Defect structures and phase transitions of FeRh alloys deformed at high speed deformation

Fe–Rh alloys of Rh concentrations ranging from 40 to 50at.% and of B2 phase were deformed by use of a compression machine capable of running tests at high speeds of impact. Induced complicated substructures and phases were examined by X-ray diffraction (XRD), transmission electron microscopy (TEM), and positron annihilation spectroscopy (PAS). A characteristic arrangement of L1₀ domains was observed, along with very small transformed A1 domains and dispersed in the residual B2 matrix. On the basis of the experimental results, we suggest a coupling of a pair of shears along {112}11−1_B2 for the transformation mechanisms from B2 to L1₀ and A1 phases.     

Structural refinement and strengthening of an Fe–Mn–Si–Cr–Ni shape memory alloy by high-speed rolling

The shape recovery under different opposing stress conditions and the various microstructures obtained have been examined following high-speed rolling. An iron-based shape memory alloy that can hardly be rolled at a high strain rate is shown to be capable of being rolled down to 50% of its original thickness by single pass. The shape recovery under the opposing stress applied during reverse transformation is found to increase notably as a result of structural refinement induced by high-speed rolling. In these tests, the specimens were twinned or transformed into hcp and bcc nanophases by the high-speed rolling performed at strain rates as high as 10⁴ s⁻¹. The current study emphasizes the contribution of the resultant structural refinement to the strengthening of the shape memory alloy.     

Thermodynamic calculation of stacking fault energy in Fe–Mn–Si shape memory alloys

Based on thermodynamic considerations together with measurement of the stacking fault probability (Psf) by X-ray diffraction profile analysis, the stacking fault energy (SFE, γ) of austenite in Fe–Mn–Si shaped memory alloys can be estimated. For instance, the stacking fault energy of an fcc(γ) phase in an Fe–30.3Mn–6.06Si was calculated as 7.8 mJ/m². Compositional dependence of stacking fault energy in these alloys with certain composition range has also been derived as SFE(γ)=180.54+7.923 wt.% Mn–46.38 wt.% Si (J/mol), showing that the stacking fault energy increases with the addition of Mn and decreases with the addition of Si.     

Growth of Fe3O4 whiskers from solid solution nanoparticles of Fe–Cu and Fe–Ag systems produced by DC plasma jet method

Fe–Cu and Fe–Ag binary systems are virtually immiscible for a whole range of composition in equilibrium. In the present study, the nanoparticles of Fe–Cu and Fe–Ag systems were produced by direct current plasma jet method. These produced nanoparticles had mean particle sizes of about 70 nm, and were a mixture of bcc and fcc phases. It was revealed by analytical high-resolution TEM observations that the nanoparticles of Fe–Cu and Fe–Ag systems were supersaturated solid solution. It has been found that numerous whiskers with a particle on their tip grow from these nanoparticles by heating above the temperature of 860 K under an Ar–O₂ atmosphere. The whiskers grow as the result of the phase separation in these solid solutions. The whiskers are composed of a Fe₃O₄ rod and a Cu₂O particle on the tip.     

Defect structure of gold introduced by high-speed deformation

The effect of deformation speed on defect structures introduced into bulk gold specimens at 298 K has been investigated systematically over a wide range of strain rate from ′=10⁻² to 10⁶ s⁻¹. As strain rate increased, dislocation structure changed from heterogeneous distribution, so-called cell structure, to random distribution. Also, stacking fault tetrahedra (SFTs) were produced at anomalously high density by deformation at high strain rate. The anomalous production of SFTs observed at high strain rate is consistent with the characteristic microstructure induced by dislocation-free plastic deformation, which has been recently reported in deformation of gold thin foils. Thus, the results of the present study indicate that high-speed deformation induces an abnormal mechanism of plastic deformation, which falls beyond the scope of dislocation theory. Numerical analysis of dislocation structure and SFTs revealed that the transition point of variation of deformation mode is around the strain rate of 10³ s⁻¹.     

