Recoverable Strain Research Articles

Understanding the asymmetric orientations and stress states in polycrystalline NiTi SMA by in-situ synchrotron-based high-energy X-ray diffraction

The stress-induced martensite transformations (SIMTs) dramatically affect the recoverable strain and mechanical response of polycrystalline NiTi. An in-depth understanding of the propagation manner and orientation preference of SIMTs is therefore crucial. In this work, we present a unique asymmetric anisotropy of SIMTs and lattice strains induced by Lüders-type deformation in polycrystalline NiTi, achieved through a combination of in-situ synchrotron X-ray diffraction and uniaxial tensile loading and unloading experiments. Our experimental findings reveal that in polycrystalline NiTi under uniaxial deformation, the asymmetry of SIMTs is attributed to the inhomogeneous strain field caused by the Lüders-type mechanism. The asymmetrical SIMT starts with the forward Lüder band and disappears along with the backward Lüder band. The austenite with the favored orientation of ⟨110⟩A//loading direction (LD) transformed and recovered back at a higher rate compared to other orientations during both loading and unloading.

Heat treatment protocol for additively manufactured nitinol shape memory alloys in biomedical applications

Additive manufacturing (AM) is getting significant attention in realizing customizable nitinol (NiTi) devices for biomedical applications. However, due to the change in composition and constituent phases occurring during printing and the microstructural inhomogeneity in the printed parts, obtaining a desired set of phase transformation behaviors and superelastic properties is a major challenge. In this work, laser powder bed fusion (LPBF) was used to fabricate NiTi at a very low laser energy density (35 J/mm3) on a titanium base plate while keeping these behaviors and properties within desirable ranges without any structural defects such as crack and delamination. Our measurements showed that the as-printed NiTi exhibited distinct one-step phase transformation with the austenite finish (Af) temperature of 2.1 °C. To increase the Af temperature to 30.2 °C (within the recommended range of Af temperature for biomedical applications), a heat treatment protocol was developed, which includes a solution cycle (at 900 °C for 1 h) followed by an aging cycle (at 450 °C for 30 min). The heat treatment protocol enabled us to attain the homogenized microstructure while creating ultrafine metastable Ni-rich precipitate, Ni4Ti3, which facilitated the desirable phase transformation behavior with the increased Af temperature. The heat-treated sample showed narrower and sharper two-step martensitic phase transformation with the formation of intermediate R-phase. The presence of both Ni4Ti3 and the R-phase was confirmed by the transmission electron microscopic (TEM) analysis. In the superelasticity test at the body temperature, these samples, starting from the 2nd cycle, demonstrated a recovery ratio of more than 90% and a recoverable strain of more than 6.5%. After 10th cycles, the stable recoverable strain was 6.52% with a recovery ratio of 96%, which is the highest superelasticity reported for the LPBF processed NiTi to the best of our knowledge. After the initial deformation process, we expect these NiTi samples to attain near full superelasticity during service. The micro-hardness study also showed that the hardness of the heat-treated samples is less affected by the cyclic loading. Therefore, this paper presents a viable heat treatment protocol, which provides an important processing roadmap in making NiTi implants by AM while maintaining excellent functional properties of NiTi for biomedical applications.

Development of an Automated Experimental System for Thermomechanical and Electrical Characterization of NiTi Shape Memory Alloys

BackgroundComprehensive datasets quantifying the coupled thermo-mechanical and electrical properties of shape memory alloys (SMAs) are lacking, as are standardized techniques for robust characterization. This hampers accurate modeling and design of SMA-based components. Objective: This work develops an automated experimental system to enable simultaneous measurement of stress-strain-temperature behavior and electrical resistivity evolution in NiTi SMA wires under controlled stress conditions. Methods: Customized test frames apply precise mechanical stresses while allowing for in situ electrical measurements and infrared imaging during complete thermal cycling protocols. Specialized instrumentation including a Keithley 2002 multimeter, Agilent E3631A programmable power supply, and FLIR A615 thermal camera are integrated with LabVIEW-based software routines for complete automation of the characterization process. Rigorous metrology principles are implemented throughout the measurement procedure to improve accuracy, repeatability, and consistency compared to prior manual techniques. Results: Extensive datasets are generated which reveal pronounced stress-dependencies in key SMA material parameters including transformation temperatures, recoverable strain, and electrical resistivity. A 3D regression model describes the comprehensive relationship between resistivity, temperature, and applied stress across the entire characterization domain. Conclusions: The automated measurement framework and methodology establishes a foundation for high-fidelity, reliable acquisition of coupled SMA property data. This will enable more accurate modeling and design of components and systems incorporating SMA actuation or sensing functions.

