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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 451 records · Page 25
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Experimental Validation of Numerical Simulations of a New-Generation NiTi Endodontic File Under Bending

The superelasticity of NiTi shape memory alloy has been used in endodontics since the 1990s. To study the mechanical behavior of endodontic instruments, a traditional approach consists in experimental investigations. However, finite element analysis constitutes another way to assess their mechanical behavior and to facilitate their design. The main aim of this study is to compare experimental and numerical bending results on different structures (NiTi wire, spreader, and instruments) to estimate the reliability of the finite element simulations. These investigations were carried out as follows. Firstly, experimental material parameters identification was performed using NiTi wires. These parameters were implemented in an appropriate NiTi model. Bending was numerically applied to the meshed structures generated by the finite element method. Experimental tests were performed on real structures under bending, with exactly the same loading, in order to compare experimental and numerical results. These results were in good agreement for each of the considered structures. This enabled the validation of the simulation results and the use of simulations to design new endodontic instruments.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Stability of Phase Transformation Temperatures During Cycling of Ti-15.8Nb-4.94Al-0.06Sc Shape Memory Alloy

The active ω phase formation decreases the martensitic transformation temperatures sharply and can even suppress the martensitic transformation during thermal cycling in Ti-Nb-based alloys. No ω phase is observed in the present Ti-15.8Nb-4.94Al-0.06Sc alloy when it is annealed at 650 °C for 4 h or subsequently aged at 200 and 250 °C for 2 h. The exclusion of ω phase remarkably improves the stability of phase transformation temperatures during thermal cycling. The martensitic transformation start temperature of the present alloy decreases by 30 °C but tends to be stable gradually during the 20 thermal cycles, owing to the saturation of lattice defects.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Superelasticity by reversible variant reorientation in a Ni-Mn-Ga microwire with bamboo grains

The link between microstructure and mechanical properties is investigated for a superelastic Ni–Mn–Ga microwire with 226 μm diameter, created by solidification via the Taylor method. The wire, which consists of bamboo grains with tetragonal martensite matrix and coarse γ precipitates, exhibits fully reversible superelastic behavior up to 4% tensile strain. Upon multiple tensile load–unload cycles, reproducible stress fluctuations of ~3 MPa are measured on the loading superelastic stress plateau of ~50 MPa. During cycles at various temperatures spanning -70 to 55 °C, the plateau stress decreases from 58 to 48 MPa near linearly with increasing temperature. Based on in situ synchrotron X-ray diffraction measurements, we conclude that this superelastic behavior is due to reversible martensite variants reorientation (i.e., reversible twinning) with lattice rotation of ~13°. The reproducible stress plateau fluctuations are assigned to reversible twinning at well-defined locations along the wire. The strain recovery during unloading is attributed to reverse twinning, driven by the internal stress generated on loading between the elastic γ precipitates and the twinning martensite matrix. Lastly, the temperature dependence of the twining stress on loading is related to the change in tetragonality of the martensite, as measured by X-ray diffraction.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Acoustic emission analysis of cyclically loaded superelastic shape memory alloy fiber reinforced mortar beams

Superelastic shape memory alloys (SMAs) are metallic alloys that can recover their nonlinear deformations upon unloading. The use of SMAs in cementitious composites as fibers can enable crack recovery and re-centering capabilities. In this study, the crack recovery characteristics of SMA fiber reinforced mortar specimens subjected to flexural cyclic loading are studied through acoustic emission analysis. SMA fiber reinforced mortar specimens with fiber volume ratios of 0.3%, 0.5% and 1.0% are tested under cyclic flexural loads. Acoustic emissions (AE) signals are captured and analyzed to characterize the crack formation and crack width development at each cycle of loading. In addition, the crack width propagation of the specimens is monitored by Digital Image Correlation measurement system and is used as a basis in AE analyses. Results show that the SMA fiber reinforced mortars exhibit considerable re-centering and crack recovery characteristics at large deformation amplitudes.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Phase transformation during mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si alloys

