt have been investigated in the as-quenched fully martensitic condition and after quenching and tempering for 1 h at 673 K (400°C) and 873 K (600°C); austenitizing was done at 1473 K (1200°C) in argon. Very good strength and toughness properties were obtained with the Fe/2 Mo/0.4 C alloy in the as-quenched martensitic condition and this is attributed mainly to the absence of internal twinning. The slightly inferior toughness properties compared to Fe/Cr/C steels is attributed to the absence of interlath retained austenite. The two 0.4 pct carbon steels having low Mo contents had approximately one-half the amount of transformation twinning associated with the two 0.4 pct carbon steels having high Mo contents. The plane strain fracture toughness of the steels with less twinning was markedly superior to the toughness of those steels with similar alloy chemistry which had more heavily twinned microstructures. Experiments showed that additions of Co to a given Fe/Mo/C steel raisedM _S but did not decrease twinning nor improve toughness. Molybdenum carbide particles were found in all specimens tempered at 673 K (400°C). The Fe/Mo/C system exhibits secondary hardening after tempering at 873 K (600°C). The precipitate is probably Mo₂C. This secondary hardening is associated with a reduction in toughness. Additions of Co to Fe/Mo/C steels inhibited or eliminated the secondary hardening effect normally observed. Toughness, however, did not improve and in fact decreased with Co additions.     

Microstructural Changes by Annealing in Ultrafine-Grained Electrodeposited Pure Iron

In situ neutron diffraction during annealing was performed for ultrafine-grained as-deposited and cold-rolled pure iron. Changes in the integrated intensity and full-width at half-maximum in the diffraction profiles during annealing were measured. EBSD measurements were performed before and after annealing to obtain microstructural change. Abnormal grain growth was clearly found at 673 K (400 °C) upon annealing; this observation corresponds to the hydrogen desorption behavior of the as-deposited specimen. The texture changes from {111}〈hkl〉 to {211}〈hkl〉 between 673 K and 873 K (400 °C and 600 °C) upon continuous heating. Such a texture change is postulated to decrease the Lankford value from 7.6 to 2.2. The 40 pct cold-rolled specimen exhibited a complicated textural evolution upon annealing, which was caused by the intrusion of recrystallization at deformation bands.     

Effect of Thermal Aging on Ductile-Brittle Transition Temperature of Modified 9Cr-1Mo Steel Evaluated with Reference Temperature Approach Under Dynamic Loading Condition

The effect of thermal aging on the ductile-brittle transition behavior has been assessed for a modified 9Cr-1Mo steel (P91) using the reference temperature approach under dynamic loading condition (T ₀ ^dy ). The steel in normalized and tempered (NT) condition and in different levels of subsequent cold work (CW) was subjected to thermal aging at temperatures of 873 K and 923 K (600 °C and 650 °C) for 5000 and 10,000 hours. For the NT and all the cold work conditions of the starting material, a drastic increase in T ₀ ^dy has been noticed after aging at 923 K (650 °C) for 10,000 h. A moderate increase was observed for the NT steel aged at 873 K (600 °C) for 5000 hours and for the 10 pct CW steel aged at 873 K (600 °C) for 10,000 h. A detailed transmission electron microscope (TEM) study of the embrittled materials aged at 923 K (650 °C)/10,000 hours and 873 K (600 °C)/10,000 hours has indicated presence of hexagonal Laves phase of Fe₂(Mo,Nb) type with different size and spatial distributions. The increase in the T ₀ ^dy is attributed to the embrittling effect of a network of Laves phase precipitates along the grain boundaries.     

The influence of Al3Zr dispersoids on the recrystallization of hot-deformed AA 7010 alloys

The recrystallization of AA 7010 alloys (Al-6 pct Zn-2.4 pct Mg-1.6 pct Cu-Zr) during solution treatment is investigated as a function of Zr content after deformation under conditions simulating hot rolling. The respective roles of the volume fraction and size of Al₃Zr dispersoids are characterized by additions of 0.05 to 0.12 pct Zr and suitable heat treatments. Plane strain compression (channeldie) tests at temperatures of 320 °C and 440 °C were conducted to strains of 1, and the samples subsequently solution-annealed at 470 °C. Recrystallization during this anneal was characterized by optical and electron microscopy and X-ray diffraction. The fraction recrystallized decreases with increasing Zr content, higher deformation temperature, and finer particle size. An original model based on the concept of the recrystallizable volume fraction is presented to predict the degree of recrystallization in materials characterized by spatially heterogeneous microstructures.     

