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This study investigated the effect of stress-induced martensite aging under tensile and compressive stresses on the functional and viscoelastic properties in Ni50.3Ti32.2Hf17.5 polycrystals containing dispersed H-phase particles up to 70 nm in size obtained by preliminary austenite aging at 873 K for 3 h. It was found that stress-induced martensite aging at 428 K for 12 h results in the appearance of a two-way shape memory effect of −0.5% in compression and +1.8% in tension. Moreover, a significant change in viscoelastic properties can be observed: an increase in internal friction (by 25%) and a change in elastic modulus in tensile samples. The increase in internal friction during martensitic transformation after stress-induced martensite aging is associated with the oriented growth of thermal-induced martensite. After stress-induced martensite aging, the elastic modulus of martensite (EM) increased by 8 GPa, and the elastic modulus of austenite (EA) decreased by 8 GPa. It was shown that stress-induced martensite aging strongly affects the functional and viscoelastic properties of material and can be used to control them.

The research paper presents a study of the effect of stress-induced martensite aging along the [001]A-deformation axis of the sample on both elastocaloric cooling capacity and superelasticity in Ni54Fe19Ga27 single crystals in compression. It has been experimentally shown that L10-martensite stabilization after the stress-induced martensite aging enhances the superelasticity parameters for the elastocaloric performance in the studied single crystals. In the stress-induced martensite aged Ni54Fe19Ga27 single crystals, the stress level of martensite formation σMs and stress hysteresis Δσ decrease by 130 MPa and by 16–17 MPa, respectively, compared with the as-grown crystals. Therefore, the stress-induced martensite aging increases the material efficiency for solid-state cooling systems: specific adiabatic temperature change per unit stress ΔTad/σMs increases by 4.4 times (ΔTad/σMs = 291.9 K/GPa (at Т = 348 K)) and coefficient of performance reaches COP = 24.5 in stress-induced martensite aged crystals as compared with the as-grown crystals (ΔTad/σMs = 62.4 K/GPa (at Т = 348 K), COP = 21.7). Smaller stress hysteresis corresponds to less energy dissipation in an operating cycle, which is also certainly useful for optimizing elastocaloric properties of a material. Moreover, both as-grown and stress-induced martensite aged crystals demonstrate high cyclic stability during loading/unloading cycles and weak temperature dependence of the elastocaloric cooling capacity ΔТad = 10.3–11.0 K in a wide operating temperature range up to 145–197 K. Thus, stress-induced martensite aged Ni54Fe19Ga27 single crystals oriented along the [001]А- direction are expected to be promising materials for elastocaloric application.

The two-step ageing of Fe-28Ni-17Co-11.5Al-2.5Nb (at.%) single crystals under and without stress, leads to the precipitation of the γ′- and β-phase particles. Research has shown that γ–α′ thermoelastic martensitic transformation (MT), with shape memory effect (SME) and superelasticity (SE), develops in the [001]-oriented crystals under tension. SE was observed within the range from the temperature of the start of MT upon cooling Ms, to the temperature of the end of the reverse MT upon heating Af, and at temperatures from Af to 323–373 K. It was found that at γ–α′ MT in the [001]-oriented crystals, with γ′- and β-phase particles, a high level of elastic energy, ΔGel, is generated, which significantly exceeds the energy dissipation, ΔGdis. As a result, the temperature of the start of the reverse MT, while heating As, became lower than the temperature Ms. The development of γ–α′ MT under stress occurs with high values of the transformation hardening coefficient, Θ = dσ/dε from 2 to 8 GPa and low values of mechanical Δσ and thermal ΔTh hysteresis. The reasons for an increase in ΔGel during the development of γ–α′ MT under stress are discussed.

In the present study, a two-step thermo-mechanical processing consisting of cold work and heat treatment steps was performed to increase the operating temperature of 316 austenitic stainless steels. A hierarchical microstructure of thermally-stable, nano twin bands was achieved forming into bundles in elongated grains. The mechanical response of the samples with this microstructure was evaluated through uniaxial tension tests at temperatures ranging from 20 °C to 500 °C and compared with those from the fully annealed samples. The results demonstrate that such hierarchical microstructure leads to a significant increase in the elevated temperature yield strengths due to the presence of nano-twin boundaries and resulting decrease in dislocation mean free path and increase in dislocation storage capacity. In fact, the yield strength ratio of the twinned and annealed samples increases with increasing temperature up to 500 °C, indicating the effectiveness of pre-existing thermally-stable twin boundaries as the strengthening source at temperatures as high as 0.46 homologous temperature. The hierarchical microstructure also led to irregular serrations through dynamic strain aging in the stress-strain response at 500 °C, which is attributed to the bi-modal microstructural length-scales present in the structure affecting the diffusion distances during dynamic strain aging. This structure also increases the tensile strength, and without a total loss in ductility, even though the flow stress of the twinned samples surpasses the tensile strength of the annealed samples, especially at elevated temperatures. Total hardening rate is consistently higher in the twinned samples as compared to the annealed samples, indicating the positive role of nano-twin boundaries in the dislocation storage capacity at elevated temperatures. Overall, the present study clearly demonstrate the positive role of thermally stable nano-twins on the elevated temperature mechanical response of austenitic stainless steels.