Mechano-synthesis of Fe–32Mn–6Si alloy by mechanical alloying of the elemental powder mixtures was evaluated by running the ball milling process under an inert argon gas atmosphere. In order to characterize the as-milled powders, powder sampling was performed at predetermined intervals from 0.5 to 192 h. X-ray florescence analyzer, X-ray diffraction, scanning electron microscope, and high resolution transmission electron microscope were utilized to investigate the chemical composition, structural evolution, morphological changes, and microstructure of the as-milled powders, respectively. According to the results, the nanocrystalline Fe–Mn–Si alloys were completely synthesized after 48 h of milling. Moreover, the formation of a considerable amount of amorphous phase during the milling process was indicated by quantitative X-ray diffraction analysis as well as high resolution transmission electron microscopy image and its selected area diffraction pattern. It was found that the α-to-γ and subsequently the amorphous-to-crystalline (especially martensite) phase transformation occurred by milling development. - Graphical abstract: Mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si shape memory alloys in the powder form: amorphous phase formation, α-to-γ phase transformation, mechano-crystallization of the amorphous, and martensite phase formation during the process. Highlights: • During MA, the α-to-γ phase transformation and amorphization occurred. • Mechano-crystallization of the amorphous phase occurred at sufficient milling time. • The formation of high amount of ε-martensite was evidenced at high milling times. • The platelet, spherical, and then irregular particle shapes was extended by MA. • By MA, the particles size was increased, then reduced, and afterward re-increased.

36 MATERIALS SCIENCE↗
DOE OSTI2014

In situ X-ray diffraction strain-controlled study of Ti–Nb–Zr and Ti–Nb–Ta shape memory alloys: crystal lattice and transformation features

Phase and structure transformations in biomedical Ti–21.8Nb–6.0Zr (TNZ) and Ti–19.7Nb–5.8Ta (TNT) shape memory alloys (at.%) under and without load in the − 150 to 100 °S temperature range are studied in situ using an original tensile module for a low-temperature chamber of an X-ray diffractometer. Alpha″- and beta-phase lattice parameters, the crystallographic resource of recovery strain, phase and structure transformation sequences, and microstress appearance and disappearance are examined, compared and discussed. For both alloys, the crystallographic resource of recovery strain decreases with temperature increase to become 4.5% for TNZ and 2.5% for TNT alloy (at RT). Loading at low temperatures leads to additional α″-phase formation and reorientation. Heating under load, as compared to strain-free heating, affects the reverse transformation sequence of both alloys in different ways. For TNZ alloy, strain-free heating results in simultaneous ω→β and α″→β transformations, whereas during heating under stress, they are sequential: β + ω→α″ precedes α″→β. For TNT alloy, strain-free heating results in reverse α″→β transformation, whereas during heating under stress, α″→β transformation is preceded by α″-phase reorientation. - Highlights: • Comparative in situ XRD analysis of Ti–Nb–Zr(Ta) shape memory alloys is realized. • Lattice parameters of β- and α″-phases are calculated in the − 150 to + 100 °C range. • The higher the temperature, the lower the α″→β transformation strain. • Loading at low temperatures results in α″-phase formation and reorientation. • Transformation sequences upon heating with and without loading are different.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Microstructure of selective laser melted nickel–titanium

In selective laser melting, the layer-wise local melting of metallic powder by means of a scanning focused laser beam leads to anisotropic microstructures, which reflect the pathway of the laser beam. We studied the impact of laser power, scanning speed, and laser path onto the microstructure of NiTi cylinders. Here, we varied the laser power from 56 to 100 W and the scanning speed from about 100 to 300 mm/s. In increasing the laser power, the grain width and length increased from (33 ± 7) to (90 ± 15) μm and from (60 ± 20) to (600 ± 200) μm, respectively. Also, the grain size distribution changed from uni- to bimodal. Ostwald-ripening of the crystallites explains the distinct bimodal size distributions. Decreasing the scanning speed did not alter the microstructure but led to increased phase transformation temperatures of up to 40 K. This was experimentally determined using differential scanning calorimetry and explained as a result of preferential nickel evaporation during the fabrication process. During selective laser melting of the NiTi shape memory alloy, the control of scanning speed allows restricted changes of the transformation temperatures, whereas controlling the laser power and scanning path enables us to tailor the microstructure, i.e. the crystallite shapes and arrangement, the extent of the preferred crystallographic orientation and the grain size distribution. - Highlights: • Higher laser powers during selective laser melting of NiTi lead to larger grains. • Selective laser melting of NiTi gives rise to preferred <111> orientation. • The observed Ni/Ti ratio depends on the exposure time. • Ostwald ripening explains the bimodal grain size distribution.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Study of the microstructure evolution of heat treated Ti-rich NiTi shape memory alloy