Heat treatment and properties of plastically deforming, highly coercive iron alloy (30% Cr, 15% Co, 2% W, 1% Mo, and 1% Ti)

The structural transformations of plastically deforming, highly coercive Kh30K15V2MT iron alloy (30% Cr, 15% Co, 2% W, 1% Mo, and 1% Ti) are studied, along with its magnetic and mechanical properties. Metallographic and X-ray data show that, besides the α solid solution that exists at 1220–1180°C, metastable α phase is present at 670–700°C. If the alloy is annealed at 670–700°C after cold deformation, no recrystallization occurs; only processes of recovery and polygonization are observed. The relation of the magnetic and mechanical properties to the initial state and structure of the single-phase α solid solution is established. Either good magnetic properties or good mechanical properties may be obtained, by adjusting the initial state of the single-phase α solid solution.     

Hot Deformation Behavior of As-Cast 2101 Grade Lean Duplex Stainless Steel and the Associated Changes in Microstructure and Crystallographic Texture

The hot deformation behavior of 2101 grade lean duplex stainless steel (DSS, containing ~5 wt pct Mn, ~0.2 wt pct N, and ~1.4 wt pct Ni) and associated microstructural changes within δ-ferrite and austenite (γ) phases were investigated by hot-compression testing in a GLEEBLE 3500 simulator over a range of deformation temperatures, T _def [1073 K to 1373 K (800 °C to 1100 °C)], and applied strains, ε (0.25 to 0.80), at a constant true strain rate of 1/s. The microstructural softening inside γ was dictated by discontinuous dynamic recrystallization (DDRX) at a higher T _def [1273 K to 1373 K (1000 °C to 1100 °C)], while the same was dictated by continuous dynamic recrystallization (CDRX) at a lower T _def (1173 K (900 °C)]. Dynamic recovery (DRV) and CDRX dominated the softening inside δ-ferrite at T _def ≥ 1173 K (900 °C). The dynamic recrystallization (DRX) inside δ and γ could not take place upon deformation at 1073 K (800 °C). The average flow stress level increased 2 to 3 times as the T _def dropped from 1273 to 1173 K (1000 °C to 900 °C) and finally to 1073 K (800 °C). The average microhardness values taken from δ-ferrite and γ regions of the deformed samples showed a different trend. At T _def of 1373 K (1100 °C), microhardness decreased with the increase in strain, while at T _def of 1173 K (900 °C), microhardness increased with the increase in strain. The microstructural changes and hardness variation within individual phases of hot-deformed samples are explained in view of the chemical composition of the steel and deformation parameters (T _def and ε).

     

Effect of Scandium on the Interaction of Concurrent Precipitation and Recrystallization in Commercial AA3003 Aluminum Alloy

In the current study, the effect of Sc addition on the interaction of concurrent precipitation and recrystallization in commercial AA3003 aluminum alloy was investigated using optical microscopy, scanning electron microscopy, and transmission electron microscopy. In case of AA3003 alloy, which was cold rolled to a true strain of 2.20 and heated at a heating rate of 150 K/s, the onset of precipitation and ending of recrystallization are signified by the critical temperature, T _C ~740 K (467 °C). There is a change in the shape of the recrystallized grains from pancake-like to equiaxed shape, as the annealing temperature increases greater than T _C. In case of AA3003 alloy microalloyed with 0.4 wt pct of Sc, the high no. density precipitation of coherent Al₃Sc precipitates always occurs before recrystallization because of the small nucleation barrier and high rate of decomposition. This leads to extremely coarse pancake-like recrystallization grains with high fraction of low-angle grain boundaries in the entire annealing temperature range, even at a high brazing temperature of 883 K (610 °C).     