Nondissipative Martensitic Phase Transformation after Multimillion Superelastic Cycles.

Superelastic alloys used for stents, biomedical implants, and solid-state cooling devices rely on their reversible stress-induced martensitic transformations. These applications require the alloy to sustain high deformability over millions of cycles without failure. Here, we report an alloy capable of enduring 10×10^{7} tensile stress-induced phase transformations while still exhibiting over 2% recoverable elastic strains. After millions of cycles, the alloy is highly reversible with zero stress hysteresis. We show that the major martensite variant is reversible even after multimillions of cycles under tensile loadings with a highly coherent (11[over ¯]0)_{A} interface. This discovery provides new insights into martensitic transformation, and may guide the development of superelastic alloys for multimillion cycling applications.

Creep and recovery in dense suspensions of smooth and rough colloids

We report the effect of particle surface roughness on creep deformation and subsequent strain recovery in dense colloidal suspensions. The suspensions are composed of hard-spherelike poly(methyl methacrylate) smooth (S) and rough (R) colloids with particle volume fractions ϕS = 0.64 ± 0.01 and ϕR = 0.56 ± 0.01, corresponding to a distance of 3.0% and 3.4% based on their jamming volume fractions (ϕJS=0.66±0.01, ϕJR=0.58±0.01). The suspensions are subject to a range of shear stresses (0.01–0.07 Pa) above and below the yield stress values of the two suspensions (σyS=0.035Pa, σyR=0.02Pa). During creep, suspensions of rough colloids exhibit four to five times higher strain deformation compared to smooth colloids, irrespective of the applied stress. The interlocking of surface asperities in rough colloids is likely to generate a heterogeneous microstructure, favoring dynamic particle activity and percolation of strain heterogeneities, therefore resulting in higher magnitude of strain deformation and an earlier onset of steady flow. Strain recovery after the cessation of stress reveals a nonmonotonic recoverable strain for rough colloids, where the peak recoverable strain is observed near the yield stress, followed by a steep decline with increasing stress. This type of response suggests that frictional constraints between geometrically frustrated interlocking contacts can serve as particle bonds capable of higher elastic recovery but only near the yield stress. Understanding how particle roughness affects macroscopic creep and recovery is useful in designing yield stress fluids for additive manufacturing and product formulations.

Cryogenic rolling induces quasi-linear superelasticity with high strength over a wide temperature range in TiNi shape memory alloys

Materials with high functional and strength performance are finding wide range of applications. In this study, we propose an approach to enhance the synergistic relationship between recoverable strain and strength in TiNi shape memory alloys (SMAs) by utilizing cryogenic rolling. Comparative analysis of the rolled samples, which experienced a thickness reduction of up to 13% at a nitrogen temperature, revealed good cycling stability, greater recoverable strain, reduced modulus, and increased strength at room temperature when compared to their undeformed counterparts. Notably, these rolled samples exhibited a significant recoverable strain (>4%) and impressive strength (0.8∼1.6 GPa) over a wide temperature range (∼400 K). Our findings suggest that these enhancements can be attributed to the emergence of the B19′ strain glass transition. This research not only illuminates the potential advantages of cryogenic rolling in shaping the functional and structural properties of SMAs but also offers a promising avenue for effectively regulating properties.

Fatigue-resistant NiTi micropillars with small hysteresis fabricated by micro severe plastic deformation

Through compressing polycrystalline NiTi micropillars down to a 40% height reduction by nanoindentation equipment and subsequently manufacturing them by focused ion beam, cuboidal NiTi micropillars with a nanocrystal/nanolaminate heterostructure were obtained. Mechanical behavior and fatigue tests show that the heterostructured NiTi micropillars processed by micro severe plastic deformation (MSPD) have a large recoverable strain (4.5%), small hysteresis (4.3 MPa), and ultrahigh fatigue resistance (> 106 cycles) under a maximum applied stress of 2.5 GPa. These properties were attributed to the extreme grain refinement and homogeneous phase transformation occurring in the nanocrystals. The findings suggest that the MSPD holds great potential for fabricating superior materials for applications in small-scale engineering devices.