A stable tensile two-way shape memory effect with a strain of (+7.0 ± 0.3) % along the [001]B2-direction upon stress-induced martensite ageing was obtained for single crystals of an Co35Ni35Al30 ferromagnetic alloy. Stress-induced martensite ageing at 398 K for 1.0 h under a compressive stress of 500 MPa along the [110]B2-direction led to the stabilization of L10-martensite variant, which contributes to sample elongation along the [001]B2-direction during stress-free cooling and reversible recovery upon subsequent heating. The tensile two-way shape memory effect was observed to be stable during stress-free thermal cycling through the phase transformation range. The characteristics of the two-way shape memory effect (reversible strain, martensitic transformation temperatures, and thermal hysteresis) did not change during 100 thermal cycles. The characteristics of the tensile two-way shape memory effect remain unchanged even after superelasticity cycling under a compressive stress of 1025 MPa applied along the [001]B2-direction at a temperature of 423 K, which is close to the stress-induced martensite ageing temperature.

The near equiatomic NiTi alloy is the most successful shape memory alloy by a large margin. It is widely and increasingly used in biomedical devices. Yet, despite having a repeatable superelastic effect and excellent shape-memory, NiTi is very far from satisfying the conditions that characterize the most reversible phase-transforming materials. Thus, the scientific reasons underlying its vast success present an enigma. In this paper, we perform rigorous mathematical derivations and accurate density-functional theory calculations of transformation mechanisms to seek previously unrecognized twinlike defects that we term involution domains, and we observe them in real space in NiTi by aberration-corrected scanning transmission electron microscopy. Involution domains lead to an additional 216 compatible interfaces between phases in NiTi, and we theorize that this feature contributes importantly to its reliability. They are expected to arise in other transformations and to alter the conventional interpretation of the mechanism of the martensitic transformation.

The main disadvantage of fcc (face-centred cubic lattice) high-entropy alloys is the low stress level at the yield point (σ0.1) at a test temperature above room temperature. This restricts their practical application at high test temperatures from 773 K to 973 K. In this study, we found that a high stress level was reached at the yield point σ0.1 ≈ G/100–G/160 (G is the shear modulus) of the [001]- and [1¯44]-oriented crystals of the Co23.36Cr23.29Fe23.80Ni21.88Al7.67 (Al0.3CoCrFeNi) high-entropy alloy (HEA) within a wide temperature range of 77–973 K under tension, due to the occurrence, of nanotwins, multipoles, dislocations under plastic deformation at 77 K and the subsequent precipitation of ordered L12 and B2 particles. It was shown that grain boundaries are not formed and the samples remain in a single-crystal state after low-temperature deformation and subsequent ageing at 893 K for 50 h. Achieving a high-strength state in the Al0.3CoCrFeNi HEA single crystals induces the orientation dependence of the critical resolved shear stresses (τcr) at T ≥ 200 K (τcr[1¯44] > τcr[001]), which is absent in the initial single-phase crystals, weakens the temperature dependence of σ0.1 above 573 K, and reduces plasticity to 5–13% in the [1¯44] orientation and 15–20% in the [001] orientation.

The oxidation behaviours of polycrystalline and monocrystalline Ni-base alloys (Ni-16Cr-8Fe (wt%)) were investigated in situ by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). The oxide layer formed is duplex: an inner chromium-rich layer and an outer layer which is rich in nickel and iron. Time evolution of the composition of inner layer from pure Cr2O3 towards spinel (NiCr2O4) was observed. The oxidation kinetics was accelerated by alloy grain boundaries, which can favour the diffusion of chromium. Both the parabolic and volatilization constants increased with increasing temperature, with kp varying from 1.9×10−3 to 1.6×10−2 nm2.s−1, and kv from 1.0×10−3 to 2.9×10−3 nm.s−1.