The influence of Sc on thermal stability of a nanocrystalline Al-Mg alloy processed by cryogenic ball milling

The microstructural evolution during annealing of a cryogenically ball-milled Al-7.5Mg-0.3Sc (in wt pct) was examined using differential scanning calorimetry and transmission electron microscopy (TEM). The as-milled alloy was a supersaturated fcc solid solution with an average grain size of ∼25 nm and heterogeneous grain morphologies and size distributions. Calorimetric measurements at a constant heating rate of 32 K/min indicated two exothermic events in association with recovery from 100 °C to 240 °C and recrystallization from 300 °C to 450 °C. Prior to recrystallization, the precipitation of Al₃Sc may occur at low annealing temperatures producing a nonuniform dispersion of approximately spherical particles with diameters of 4 to 5 nm. Recrystallization gave rise to heterogeneous microstructures with bimodal grain size distributions, which may result from the heterogeneity of microstructure in the as-milled state. The heterogeneous microstructures of the recrystallized Al-Mg-Sc alloy were similar to those observed in the recrystallized Sc-free Al-Mg alloy.     

Fabrication of Al2O3-reinforced Ni3Al composites by a novel in situ route

A novel in situ technique has been used to fabricate an Al₂O₃-reinforced Ni₃Al matrix composite. The composite was prepared by first incorporating a low volume fraction of continuous Al₂O₃ fibers in a Ni₃Al alloy containing 0.34 at. pct Zr. Pressure casting was used to embed the fibers. Casting resulted in partial reduction of the Al₂O₃ fiber by the Zr present in the matrix and the formation of a layer of ZrO₂ on the surface of the fibers. The final composite was then prepared by air annealing the precursor composite at 1100 °C for 10 days. Air annealing led to the formation of networks of Al₂O₃ around the fibers. The matrix in the immediate vicinity of the networks consisted of Ni₃Al particles in a matrix of disordered α-Ni(Al). The Al₂O₃ networks raised the yield and tensile strength of the material by 35 and 18 pct, respectively. The composite had a tensile ductility of 14 pct.     

Precipitation in a Cu-30 Pct Ni-1 Pct Nb alloy

Decomposition of a Cu-30 pct Ni-1 pct Nb alloy on aging in the range of 866 K (600°C) to 1073 K (800°C) was investigated. The initial decomposition, concomitant with age hardening, occurred through the precipitation of body centered tetragonal metastable Ni₃Nb-γ” precipitates on the 100 matrix planes. Equilibrium orthorhombicβ phase formed either through a grain boundary cellular reaction at low temperature (≤973 K (700°C)) or as Widmanstaettenplatelets on the 1ll planes at higher temperatures (≥1073 K (800°C)) with the following crystallographic relationship: (0l0)_β//111_γ [100]β//[1•11]_γ. Based on the observations, a schematic transformation sequence is presented.     

The influence of thermomechanical processing variables on superplasticity in a High-Mg,Al-Mg alloy

The superplastic response of an Al-10.2 pct Mg-0.52 pct Mn alloy, warm rolled at 573 K (300 °C), may be enhanced by annealing at a lower temperature, 473 K (200 °C), prior to subsequent stressstrain testing at a warm temperature,e.g., 573 K (300 °C). This enhancement is attributed to recovery and precipitation during annealing effectively retarding continuous recrystallization and growth during subsequent deformation. The finer resultant structure more readily sustains superplastic flow processes. The warm-rolled structure, a refined subgrain structure in conjunction with fine β (Mg₅Al₈) and MnAl₆ precipitates, will statically recrystallize only upon heating to a temperature above the Mg solvus, such as 713 K (440 °C). Such recrystallization results in a relatively fine-grained material but also suppresses warm-temperature superplasticity; deformation at 573 K (300 °C) takes place by dislocation flow in the recrystallized material. At temperatures above the Mg solvus, both warm rolled and recrystallized materials exhibit superplastic elongations but cavitate extensively as a result of deforming by boundary sliding. Formerly with Materials Group, Mechanical Engineering Department, Naval Postgraduate School, Monterey, CA Formerly Graduate Student in Mechanical Engineering, Naval Postgraduate School, Monterey, CA     

On the improvement of creep strength and ductility of Ni-20 pct Cr by small zirconium additions

The creep and fracture properties of high-purity Ni-20 pct Cr and Ni-20 pct Cr-0.11 pct Zr alloys are compared at 1073 K in vacuum. The Ni-20 pct Cr alloy cavitates at the grain boundaries and fractures intergranularly after strains of typically 20 pct. The observed cavity growth rates are in keeping with those predicted. Alloying with zirconium substantially increases the creep strength and ductility. Creep rupture associated with dynamic recrystallization occurs, and voids are observed only in heavily necked parts of the samples. In addition to Ni₅Zr and ZrO₂ inclusions, a Zr₄C₂S₂ carbo-sulfide was identified. Thus, the sulfur-gettering effect of zirconium even at very low residual sulfur levels (20 wt ppm) was confirmed. The zirconium-induced increase in the creep strength is discussed, and the inhibition of creep cavitation by zirconium is examined within the framework of thermal cavity nucleation. Lowering of the grain boundary diffusivity and the grain boundary free energy as well as dynamic recrystallization are likely to reduce cavity nucleation and growth rates in Ni-Cr-Zr and will thus increase its ductility. Finally, the results are used to illustrate the critical importance of minor alloying additions in constructing and using fracture mechanism maps.     