Comparison between methods for determining the effective vertical yield stress of intermediate fine-grained soils.

Effective vertical yield stress (σ'xy) is essential in accurately describing fine-grained soils' mechanical properties and their behaviour under load over time. It helps assess settlements and stress history. In most constitutive models, this parameter indicates changes in the soil behaviour due to the development of recoverable and irrecoverable strains resulting from loading. The results of oedometric compression tests for 25 soil samples with a wide range of plasticity parameters were used for the investigation. The intermediate fine-grained soils comprised different proportions of clayey, silty and sandy fractions. An in-depth, two-staged statistical analysis was carried out to compare twelve methods of determining effective vertical yield stress, namely: Casagrande (CM), Pacheco Silva (PSM), Butterfield (BTM), Oikawa (OIM), Onitsuka (ONM), Boone (BM), Becker (WM), Morin (WPUVSM) Wang & Frost (DSEM), Tavenas (SEM), Senol (SLSEM), and Janbu (JM). It aimed to check the association of these methods and the consistency of the obtained results. Based on the difference analysis, the methods originated in the work approach (i.e. WM, WPUVSM, DSEM) and CM gave comparable σ'xy values. The methods utilised bi-logarithmic plots (i.e. BTM, OIM, ONM) received slightly greater or lesser σ'xy values than BM and JM. The remaining methods were characterised by medium to the high variability and were sensitive to even the slightest disturbances resulting from the procedure of determining σ'xy.

Microstructure and properties of a shape memory alloy Ti–Ni–Al–V fabricated by double-wire arc additive manufacturing

In this study, a novel heterogeneous double-wire arc additive manufacturing method was used for the in-situ synthesis of a novel Ti–Ni–Al–V alloy wall. The results indicated that the synthesis wall was composed of the NiTi2, B2, and Ni4Ti3 phases from the bottom to the top. With an increase in deposition layers, the Ti2Ni content decreased. The hardness at the bottom was ∼685.4 HV0.2, while that of the middle and stable regions was 553 HV0.2. The maximum compressive strength was 2100 MPa. The fracture morphology was brittle. After cyclic compression, the recoverable and unrecoverable strains were 4.79 % and 1.21 %, respectively, indicating excellent recovery characteristics.

Non-negligible role of gradient porous structure in superelasticity deterioration and improvement of NiTi shape memory alloys

Bone-mimicking gradient porous NiTi shape memory alloys (SMAs) are promising for orthopedic implants due to their distinctive superelastic functional properties. However, premature plastic deformation in weak areas such as thinner struts, nodes, and sharp corners severely deteriorates the superelasticity of gradient porous NiTi SMAs. In this work, we prepared gradient porous NiTi SMAs with a porosity of 50% by additive manufacturing (AM) and achieved a remarkable improvement of superelasticity by a simple solution treatment regime. After solution treatment, phase transformation temperatures dropped significantly, the dislocation density decreased, and partial intergranular Ti-rich precipitates were transferred into the grain. Compared to as-built samples, the strain recovery rate of solution-treated samples was nearly doubled at a pre-strain of 6% (up to 90%), and all obtained a stable recoverable strain of more than 4%. The remarkable superelasticity improvement was attributed to lower phase transformation temperatures, fewer dislocations, and the synergistic strengthening effect of intragranular multi-scale Ti-Ni precipitates. Notably, the gradient porous structure played a non-negligible role in both superelasticity deterioration and improvement. The microstructure evolution of the solution-treated central strut after constant 10 cycles and the origin of the stable superelastic response of gradient porous NiTi SMAs were revealed. This work provides an accessible strategy for improving the superelastic performance of gradient porous NiTi SMAs and proposes a key strategy for achieving such high-performance architectured materials.