Near-field and far-field high-energy diffraction microscopy and microcomputed tomography X-ray techniques were used to study a bulk single crystal nickel-titanium shape memory alloy sample subjected to thermal cycling under a constant applied load. Three-dimensional in situ reconstructions of the austenite microstructure are presented, including the structure and distribution of emergent grain boundaries. After one cycle, the subgrain structure is significantly refined, and heterogeneous {\Sigma}3 and {\Sigma}9 grain boundaries emerge. The low volume and uneven dispersion of the emergent {\Sigma} boundaries across the volume show why previous transmission electron microscopy investigations of {\Sigma} grain boundary formation were inconsistent., Comment: accepted in Scripta Materialia

Modern X-ray diffraction techniques are now allowing researchers to collect long-desired experimental verification data sets that are in situ, three-dimensional, on the same length scales as critical microstructures, and using bulk samples. These techniques need to be adapted for advanced material systems that undergo combinations of phase transformation, twinning and plasticity. One particular challenge addressed in this article is direct analysis of martensite phases in far-field high-energy diffraction microscopy experiments. Specifically, an algorithmic forward model approach is presented to analyze phase transformation and twinning data sets of shape memory alloys. In the present implementation of the algorithm, the crystallographic theory of martensite (CTM) is used to predict possible martensite microstructures (i.e. martensite orientations, twin mode, habit plane, twin plane and twin phase fractions) that could form from the parent austenite structure. This approach is successfully demonstrated on three single- and near-single-crystal NiTi samples where the fundamental assumptions of the CTM are not upheld. That is, the samples have elastically strained lattices, inclusions, precipitates, subgrains, R-phase transformation and/or are not an infinite plate. The results indicate that the CTM still provides structural solutions that match the experiments. However, the widely accepted maximum work criterion for predicting which solution of the CTM should be preferred by the material does not work in these cases. Hence, a more accurate model that can simulate these additional structural complexities can be used within the algorithm in the future to improve its performance for non-ideal materials.

We present experimental results on the instrumented Vickers micro-indentation and compression of solutionized Ni-rich NiTi single crystals. The tests are conducted at room temperature where the solutionized Ti-50.9 at percent Ni material is 18 degrees above Af and the solutionized Ti-51.5 at percent Ni material is more than 100 degrees above Af. Aside from elastic deformation, it is discovered that dislocation motion and a reversible stress-induced martensitic transformation influence the micro-indentation response of Ti-50.9 at percent Ni, while the micro-indentation of Ti-51.5 at percent Ni only induces irreversible dislocation motion. The effect of the surface normal orientation on material hardness was negligible in the Ti-51.5 at percent Ni and followed trends anticipated by the activation of favorable slip systems in the Ti-50.9 at percent Ni. Compression tests on the identical Ti-50.9 at percent Ni samples revealed deformation by coupled stress-induced martensite and plastic flow, depending on the crystallographic orientation. The trends in hardness with surface normal orientation were not commensurate with the orientation dependence of the uniaxial compressive transformation or “yield” strength. The ramifications of the results in terms of comparing micro-indentation and macro-compression and the interactions between plasticity and the stress-induced martensitic transformation are discussed.

A near single-variant martensitic state of Co[Formula: see text]Ni[Formula: see text]Ga[Formula: see text] alloy was induced by a static axial stress of 66[Formula: see text]MPa. Upon application of a magnetic field pulse, the single-variant state of stressed specimen was transformed into a hierarchic martensitic structure at micron, submicron and nanometer scales. The martensitic structures, which were induced during the magnetic field pulse, did not disappear after the field was switched off. This stability of the field-induced martensitic structure is attributed to the appearance of additional twinning systems with hardly mobile twin boundaries.

Room temperature monotonic and cyclic stress–strain curves for single crystal and polycrystalline NiTi shape memory alloys containing Ti3Ni4 precipitates are presented. The tensile and compressive single crystal results illustrate the importance of crystallographic texture, the unidirectional nature of the martensitic transformation, and martensite detwinning on tension-compression stress–strain asymmetry in polycrystalline NiTi. Moreover, results on the fatigue of NiTi single crystals demonstrate the fundamental characteristics of cyclic deformation in NiTi alloys and the importance of texture on the fatigue of polycrystalline NiTi. © 2001 Elsevier Science B.V. All rights reserved.

Single crystals of NiTi (with 50.8 at.% Ni) were subjected to cyclic loading conditions at room temperature which is above the M s (martensite start) temperature of −30°C. The single crystals exhibited remarkable cyclic hardening under zero to compression strain control experiments. The stress range under strain control increased by as much as a factor of 3 in compression. The increase in stress range is primarily due to the increasing strain hardening modulus. In the tension case, loop shape changes occurred but the increase in stress range is rather small. The fatigue cycling was undertaken with a strain range of 3% which is far below the theoretical transformation strains levels exceeding 6%. The maximum stress levels reached in the experiments are below those that cause martensite slip. Therefore, the stress–strain response is governed by transformation from the austenite to the martensitic phases and the dislocation structure evolution in the austenite domains. Two single crystal orientations [148] and [112] were examined during the experiments with single and double CVP (correspondent variant pair) formations respectively. The strain hardening in compression cases is rather substantial with the stress range in the double CVP case surpassing the single CVP case. Two heat treatments were selected to produce coherent and incoherent precipitates in the microstructure respectively. The influence of the coherent precipitates on the stress–strain response is significant as they lower the transformation stress from austenite to martensite, and at the same time, they raise the flow stress of the austenite and martensite domains leading to higher saturation stresses in fatigue.