Tensile behavior change depending on the microstructure of a Fe–Cu alloy produced from rapidly solidified powder

The relationship between consolidating temperature and the tensile behavior of iron alloy produced from Fe–Cu rapidly solidified powder is investigated. Fe–Cu powder fabricated by high-pressure water atomization was consolidated by heavy rolling at 873–1273 K. Microstructural changes were observed and tensile behavior was examined. Tensile behavior varies as the consolidating temperature changes, and these temperature-dependent differences depend on the morphology of the microstructure on the order of micrometers. The sample consolidated at 873 K shows a good strength/elongation balance because the powder microstructure and primary powder boundaries are maintained. The samples consolidated at the higher temperatures have a microstructure of recrystallized grains, and these recrystallized samples show the conventional relationship between tensile behavior and grain size in ordinal bulk materials.     

Dislocation structures introduced by high-speed deformation in bcc metals

Systematic experiments were carried out over a wide range of strain rate, 10⁰–10⁶ s⁻¹, so as to reveal the deformation mode in bcc crystals, especially at high strain rate. Dislocation structure showed heterogeneous distribution at low strain rates in all three bcc metals examined. At higher strain rates exceeding 10³ s⁻¹, distribution of dislocations was random, and the formation of small dislocation loops was observed in V and Nb. In Mo, small dislocation loops were not formed by deformation, even at high strain rates. However, post-deformation annealing of an Mo specimen that had been deformed by 20% at 5×10⁵ s⁻¹ produced dislocation loops. The inside–outside contrast method identified these loops to be of vacancy type. These results reveal that in Mo vacancy clusters are not formed directly from the interaction of dislocations, but by the aggregation of vacancies. In V and Nb, the same formation process is believed to occur at high strain rates. These results suggest that the different mode of plastic deformation at high strain rates accompanied by production of vacancies also occurred in bcc metals.     

Evaluation of Stored Energy from Microstructure of Multi-component Nanostructured Cu

A polycrystalline Cu of 99.995% purity has been deformed by dynamic plastic deformation at liquid nitrogen temperature to a strain of 2.1 (LNT-DPD Cu). Three distinct regions that are dominated by dislocation slip, shear banding and nanotwinning, form a multi-component nanostructure. The microstructure of each region has been quantified by transmission electron microscopy assisted by Kikuchi line analysis. Based on the structural parameters the stored energy of each region was evaluated, and the total energy can be assumed to be a linear additivity of that in each region weighted by the respective volume fraction. A microstructure based evaluation of the stored energy of multi-component nanostructure has been proposed.     

Microstructural characterization of transformable Fe–Mn alloys at different length scales

The as-annealed and deformed Microstructure of transformable Fe–Mn alloys were, comprehensively, characterized over a wide range of length scales. Differential interference contrast optical metallography, combined with a tinting etching method, was employed to examine the grain morphology. A new specimen preparation method, involving electro-polishing and electro-etching, was developed for scanning electron microscopy and electron back-scattered diffraction analysis. This method leads to a very good imaging contrast and thus bridges the length scale gap between optical metallography and transmission electron microscopy. Moreover, it enables simultaneous scanning electron microscopy and electron backscatter diffraction analysis which allows correlations among morphology, crystal orientation and phase analysis in the length scale of microns. Transmission electron microscopy investigations were also made to evaluate the thermal and mechanical transformation products as well as defect structures.     

Structure and magnetic properties of nanocrystalline mechanically alloyed Fe–10% Ni and Fe–20% Ni

The mechanical alloying technique has been used to prepare nanocrystalline Fe–10 and Fe–20 wt.% Ni alloys from powder mixtures. The structure and magnetic properties were studied by using X-ray diffraction and hysteresis measurements, respectively. For both alloys studied, a disordered body centered cubic solid solution forms after 24 h milling time. The higher the milling time, the larger the lattice parameter. The steady-state grain size is ≈10 nm. The reduction of the grain size increases the saturation magnetization and decreases the coercivity. Nanocrystalline Fe–10 and Fe–20 wt.% Ni have been shown to exhibit a soft magnetic behavior.     

Determination of N-body potential for Fe–Cr alloy system and its application to defect study

Attempts have been made to construct the N-body potential for Fe–Cr alloy system by mixing Finnis-Sinclair potential for Fe and that for Cr under the rule for the electron density given by Ackland and Vitek and the rule for the pair term given by Johnson through the adjustment of the heat of the solution of Fe–Cr alloy and the size factor of the Cr atom in the Fe matrix to the experimental values. The obtained potential was used for the determination of the defect structures, e.g., a vacancy-Cr complex (V-Cr) and a self-interstitial atom (SIA-Cr) complex (I-Cr). The binding energy of this complex is very small, i.e., 26 meV, which is not contradictory to the experimental result, namely, less than 105 meV obtained in the muon experiment and the vacancy migration temperature obtained by the positron annihilation lifetime experiment, i.e., about 200 K for both pure Fe and Fe–Cr alloy. Calculations were made for the various types of I-Cr complexes, but mixed dumbbell type complex is not the most stable structure. The most stable configuration is the structure where Cr atom sits beside the 1 1 1 Fe crowdion and the binding energy for this structure is 0.12 eV.     