Reveling the orientation preference along with localized Lüders-type deformation in polycrystalline NiTi SMA by in-situ synchrotron-based high energy X-ray diffraction

The stress-induced martensite transformations (SIMTs) in near-equiatomic NiTi shape memory alloys (SMAs) predominantly occur through localized, inhomogeneous, and intense Lüders-type mechanisms, which significantly influence the recoverable strain and mechanical response of the material. An in-depth understanding of the propagation manner and orientation preference of SIMTs is therefore crucial. In this study, we present a unique asymmetric anisotropy of SIMTs and lattice strains induced by Lüders-type deformation in polycrystalline NiTi, achieved through a combination of in-situ synchrotron X-ray diffraction and uniaxial tensile loading experiments. Our experimental findings reveal that in polycrystalline NiTi under uniaxial tensile loading, the austenite with the favored orientation of ⟨110⟩A//loading direction (LD) is consumed faster compared to other orientations, resulting in residual austenite with an orientation of ⟨431⟩//LD within the Lüders banding area. In contrast, the high-strain residual austenite with few favored orientations transforms fairly slowly and remains well beyond the transformational plateau. Our work provides valuable new insights into the microstructural nature of the Lüders-type deformation mechanism of polycrystalline NiTi, and the enhanced understanding of these complex interactions holds promise for optimizing the performance and design of SMAs in practical applications.

High-throughput membrane deflection characterization of shape memory alloy thin films

Nickel–Titanium (Ni–Ti) shape memory alloy thin films are currently gaining significant attention for small-scale systems, but device integration is still challenging due to its high compositional-dependent behavior. Therefore, it is crucial to identify the optimal parameters required to fabricate desirable samples. In this study, combinatorial high-throughput membrane deflection experiments were performed to investigate the mechanical properties of submicron-thick Ni–Ti thin films. The mechanical properties of freestanding Ni–Ti thin films, sputter-deposited with compositions and thicknesses ranging from 45.7 at. % to 52.7 at. % nickel and 270–530 nm were evaluated. With an increase in the Ni content, the crystallinity and existing phases of the films varied and exhibited an overall increasing trend of elastic modulus, transformation stress, percentage of recoverable strain and hysteresis area. Based on the obtained results, the compositional ratio of Ni–Ti films can be tailored accordingly to meet the different requirements of small-scale devices, and to then extend the employment of this high-throughput methodology in exploring advanced metallic alloys and ceramic composites.

Achieving near zero-hysteretic superelasticity in a Ni43Fe18Ga27Co12 single-crystalline microwire via Lüders-like phase transformation

Ni43Fe18Ga27Co12 single-crystalline microwires directly fabricated by the Taylor liquid drawing method show the nature of a strong first-order martensitic transformation under external stress or load-biased temperature cycling. By eliminating the nucleation energy barrier through localized plastic deformation, a fully recoverable superelastic strain approaching 11 % with negligible hysteresis is achieved in the course of tensile deformation. Based on in-situ synchrotron high-energy X-ray diffraction analysis, the mechanism of nearly non-hysteretic transformation is unraveled as a sharp, Lüders-like phase transformation. It is found that a single martensitic domain propagates continuously in a monolithic fashion under superelastic cycling with poor crystallographic compatibility of λ2 = 0.950 and small volume change of ∆V = -0.17 % accompanying martensitic transformation. We attributed such near zero-hysteretic transformation characteristics to combining conditions of low crystal defect density, high nucleation barriers but without continual nucleation events, flexibility of the microwire, and small volume change.

Grain refinement of NiTi alloys during ultrasound-assisted wire-arc directed energy deposition

ABSTRACTAchieving grain refinement in the wire-arc directed energy deposition (DED) process of NiTi alloy is highly challenging. We have successfully obtained NiTi alloy with a fine microstructure and observed an improvement in superelastic recoverability by introducing an ultrasound-assisted field during the deposition process. The results show that the average grain size of the NiTi alloy samples decreased from 147.3 to 72.2 μm. Additionally, the recoverable strain of the samples increased significantly from 3.7% to 4.4%. This is attributed to the ultrasonic cavitation and acoustic streaming phenomena during the ultrasound-assisted process, which promotes the columnar-to-equiaxed transition (CET) during the solidification process. Fundamentally, the key to the enhancement of recoverable strain after ultrasound-assisted is that the formation of equiaxial grains provides more strain compatibility to the grain boundaries, which reduces the formation of dislocations during deformation.