Martensitic evolution in Ti-rich NiTi alloy, Ti50.5Ni49.5, has been investigated as a function of annealing, solution treatment and a combination thereof and a detailed electron microscopic investigation carried out. Self-accommodated martensite plates resulted in all heat treated samples. Martensitic < 011 > type II twins, which are common in NiTi shape memory alloys, was found in both as-received and heat-treated samples. Solution treated samples, additionally, showed {11-1} type I twinning was also found in samples that have been annealed after solution-treatment. Another common feature of the microstructure in both as-received and heat treated samples is the formation of Ti{sub 2}Ni precipitates. The size, number and dispersions of these precipitates can be controlled by resorting to a suitable heat treatment e.g. solution treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Influence of the microstructure on the resulting 18R martensitic transformation of polycrystalline Cu−Al−Zn thin films obtained by sputtering and reactive annealing

We report the influence of the microstructure on the martensitic transformation in polycrystalline Cu−Zn−Al thin films with 18R structure. The films are grown in two steps. First, Cu−Al thin films are obtained by DC sputtering. Second, the Zn is introduced in the Cu−Al thin films by the annealing them together with a bulk Cu−Zn−Al reference. The crystalline structure of the films was analyzed by X-ray diffraction and transmission electron microscopy. The martensitic transformation temperature was measured by electrical transport using conventional four probe geometry. It was observed that temperatures above 973 K are necessary for zincification of the samples to occur. The resulting martensitic transformation and its hysteresis (barrier for the transformation) depend on the grain size, topology and films thickness. - Highlights: • Polycrystalline Cu−Al−Zn thin films with nanometric grain size are sintered. • Influence of thermal annealing process on the microstructure is analyzed. • Martensitic transformation of Cu−Al−Zn thin films is strongly affected by the microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of the microstructures and the shape memory properties of the Fe-Mn-Si-Cr-Ni-C shape memory alloy after severe plastic deformation by differential speed rolling and subsequent annealing

Highlights: • The Fe-SMA was subjected to severe plastic deformation and then annealed. • Recovery strain increased with increasing grain size. • An optimum grain size existed for the largest recovery stress. • Grain reduction is useful for having a high recovery stress. - Abstract: The Fe-13.51Mn-4.82Si-8.32Cr-3.49Ni-0.15C shape memory alloy was subjected to severe plastic deformation by high-ratio differential speed rolling and subsequent annealing (between 873 and 1373 K) to find the factors that affect recovery stress and recovery strain. As the annealing temperature increased (i. e., as grain size increased), the recovery strain increased. This was attributed to decrease in the density of grain boundaries and the density of twins with increasing grain size. The recovery stress, however, showed a different behavior. It increased with annealing temperature up to 973 K, at which an ultrafine grain size near 1.6 μm was obtained, and then decreased with further increase in the temperature. The difference between the recovery strain and the plastic strain induced by recovery stress under constrained displacement during cooling was proposed to determine the amount of recovery stress. There was an optimum grain size for the largest difference between the recovery strain and the plastic strain. The current study shows that grain-size reduction is not good for having a high recovery strain but it is beneficial for having a high recovery stress in the Fe-Mn-Si shape memory alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The shape recovery conditions for Fe–Mn–Si alloys: An interplay between martensitic transformation and plasticity

