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Synthesis of monodisperse CeO 2 -ZrO 2 particles exhibiting cyclic superelasticity over hundreds of cycles
Nano- and microscale CeO 2 –ZrO 2 (CZ) shape memory ceramics are promising materials for smart micro-electro-mechanical systems (MEMS), sensing, actuation and energy damping applications, but the processing science for scalable production of such small volume ceramics has not yet been established. Herein, we report a modified sol-gel method to synthesize highly monodisperse spherical CZ particles with diameters in the range of ~0.8-3.0 μm. Synchrotron X-ray micro-diffraction (μSXRD) confirmed that most of the particles are single crystal after annealing at 1450°C. Having a monocrystalline structure and a small specimen length scale, the particles exhibit significantly enhanced shape memory and superelasticity properties with up to ~4.7% compression being completely recoverable. Highly reproducible superelasticity through over five hundred strain cycles, with dissipated energy up to ~40 MJ/m 3 per cycle, is achieved in the CZ particles containing 16 mol% ceria. This cycling capability is enhanced by ten times compared with our first demonstration using micropillars (only 50 cycles in Lai et al, Science, 2013, 341, 1505). Furthermore, the effects of cycling and testing temperature (in 25°C-400°C) on superelasticity have been investigated.
Nanocrystalline strain glass TiNiPt and its superelastic behavior
TiNi-based shape-memory alloys are known to exhibit a strain glass state under certain conditions, generally in the presence of high-density defects such as excess solute atoms or alloying elements, dislocations, and nanoprecipitates. In this paper, we report a strain glass transition in a nanocrystalline Ti 50 Ni 35 Pt 15 alloy. The nanocrystalline strain glass state is achieved by a combined effect of high-density grain boundaries and high concentration doping of Pt atoms in the B2 matrix. The nanocrystalline Ti 50 Ni 35 Pt 15 strain glass alloy showed a large near-complete progressive superelasticity with a recovery strain of about 6% and a low apparent Young's modulus of about 30 GPa in a wide temperature range of over 200 °C. In situ synchrotron x-ray diffraction measurement showed that the strain glass B2 [B2(SG)] phase experienced B2(SG)→R→B19 transformation upon loading and B19→B2(SG) upon unloading. The findings of this study provide insight for the development of nanocrystalline strain glass shape-memory alloys.
Smart material based multilayered microbeam structures for spatial self-deployment and reconfiguration: A residual stress approach
Alleviation of the potentially damaging effects induced by residual stresses was comprehensively investigated in previous research. Here, this paper, however, presents a spatially self-deployable and reconfigurable multilayered microbeam which takes advantage of residual stresses and shape memory effects. Reconfigurable mechanism of a typical four-layered microbeam composed of Pt\Ni 50 Ti 50 \Ni 50 Ti 50 \Pt is introduced, followed by analytical modeling of the maximum distance of the self-deployed gap as functions of variable structural and material parameters, including compressive residual stress in Pt layers and tensile residual stress in Ni 50 Ti 50 layers. Analytical solutions given by the static model agree well with the results obtained via finite element models (FEMs). Fabrication, characterization, and in-situ experiments were carried out to validate the feasibility of deployment of the as-released four-layered microbeam. The maximum distance of the gap was measured to be 41.39 μm at 20 °C, which could be increased to 51.73 μm thanks to controllable reconfiguration driven by shape memory effects. Theoretical analysis of such self-deployment and reconfiguration suggested a tensile residual stress increase by 52 MPa in Ni 50 Ti 50 layers. The multilayered microbeam structure with capabilities of self-deployment and reconfiguration offers great potential for various emerging applications, such as micro robotics, medical drug delivery devices, and intelligent chip scale spacecraft.
Microstructure, Phase Transformation, Mechanical Behavior, Bio-corrosion and Antibacterial Properties of Ti-Nb-xSn (x = 0, 0.25, 0.5 and 1.5) SMAs
Porous Ti-Nb-xSn shape memory alloys (SMAs) are fabricated by microwave sintering technology. The microstructures exhibit needle-like morphologies, β{sub (N)} (normal straight and crossed needles along with needle-like morphology that resembles spaghetti or irregular lines with α-phases in between) as well as plate-like morphologies [normal straight plate-like morphology, α′′ and dendritic plate-like morphology, β{sub (D)}]. Increases in Sn addition significantly induce an increase in the density of the α-phase. XRD patterns exhibited three phases, namely the β-main phase with smaller intensities of α′′ and α. Further, the addition of 0.25% Sn led to more effective improvement in the intensity of the α′′-phase compared with 0.5% and 1.5% Sn addition. Additions of Sn also enhanced the fracture strength and its corresponding strain along with the shape memory effect (SME), where the best enhancement was achieved at 0.25% Sn. The corrosion rate (Ri) was reduced by rising Sn content, while both corrosion resistance and antibacterial zones were increased. The lower elastic modulus, as well as the robust mechanical properties and bioactivity, made these SMAs rather suitable for biomedical application purposes, where the low elastic modulus had value in terms of avoiding the problem of “stress shielding.”.