Oxidation-induced superelasticity in metallic glass nanotubes.

Although metallic nanostructures have been attracting tremendous research interest in nanoscience and nanotechnologies, it is known that environmental attacks, such as surface oxidation, can easily initiate cracking on the surface of metals, thus deteriorating their overall functional/structural properties1-3. In sharp contrast, here we report that severely oxidized metallic glass nanotubes can attain an ultrahigh recoverable elastic strain of up to ~14% at room temperature, which outperform bulk metallic glasses, metallic glass nanowires and many other superelastic metals hitherto reported. Through in situ experiments and atomistic simulations, we reveal that the physical mechanisms underpinning the observed superelasticity can be attributed to the formation of a percolating oxide network in metallic glass nanotubes, which not only restricts atomic-scale plastic events during loading but also leads to the recovery of elastic rigidity on unloading. Our discovery implies that oxidation in low-dimensional metallic glasses can result in unique properties for applications in nanodevices.

Time-Scaling Creep in Salt Rocks for Underground Storage

Salt is an elastoviscoplastic material that exhibits time-dependent deformation (creep). Experimental measurements of salt creep behavior help predict underground gas repositories’ long-term geomechanical behavior. Previous time-scaling creep experiments have focused on the axial strain of unconsolidated sands. i.e., time-scaling creep effects under zero lateral strain conditions without describing the creep behavior of the radial strain. In addition, the time-scaling creep of the radial and axial strain has not been investigated in salts. A comparative testing procedure and analysis method was conducted on Spindletop salt plugs using triaxial tests for multistage triaxial tests (MST) and different holding time durations and stress regimes, resulting in time-dependent strain responses (creep tests). The MST showed evolving deformational mechanisms under the mapped yield surface based on the irrecoverable to recoverable strain ratio beginning with crack closure or conformance, plasticity, and ending at early crystal surface failure. Unlike unconsolidated sands, salts showed both time and strain amplitude scaling. The axial and radial strain data show scaling behavior under low and high levels of deviatoric stress separated by a transitional period. The salt showed only an axial creep response at low deviatoric stress distally from the yield surface (one-dimesional (1D) response or zero lateral strain), which indicates negative dilatant deformation or uniaxial compaction. In contrast, the salts showed equal strain amplitude scaling factors both axially and radially at high deviatoric stress proximal to the yield surface (two-dimensional (2D) response or unconstrained boundary condition), which suggests positive dilatant deformation. Microstructural images showed accumulated creep damage under high deviatoric stress associated with parallel planes of dislocation-intergranular slip, microcracking, and compaction-induced dilational strains. The period of scaling is interpreted as regions where a single mechanism is dominating. Strain amplitude scaling for both low and high deviatoric creep stress tests provides inputs for a constitutive model of creep response in understanding the magnitude of mechanical damage associated with time-independent stress-strain curves in salts for the structural integrity of salt caverns during cyclic fluid injection and depletion.

Nanostructured Ti–Ni–Co Alloys Showing Shape‐Memory Actuation of Large Work Output at Low Temperature

In the present study, by combining the effect of point defect doping and nanostructure, low‐temperature shape‐memory alloys (SMAs) are developed showing good actuation property. The doping of Co into Ti–Ni host alloy suppresses the martensitic transformation to lower temperature. By post‐deformation annealing, the partially recrystallized state containing dense dislocations and nanoprecipitates is achieved. And, this remarkably strengthens the matrix to avoid irreversible strain under large external load. A alloy thereby exhibits a recoverable actuation strain of 4.5% under biased tensile stress of 800 MPa at temperatures below −50 °C. The work output up to outperforms most SMAs, showing a promise for low‐temperature actuator applications.