The influences of grain boundaries and relative grain misorientations on stress-induced martensitic transformations in NiTi are studied using unique experiments and finite element modeling. Tensile and compressive mechanical tests reveal that polycrystalline NiTi with a dominant fiber texture and single crystal NiTi oriented along the [111] direction exhibit nearly identical stress–strain curves during a stress-induced martensitic transformation. Micro-mechanical finite element simulations of fiber textured polycrystals and single crystals undergoing a multi-variant martensitic transformation confirm the relative indifference of the macroscopic transformation attributes to the presence of grain boundaries. On the microscale, the finite element simulations further reveal that the insensitivity of the transformation to intergranular constraint is linked to the local stress disturbance created by transforming grains. The transformation of grains that are favorably oriented with respect to the loading axis creates local stresses that invariably assist the transformation in neighboring grains, effectively lowering the influence of grain misorientations and boundaries on the macroscopic transformation behavior.

Transmission electron microscopy is used to determine the microstructures of a Ti-50.8 at% Ni alloy given different aging treatments. Two different peak-aging treatments are shown to result in disk shaped semi-coherent Ti{sub 3}Ni{sub 4} precipitates with a diameter ranging from 50 nm to 200 nm depending on the aging temperature. In the peak-aged materials, strong strain fields are clearly visible on TEM micrographs. An Eshelby based model is used to predict the local stress fields due to the differences in the lattice parameters of the precipitates and surrounding matrix. The position dependent local stress fields are then resolved onto the 24 different martensite correspondence variant pairs (CVP`s). It is further demonstrated that due to the unique orientation relationship that exists between the precipitate variants and the martensite CVP`s, the local resolved shear stresses are extremely large on some CVP`s and negligible on others. When the Ni rich NiTi is over-aged, it is found that the precipitates coarsen to approximately 1000 nm, they become in-coherent, and the local stress fields disappear. It is also determined that after over-aging in the average composition of the matrix drops from 50.8 at% Ni to approximately 50.4 at% Ni. In a subsequent paper (part 2)more » the results here are used to explain the dependence of the critical transformation stress levels and martensite start temperatures on the aging treatment.« less

An experimental study was performed to determine the effect of aging on martensitic transformations in NiTi, Polycrystalline and single crystal NiTi ([100], [110], and [111] orientations) were both considered, Stress-induced transformations in polycrystalline NiTi were found to closely resemble transformations in single crystals of the [110] and [111] orientations. Solutionized and over-aged single crystals exhibited a strong orientation dependence of the critical stress required to trigger the transformation, σcr The Schmid law was able to accurately predict the orientation dependence of σcr in the solutionized and over-aged single crystals. Peak-aged single crystals demonstrated a much weaker orientation dependence of σcr and in general, the Schmid law was not obeyed. By considering the local stress fields outside of the semi-coherent precipitates, the decrease in the orientation dependence of σcr was accounted for. The martensite start temperatures, Ms, in aged single crystal and polycrystalline NiTi were much higher than in solutionized samples In peak-aged NiTi the increase was primarily attribited to the local stress fields outside the coherent precipitates which create preferential nucleation sites for the martensite. In the over-aged NiTi the increase in Ms was primarily attributed to the decrease in the average Ni concentration of the matrix surrounding the coarsened precipitates.

Austenitic manganese steel, so called Hadfield manganese steel, is frequently used in mining and railroad frog applications requiring excessive deformation and wear resistance. Its work hardening ability is still not completely understood. Previous studies attributed the work-hardening characteristics of this material to dynamic strain aging or an imperfect deformation twin, a so-called pseudotwin. Unfortunately, these previous studies have all focused on polycrystalline Hadfield steels. To properly study the mechanisms of deformation in the absence of grain boundary or texture effects, single crystal specimens are required. The purpose of this work is the following: (1) observe the inelastic stress-strain behavior of Hadfield single crystals in orientations where twinning and slip are individually dominating or when they are competing deformation mechanisms; and (2) determine the microyield points of Hadfield single crystals and use micro-mechanical modeling to predict the stress-strain response of a single crystal undergoing micro-twinning.