Effect of wheel speed and annealing temperature on microstructure and texture evolution of Ni{sub 45}Mn{sub 36.6}In{sub 13.4}Co{sub 5} ribbon
Ni{sub 45}Mn{sub 36.6}In{sub 13.4}Co{sub 5} magnetic shape memory alloy was successfully produced as preferentially textured ribbon by melting spinning with different wheel speed. X-ray diffraction (XRD) and electron back scatter diffraction (EBSD) were used to study structure and texture evolution of these melt-spun ribbons. The thickness of melt-spun ribbon is 42 μm, 65 μm and 30 μm depending on wheel speed of 1 0 m/s, 15 m/s and 20 m/s, respectively. Density of α fiber texture (〈100〉//ND) vary with wheel speed changes, and is most intensive in the ribbon with wheel speed of 15 m/s. Grains of the ribbons grow after being annealed at 873 K, 973 K, 1073 K and 1173 K, recrystallization was not observed in ribbons after being annealed at 873 K but occurred in ribbons after being annealed at higher temperatures. The α fiber texture becomes weaker to some extent after annealing at different temperatures, due to new recrystallization texture formed at the process of annealing. - Highlights: •Sectional part of shape memory ribbon is firstly investigated by EBSD method. •Thickness and texture of ribbons vary with wheel speed. •Annealing temperature affect texture and microstructure evolution greatly. •Recrystallization textures were observed in ribbons after being annealed.
Manipulation of magnetostructural transition and realization of prominent multifunctional magnetoresponsive properties in NiCoMnIn alloys
Promising multifunctional magnetoresponsive effects such as magnetoresistance, magnetostrain, and the magnetocaloric effect have recently been extensively studied in Ni-Mn-based metamagnetic shape memory alloys, but large reversible magnetoresponsive effects are usually obtained under high magnetic fields, which is an obstacle for practical applications. In this work, through manipulating magnetostructural transition, we achieved large reversible magnetoresponsive effects under a relatively low magnetic field of 3 T in a Ni-Co-Mn-In alloy. By systematically tuning the Mn/In ratio and Co substitution, an optimum composition Ni 49 Co 3 Mn 34 In 14 with a low thermal hysteresis (8 K), a narrow transformation interval (7 K) and a high sensitivity of transformation temperature to field change (6KT -1 ), was obtained. Good geometric compatibility between austenite and martensite was revealed by in situ synchrotron high-energy x-ray diffraction experiment, which accounts for the low hysteresis and narrow transformation interval. A reversible transformation between pure austenite and pure martensite is induced by a relatively low field of 3 T, which was directly evidenced by in situ neutron diffraction experiments. As a result, a large reversible magnetocaloric effect with entropy change of 16.5Jkg -1 K -1 , a large reversible magnetostrain of 0.26%, and a large reversible magnetoresistance of 60%, under a relatively low field of 3 T, were simultaneously achieved. These reversible magnetoresponsive effects are comparable to the maximum reversible values obtained under high fields in other Ni-Mn-based alloys, but the magnetic field we applied is much lower. This research may guide the design of metamagnetic shape memory alloys with low-field-induced magnetoresponsive properties for magnetic refrigeration, magnetic sensing, and magnetic recording applications.
A helical actuator driven by biased SMA: design, model, and experiment
A helical actuator driven by biased shape memory alloy (SMA) patterns embedded into a soft composite ribbon base is presented in this work. Instead of common U-shape SMA wires, a single SMA wire is woven into planar patterns, which enable helical deformation of the composite ribbon from an initially flat geometry. An analytical static model is established for accurate and rapid prediction of the helical reconfiguration arising from the shape memory effect of woven SMA patterns, followed by validation of the static model using the finite element method (FEM). The finite element results are compared with the analytical solutions given by this static model, which show a high agreement. Parametric study of the influences of eight independent design variables on the dependent helical parameters, such as combined curvatures, pitches, and helical angles, is completed. It is found that the helically deformed geometry is mainly dominated by diameters, biased positions, inclined angles, and numbers of skewed segments of the SMA wire. Fabrication and in-situ experimental test of a prototype of such helical actuators qualitatively demonstrate its dramatic three-dimensional (3D) spiral reconfiguration from a two-dimensional (2D) flat ribbon. In conclusion, such SMA patterns will allow more diverse designs of soft actuators for a wider range of robotic applications.