Microstructure and Magnetic Properties of Ni2(Mn,Fe)Ga Heusler Alloys Rapidly Solidified by Melt Spinning

The microstructure and magnetic properties of Ni₂MnGa base alloys with “Fe” substitution in place of “Mn” are studied. The processing technique used is melt spinning at wheel speeds of 20 m/s and 30 m/s followed by annealing at 1273 K (1000 °C) for 1 hour. Fe content is varied from 2 at. pct to 11 at. pct for alloys of Ni₅₀Mn_(25?x)Fe _x Ga₂₅ with Heusler stoichiometry. Austenite with B2 partial atomic ordering and premartensitic tweed structures were found at room temperature for all the alloys at different wheel speeds. After annealing at 1273 K (1000 °C) for 1 hour, austenite phase with L2₁ Heusler atomic ordering is stabilized in samples of all the processing conditions. Saturation magnetization, martensitic transformation temperature, and Curie temperature are measured. Martensite temperature and Curie temperature increase in proportion to iron content in the alloy. Saturation magnetization is sensitive to the phase content and compositional inhomogeneities.     

Particle Stimulated Nucleation in Coarse-Grained Ferritic Stainless Steel

Particle-stimulated nucleation (PSN) is investigated in Nb-containing ferritic stainless steel. Coarse-grained sheets were cold rolled to 80 pct thickness reduction and annealed from 973 K to 998 K (700 °C to 725 °C) to obtain partially recrystallized microstructures. Electron backscatter diffraction was performed around coarse niobium carbonitride particles (larger than 1 ??m) within coarse grains (~1 mm), with different host orientations in both deformed and annealed states. In the deformed state, the deformation zones around both spherical and rectangular particles were investigated. The local lattice rotations about the transverse direction necessary to accommodate the particle-matrix strain incompatibility were observed in all grains investigated. After annealing, recrystallization occurs preferentially around coarse particles at the initial stages of recrystallization. Based on a total number of 130 grains nucleated via PSN, we observe both, randomly oriented and minor {111}??110?? oriented texture components. The results also reveal that PSN in this material is not associated with a specific host orientation.     

Recrystallization behavior of a heavily cold-rolled Ni3Al(B,Zr) alloy

The present article describes the microstructural changes during recrystallization annealing of a 73 pct cold-rolled Ni₃Al(B,Zr) alloy along with a study of the recrystallization kinetics. The deformed γ regions, mostly within and near the shear bands, appear to recrystallize first. The recrystallization front leaves behind a lamellar discontinuous precipitation within the newly formed strain-free γ grains, when annealing is done at lower temperatures. At higher annealing temperatures, the precipitates within γ assume a globular morphology. This precipitate is presumably made up of γ′ particles. When γ recrystallization is nearly complete, the γ′ regions start to recrystallize. The two-stage recrystallization process is also corroborated from the kinetics results, which show that the activation energy up to 50 pct recrystallization of the material is only 117 kJ/mole, whereas beyond 50 pct until the completion of recrystallization, an activation energy of ∼274 kJ/mole is obtained.     

Breakdown of primary grain boundary inhibition in 3 pct si-fe sheet

Grain boundary inhibition in 11-mil cold rolled decarburized 3 pct Si-Fe sheet was observed to break down by isothermal annealing at temperatures in excess of 1075°C. Small MnS particles (-r < ~260Å) responsible for inhibiting primary grain growth in this material were observed to undergo complete dissolution within 3 min at temperatures of 1100°C and higher. Calculated dissolution rates were in good agreement with this observation. The dissolution of these particles produced appreciable primary grain growth during the early stages of (110)[00l] secondary recrystallization which was responsible for an overall reduction in the volume percent of (H0)[00l] grains produced on prolonged isothermal annealing at temperatures above 1075°C.