Generation of vacancies in high-speed plastic deformation

In a recent experiment, crystalline metals were subjected to high-speed plastic deformation, and subsequently a number of vacancy clusters were observed without any trace of dislocations. In an effort to explain this result, in the present study fluid-like behavior of solid in ultra-high-speed deformation is considered, and the possibility of spontaneous generation of vacancies analogous to cavitation in high-speed fluid flow is discussed. Similar to a large velocity gradient that induces turbulence in a high-speed fluid flow, large shear stress induced in a solid material during the course of high-speed deformation may generate vacancies instead of dislocations, if the dislocations cannot follow the deformation speed. In this paper, similarities between dislocation in solid and vortex in a fluid discussed, along with similarities between vacancy in a solid and cavitation in fluid, and a mechanism of vacancy production under high-speed plastic deformation of crystalline materials is proposed.     

A novel thermal treatment on a Mg–4.2Y–2.3Nd–0.6Zr (WE43) alloy

A double-stage thermal treatment has been adopted on a Mg–Y–Nd–Zr (WE43) alloy, following suggestions of a previous calorimetric investigation. A secondary precipitation is claimed to occur at a temperature as low as 150 °C after a preliminary precipitation at 210 °C, with the effect of enhancing the hardness increase and reducing the annealing times.     

Formation of vacancy clusters in deformed thin films of Al–Mg and Al–Cu dilute alloys

In the present study, vacancy clusters in elongated Al–Mg and Al–Cu thin films (Mg/Cu CONCENTRATION=0.05–1.70 at.%) were examined by electron microscopy. No dislocations were observed in these films. In Al–Mg thin films deformed at room temperature, a large number of stacking fault tetrahedra (sft) were observed alongside a few vacancy loops. The opposite was true for Al–Cu thin films, where well-grown loops predominated, and only a few sft were observed. The Al–Cu film results show that the majority of vacancies form loops larger than sft. We also deformed Al–0.05at.% (Mg or Cu) alloys in liquid nitrogen and cold-transferred to an electron microscope. In Al–Mg, a large number of dotted defects (possibly sft) were observed, while very few such defects were observed in Al–Cu. This indicates that loops observed in Al–Cu thin films deformed at room temperature, grew during/after deformation. The likely contribution of strain-induced vacancies in deformed Al thin films to the voiding in VLSI interconnect wires due to electro-migration were discussed.     

Plastic deformation of Al13Fe4 particles in Al–Al13Fe4 by high-speed compression

Spray-formed Al–Fe alloys having undergone high-speed deformation were examined under a high-voltage electron microscope. Two types of specimens were examined; one containing fine Al₁₃Fe₄ particles, and the other containing large particles. In the former specimen, deformation is found to proceed in three patterns, depending on specimen thickness and strain rate: (1) without deformation of the Al₁₃Fe₄; (2) breaking of the Al₁₃Fe₄; or (3) melting of the Al₁₃Fe₄. Local melting is found to alter some of the Al₁₃Fe₄ particles, to impart five-fold symmetry in diffraction or an amorphous structure. In the latter specimen, introduction of glide dislocations enabled us to determine a shear system in the mc102 monoclinic c2/m crystal of Al₁₃Fe₄. On the bases of these observations, the mechanism of high-speed deformation is discussed while taking into account the highly stressed and/or heated states of Al₁₃Fe₄ embedded in Al matrix.     

Positron annihilation study of vacancy-type defects in high-speed deformed Ni, Cu and Fe

Vacancies and vacancy clusters in Ni, Cu, and Fe induced by high- and low-speed deformations are studied systematically by positron annihilation techniques and are compared with those induced by the conventional-rolling. To clarify the nature of the defects, the experimental results are compared with our superimposed-atomic-charge calculations of the positron lifetimes in the vacancy clusters as a function of their size. It is found that the deformation-induced defects in the fcc and bcc metals are significantly distinct. In the fcc metals of Ni and Cu, monovacancies with high number densities are induced by the high- and low-speed deformations and by heavy conventional-rolling (>10% in Ni and >40% in Cu). Vacancy clusters are observed after the high- and low-speed deformation for Ni and after the conventional-rolling for Cu. On the contrary, dislocations and vacancy clusters are introduced in bcc Fe regardless of the type or degree of deformation.     