CRADA 2022-03 Final Report: Advanced Bearing Materials for Harsh Service Conditions
Develop advanced bearing materials for hydrogen gas turbines and wind turbines. Two candidate materials have been selected based on Ames lab’s recent work on high entropy alloys and shape memory alloys. These materials are designed to exhibit a balance of hardness, strength, toughness, and corrosion resistance. The hydrogen diffusion coefficient in the NiTi based shape memory alloy is two order of magnitude lower than that of the conventional case hardened bearing steel. We plan to atomize these materials into powders, additive manufacture cylindrical bearings, then test these bearing for rolling-contact fatigue, corrosion properties, and hydrogen embrittlement. We are a vertically integrated team comprises of national labs, bearing manufacturers, raw material powders makers, and aircraft gas turbine manufacturer.
Device and method for treatment of openings in vascular and septal walls
A device, system and method for treatment of an opening in vascular and/or septal walls including patent foramen ovale. The device has wings/stops on either end, an axis core covered in a shape memory foam and is deliverable via a catheter to the affected opening, finally expanding into a vascular or septal opening where it is held in place by the expandable shape memory stops or wings.
In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials
Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentation studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.
Tuning the temperature range of superelastic Ni-Ti alloys for elastocaloric cooling via thermal processing
Abstract Caloric cooling enlisting solid-state refrigerants is potentially a promising eco-friendly alternative to conventional cooling based on vapor compression. The most common refrigerant materials for elastocaloric cooling to date are Ni-Ti based superelastic shape memory alloys. Here, we have explored tuning the operation temperature range of Ni 50.8 Ti 49.2 for elastocaloric cooling. In particular, we have studied the effect of thermal treatments (a.k.a. aging) on the transformation temperature, superelasticity, and elastocaloric effects of Ni 50.8 Ti 49.2 shape memory alloy tubes. The isothermal compressive test revealed that the residual strain of thermally-treated Ni-Ti tubes at room temperature approaches zero as aging time is increased. Short-time aging treatment at 400 °C resulted in good superelasticity and elastocaloric cooling performance with a large tunable austenite finish ( A f ) temperature range of 24.7 °C, as determined from the A f temperature of the samples that were aged 5–120 min. The main reason of the property change is the formation of a different amount of Ni 4 Ti 3 precipitates in the NiTi matrix. Our findings show that it is possible to tailor the A f temperature range for development of cascade elastocaloric cooling systems by thermally treating a starting single composition Ni-Ti alloy.
Tungsten-loaded SMP foam nanocomposites with inherent radiopacity and tunable thermo-mechanical properties
Shape memory polymer (SMP) foams have been developed for use in neurovascular occlusion applications. These materials are predominantly polyurethanes that are known for their biocompatibility and tunable properties. However, these polymers inherently lack X–ray visibility, which is a significant challenge for their use as implantable materials. Herein, low density, highly porous shape memory polyurethane foams were developed with tungsten nanoparticles dispersed into the foam matrix, at increasing concentrations, to serve as a radiopaque agent. Utilizing X–ray fluoroscopy sufficient visibility of the foams at small geometries was observed. Thermal characterization of the foams indicated altered thermal response and delayed foam actuation with increasing nanoparticle loading (because of restricted network mobility). Mechanical testing indicated decreased toughness and strength for higher loading because of disruption of the SMP matrix. Altogether, filler addition imparted x–ray visibility to the SMP foams and allowed for tuned control of the transition temperature and actuation kinetics for the material.
A first-principles based description of the Hf-Ni system supported by high-temperature synchrotron experiments
Hf-Ni is an important binary system for high temperature alloys and shape memory alloys which has been investigated several times in the literature but often using samples of Hf contaminated by Zr. The thermodynamics of this system are remodeled in this work based on first-principles calculations and additional experiments using Hf with relatively low Zr contamination (0.25 wt. %). Diffusion couples in the Ni-rich portion of the Hf-Ni system heat treated at 1173, 1273 and 1373 K are used to measure phase stability and Hf solubility in the fcc phase. The solubility observed in fcc Ni from Ni/Ni 50 Hf 50 (at.%) diffusion couples is larger than that observed in previous experiments. These results are the only source fit to during modeling of the fcc solubility to mitigate effects from Zr contamination. Data in the literature suggests that the high temperature crystal structure of the B33 NiHf phase is, in fact, the B2 structure. High temperature synchrotron measurements provide confirmation of this crystal structure. Modeling of the B2 phase was aided by first-principles calculations using special quasi-random structures (SQS). Finally, the present CALPHAD model will prove useful when designing shape memory alloys containing Hf and when modeling the Hf activity in Ni-base high temperature alloys.