Ni–Ti multicell interlacing Gyroid lattice structures with ultra-high hyperelastic response fabricated by laser powder bed fusion

Ni–Ti alloys based on triple-periodic minimal surface lattice metamaterials have great application potential. In this work, the triply periodic minimal surface (TPMS) lattice structures with the same volume fraction from a normal Gyroid lattice to an octuple interlacing Gyroid lattice were prepared by the laser powder bed fusion (LPBF) technique. The influence of the interlacing-cell number on manufacturability, uniaxial compression mechanical behaviors, and hyperelastic responses of Ni–Ti lattice structures are analysed by experiments. The stress distributions and fracture mechanism of multicell interlacing lattice structures are illustrated by the finite element method. The obtained results reveal that when the volume fraction is the same, the specific surface area of the lattice structure increases with increasing interlacing-cell number, and the curvature radius of the single-cell strut reduces, which leads to the decrease in the manufacturability of the lattice structure. Meanwhile, the diameter of the single cell strut decreases, and the stress it can bear decreases, which leads to a decline in the compressive mechanical property of the lattice structure. However, the number of struts increases with the increase of interlacing cells, which makes the stress distribution of the lattice structure more uniform. The cyclic compression results indicate that with increasing interlacing-cell number, the proportion of the hyperelastic recoverable strain increases, and the residual strain in the cyclic compression test decreases. For the lattice structure with a chiral arrangement of single cells, the manufacturability, compressive mechanical properties, and hyperelasticity are comparable to those with a normal arrangement. Notably, the Ni–Ti Gyroid TPMS lattice structures have superior hyperelasticity properties (98.87–99.46 % recoverable strain).

Laser additive manufactured NiTi-based bioinspired helicoidal structure with excellent pseudoelasticity and energy absorption capacity

Functionality-driven biomimetic additive manufacturing (AM), as a research hotspot of 3D printing field, is providing unprecedented opportunities for developing next-generation functional materials in mechanical, electrical, optical and biomedical engineering. In this work, we developed a laser AM-ed NiTi-based helicoidal structure with excellent pseudoelasticity and energy absorption capacity, inspired by the biological architecture in the exoskeleton of the crab's claw. The rotation angle θ corresponding to the misorientation of rods in adjacent layers, as the key structure parameter, was involved into the investigations on the forming quality, pseudoelastic response and fracture behavior of the laser AM-ed helicoidal structures. The results showed that an increase in θ could improve the forming accuracy of rods but decrease the porosity due to the formation of more closed pores filled with unmelted powder particles. These pores formed by the helically stacked rods had sharp edges that could trigger earlier stress concentration and phase transformation or even strain hardening during the loading process. In views of more uniform stress distribution, the helicoidal structure with θ = 36° exhibited the largest recoverable strain of 4.32 %. Regarding the deformation and fracture behavior, it was found that the helicoidal structures with small θ were inclined to exhibit an auxetic deformation behavior and a sluggish fracture process, while the ones with larger θ were prone to a buckling deformation mode and a sudden failure. Furthermore, all helicoidal structures presented excellent energy absorption properties in terms of both unit volume and unit mass values, which could be attributed to the cross-scale hierarchical structures.

Ti30Zr10Hf10Ni35Cu15 high-entropy shape memory alloy with tunable transformation temperature and elastocaloric performance by heat treatment

This work investigates the influence of heat treatments on a pseudo-binary Ti30Zr10Hf10Ni35Cu15 high-entropy shape memory alloy. Heat treatments on the alloy resulted in the formation of second phases and thus were able to adjust its transformation temperatures. This phenomenon results from the formation of H-phase and (Zr,Hf)7Cu10 phase during low-temperature and high-temperature aging, respectively. The superelasticity of solution-treated, 500 °C-aged and 700 °C-aged samples was tested under compression, and all samples exhibited nearly 5 % recoverable strain and 15 °C elastocaloric cooling capacity. Further cyclic compression tests confirmed their stability, with up to 75 % of the initial cooling capacity retained after 5000 compression cycles. Due to its high yield strength, the Ti30Zr10Hf10Ni35Cu15 high-entropy shape memory alloy showed great superelasticity and elastocaloric performance at various testing temperatures. Furthermore, with heat treatments, the austenitic transformation finishing temperature (Af) of the alloy was tunable to between −10 °C (furnace-cooled) and 60 °C (700 °C-aged) with promising functional performance. These features expand the application range of TiZrHfNiCu high-entropy shape memory alloys as potential superelastic and elastocaloric materials.