Highlights: • Fe15Mn5Si9Cr5Ni samples were rolled at 800 °C and annealed at 650 (C1) and 1000 °C (C2). • TEM analysis was performed. • High density of stacking faults and appropriate density of dislocation appears in C1. • Complex dislocation arrays due to plastic deformation are observed in C2. • Shape memory properties depend on the thermomechanical treatment. - Abstract: This work analyses the improvement of the shape memory properties of Fe-Mn-Si based alloys, and expands upon and deepens recently published developments concerning this topic. We prepared TEM specimens from a Fe-15Mn-5Si-9Cr-5Ni sheet rolled at 800 °C and annealed at 650 °C–92% shape recovery – and from another sheet annealed at 1000 °C–45% shape recovery. Here, we analyse the development of microstructure during the γ ↔ ε martensitic transformation and correlate it with the shape memory behaviour. Among the observed microstructural features, the introduction of complex dislocation arrays due to plastic deformation appears to be critical for shape memory development, since they can arrest the backward movement of Shockley partial dislocations over the original path. Tailoring the microstructure in order to introduce a high stacking-fault density accompanied by an appropriate dislocation density remains a key issue in the design of these kinds of functional materials.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Recrystallization and martensitic transformation in nanometric grain size Cu-Al-Ni thin films grown by DC sputtering at room temperature

Highlights: • Polycrystalline Cu-Al-Ni thin films with nanometric grain size are grown by DC sputtering. • Influence of thermal annealing process at low temperatures on the microstructure is analyzed. • Strained martensitic transformation is observed for films with grain size average of 30 nm. - Abstract: We report the recrystallization of metastable hexagonal and body centered cubic BCC phase in free-standing 6 μm thick Cu-Al-Ni films grown by DC sputtering at room temperature. The results show that the BCC phase recrystallizes to L2{sub 1} at around 533 K together with precipitation of γ{sub 2}-phase. Annealing temperatures (533 K–623 K) at short times (0–30 min) produce systematic increment of the fraction of γ{sub 2}-phase. Films with phase coexistence of hexagonal, γ{sub 2} and L2{sub 1} structure display temperature driven martensitic transformation. This transformation is observed for samples with austenite grain size of around 30 nm. In all cases, the martensitic transformation temperature (M{sub S}) notoriously decreases (compared to bulk) and systematically increases with the annealing temperatures and annealing time. In addition, the films display extended transformation and retransformation ranges along with asymmetric hysteresis, which may be associated to restitutive forces due to elastic deformations at martensite – martensite and martensite – austenite interfaces. Annealing temperatures above 623 K produce fast precipitation to equilibrium α- and γ{sub 2}-phases. The austenitic phase can be recovered after annealing over 1000 K and fast quenching in ice-water.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Martensite crystal structure in Ru-based high temperature shape memory alloys

Highlights: • A three level twinned microstructure is recognized in the β″ phase. • Wavy contrast boundaries which are typical for translation interfaces • Displacements are translations of tetragonal β′ phase, lost during transformation. • Six times bigger monoclinic cell is characterized by the disappearance of 5 translations. - Abstract: High temperature shape memory alloys RuNb and RuTa were investigated by X-ray diffraction in order to determine the structure of the low temperature β” martensite. Powder X-ray diffraction and Rietveld analysis confirm the monoclinic symmetry and allow a precise determination of the atom positions. The low temperature microstructure is the result of a martensitic transformation from a tetragonal β′ martensite. The analysis of how it is controlled by the space groups of the two phases and by their relative orientation is performed by transmission electron microscopy. A three level twinned microstructure is recognized in the β” phase. The investigation at the smallest scale twins reveals the presence of wavy contrast boundaries which are typical for translation interfaces. High resolution transmission electron microscopy images, accompanied by phase contrast imaging analysis, have been used to determine the translation vectors associated to the interfaces. These displacements are the translations of the tetragonal β′ phase which are lost during the transformation. The combination of X-ray diffraction and transmission electron microscopy investigation allows the suggestion of a global distortion mechanism that explains the atomic displacements in the β” form.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Thermodynamic constitutive model for load-biased thermal cycling test of shape memory alloy