Effect of initial temper on the creep behavior of a Mg–Gd–Nd–Zr alloy

The effect of initial temper on the tensile creep behavior of a cast Mg–Gd–Nd–Zr alloy has been investigated. Specimens in unaged, underaged and peak-aged conditions exhibit a sigmoidal creep stage between the primary and steady-state creep stage, while the overaged specimens have no such creep stage. Transmission electron microscope observations revealed that sigmoidal creep stage was induced by the dynamic precipitation in the microstructure, and the rapid formation of β₁-phase and β-phase plates takes responsibility for the softening of material in this stage. Comparative evaluation of creep properties of the specimens showed that alloy in overaged condition had creep resistance superior to those in other conditions. Stress and temperature dependence of the steady-state creep rate were studied over a temperature range of 250–300 °C and stress range of 50–100 MPa, and a dislocation creep mechanism was proposed for the alloy.     

Microstructural study of titanium–palladium–nickel base thin film shape memory alloys

A new generation of thin film shape memory alloys has been developed with 1.65 μm thickness for micro-actuator applications. In this work, the microstructure of thin film Titanium–Palladium–Nickel (TiPdNi) shape memory alloys deposited using ion beam assisted deposition from a Ti₅₀Pd₃₀Ni₂₀ target is studied. The TiPdNi thin films were deposited with and without substrate heating during deposition. As-deposited films without substrate heating were found to be amorphous. Deposition on heated substrate produced a dense, columnar crystalline structure. Microstructures of bulk TiPdNi thin films as well as the interfacial region between the film and substrate were characterized by various techniques including transmission electron microscope, scanning transmission electron microscope, scanning electron microscope-energy dispersive X-ray spectroscopy and scanning transmission electron microscope-energy dispersive X-ray spectroscopy. A transition layer with 70 nm thickness is observed at the interface between the bulk film and silicon substrate. It is composed of three layers; two amorphous layers above the silicon substrate and a 50 nm thick twin absent layer, which was identified as B2 austenite phase by Fourier spectra analysis. In the bulk film, nano-scale grains in the range of 80–200 nm were observed. The width of twin band of the film was very narrower in the range of 5 nm.     

β to ω phase transformation due to aging in a Ti–Mo alloy deformed in impact compression

We investigated the roles of vacancies and their clusters introduced in a Ti–20mass% Mo alloy by high-speed compression in the formation of aged ω-phase crystals. Specimens were deformed by a static compression mode and a high-speed compression mode, and were then aged. The relationships between morphology of aged ω-phase crystals and deformation modes are discussed along with the roles of vacancies and their clusters in the nucleation and growth of aged ω-phase crystals. Aged ω-phase crystals were found to be smaller but of higher density in a high-speed deformation specimen. These results suggest that vacancies and their clusters easily become nucleation sites of aged ω-phase crystals. Several aged ω-phase crystals in a high-speed deformation specimen were of string-like shape. High-resolution electron microscopy confirmed that the string-like crystals have the ω-phase crystal structure. One of the roles of vacancies of and their clusters introduced by high-speed deformation is considered to be relief of compressive stress, which is predicted to arise in the course of transformation.     

Quantifying the Microstructures of Pure Cu Subjected to Dynamic Plastic Deformation at Cryogenic Temperature

A pure Cu (99.995 wt%) has been subjected to dynamic plastic deformation at cryogenic temperature to a strain of 2.1. Three types of microstructures that are related to dislocation slip, twinning and shear banding have been quantitatively characterized by transmission electron microscopy (TEM) assisted by convergent beam electron di?raction (CBED) analysis. Microstructures originated from dislocation slip inside or outside the shear bands are characterized by low angle boundaries (<15°) that are spaced in the nanometer scale, whereas most deformation twins are deviated from the perfect Σ3 coincidence (60°/<111>) up to the maximum angle of 9°. The quantitative structural characteristics are compared with those in conventionally deformed Cu at low strain rates, and allowed a quantitative analysis of the flow stress-structural parameter relationship.