Effect of laser scanning speed on the microstructure, phase transformation and mechanical property of NiTi alloys fabricated by $\mathrm{LPBF}$
This study investigated the effects of laser scanning speed on the microstructure, phase transformation and properties of NiTi alloys fabricated by laser powder bed fusion (LPBF). In this study, the contributions of metallurgical factors under different scanning speeds, such as Ni evaporation, Ni4Ti3 precipitation, dislocations and internal stress, to the transformation temperature and transformation latent heat were clarified through specially designed experiments. Ni evaporation is found to have the most profound effect, followed by precipitation. Increasing scanning speed is found to reduce Ni loss, thus cause less increase in the transformation temperature and transformation heat of the LPBF-NiTi alloys. Increasing scanning speed also increases the microstructure non-uniformity and thus widens the transformation temperature interval. The orientations of residual stress exhibit strong crystallographic stiffness dependence. The LPBF-NiTi alloys with different scanning speeds all exhibited high strains (>13.4%) and excellent shape memory effect. A LPBF-NiTi honeycomb structure exhibited 96% shape recovery rate after a 60% pre-compressive deformation. Besides, there is an optimum scanning speed for minimum porosity and smallest average pore size. However, the pore structure is found to have weak influence on the tensile behaviour of the LPBF-NiTi alloys, possibly due to the high defect tolerance of the martensitic transformation.
Effects of deposition and annealing conditions on the crystallisation of NiTi thin films by e-beam evaporation
This Letter demonstrates the effects of deposition and annealing conditions on the crystallisation of nickel–titanium (NiTi) thin films deposited by the e-beam evaporation. NiTi thin films of 0.5 μm thick are fabricated on P-type (110) silicon substrates using the e-beam evaporation technique. We find that with the characterisations using the X-ray diffraction method, the results indicate that low e-beam deposition rate and argon employed annealing procedures can be beneficial to the formation of NiTi crystalline structure. Additionally, the as-deposited NiTi thin films without annealing procedures are amorphous, when deposited on the substrates at low temperatures. The differential scanning calorimetry studies show NiTi thin films formed by the e-beam evaporation are Ni-rich. Furthermore, SEM images illustrate that high-precision patterned NiTi thin film microstructures can be fabricated by combining with the e-beam evaporation and lift-off resist methods, without any wet or dry etching procedures. The proposed fabrication process for NiTi thin film microstructures shows great potential for application in shape memory alloy medical devices, as well as the micro-robotics.
Volatile organic compound emissions from 4D printing: Effects of material composition and external stimulus
4D printing of stimuli-responsive materials extends 3D printing by enabling the fabricated structures to transform their shapes and properties over time in response to external stimuli. Numerous research efforts have been dedicated to developing new smart materials, enhancing material printability, and ensuring time-evolving properties. Meanwhile, the use of smart materials and external stimuli in 4D printing has introduced the possibility of air emissions that can potentially deteriorate the indoor air quality at the workplace and pose continuous health hazards to users during the production and use phases. These potential air emissions caused by 4D printing have not yet been assessed in current literature, leading to unknown occupational hazards and human health effects. This study focuses on stereolithography-based 4D printing with constrained thermo-mechanics and builds an emission model to quantify the volatile organic compound emissions from printing, shape programming, and shape recovery stages. The established model mathematically links the emission characteristics with material compositional design and stimuli-response mechanisms. Additionally, shape fixity and recovery abilities are considered to analyze the trade-off between the air emissions and stimuli-response performance of 4D printed parts. Case study results suggest that the methacrylate-based thermo-responsive material with higher glass transition temperature leads to higher air emissions, surpassing the permissible exposure level in the indoor environment. By altering the thermo-temporal conditions, a 61.29% reduction in emission yield can be achieved while ensuring a satisfactory shape memory performance.
Contact Load in a Tight Thermomechanical Pipeline Joint
The contact problem for pipeline connection by means of a connector with shape memory is solved. In the solution, the actual deformation of the pipe is taken into account on the basis of the thermomechanical diagram. The thermal shape recovery of the connector is modeled. The conditions in which this approach may be employed are formulated. As an example, the contact load in a joint is determined.