Graphical abstract: - Highlights: • Thermodynamic calculation model for martensitic transformation of shape memory alloy was proposed. • Evolution of the self-accommodation was considered independently by a rate-dependent kinetic equation. • Finite element calculation was conducted for B2–B19′ transformation of Ti–44.5Ni–5Cu–0.5 V (at.%). • Three-dimensional numerical results predict the macroscopic strain under bias loading accurately. - Abstract: This paper presents a three-dimensional calculation model for martensitic phase transformation of shape memory alloy. Constitutive model based on thermodynamic theory was provided. The average behavior was accounted for by considering the volume fraction of each martensitic variant in the material. Evolution of the volume fraction of each variant was determined by a rate-dependent kinetic equation. We assumed that nucleation rate is faster for the self-accommodation than for the stress-induced variants. Three-dimensional finite element analysis was conducted and the results were compared with the experimental data of Ti–44.5Ni–5Cu–0.5 V (at.%) alloy under bias loading.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Investigations on the electronic, structural, magnetic properties related to shape-memory behavior in Ti{sub 2}CoX (X=Al, Ga, In)

Highlights: • The analysis of phase stability trend is studied for Ti{sub 2}CoX(X = Al, Ga, In). • Ti{sub 2}CoGa is more suitable as shape memory alloy. • Total magnetic moments disappear with a increase of c/a ratio for all systems. • Density of states at the Fermi level are also shown. - Abstract: Using the full-potential local orbital minimum-basis method, we have performed a systematic investigations on the electronic, structural, and magnetic properties related to shape memory applications for Ti{sub 2}CoX (X=Al, Ga, In) alloys. Our results confirm that these alloys are half-metallic ferromagnets with total magnetic moment of 2μ{sub B} per formula unit in austenite phase, and undergo a martensitic transformation at low temperatures. The relative stabilities of the martensitic phases differ considerably between Ti{sub 2}CoX (X=Al, Ga, In). Details of the electronic structures suggest that the differences in hybridizations between the magnetic components are responsible for trends of phase. Quantitative estimates for the energetics and the magnetizations indicate that Ti{sub 2}CoGa is a promising candidate for shape memory applications.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Design and Synthesis of Selective Phosphodiesterase 4D (PDE4D) Allosteric Inhibitors for the Treatment of Fragile X Syndrome and Other Brain Disorders

Novel pyridine- and pyrimidine-based allosteric inhibitors are reported that achieve PDE4D subtype selectivity through recognition of a single amino acid difference on a key regulatory domain, known as UCR2, that opens and closes over the catalytic site for cAMP hydrolysis. The design and optimization of lead compounds was based on iterative analysis of X-ray crystal structures combined with metabolite identification. Selectivity for the activated, dimeric form of PDE4D provided potent memory enhancing effects in a mouse model of novel object recognition with improved tolerability and reduced vascular toxicity over earlier PDE4 inhibitors that lack subtype selectivity. The lead compound, 28 (BPN14770), has entered midstage, human phase 2 clinical trials for the treatment of Fragile X Syndrome.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2013

Extended investigation of intermartensitic transitions in Ni-Mn-Ga magnetic shape memory alloys: A detailed phase diagram determination

Martensitic transitions in shape memory Ni-Mn-Ga Heusler alloys take place between a high temperature austenite and a low temperature martensite phase. However, intermartensitic transformations have also been encountered that occur from one martensite phase to another. To examine intermartensitic transitions in magnetic shape memory alloys in detail, we carried out temperature dependent magnetization, resistivity, and x-ray diffraction measurements to investigate the intermartensitic transition in Ni{sub 50}Mn{sub 50–x}Ga{sub x} in the composition range 12≤x≤25 at. %. Rietveld refined x-ray diffraction results are found to be consistent with magnetization and resistivity data. Depending on composition, we observe that intermartensitic transitions occur in the sequences 7M→L1{sub 0}, 5M→7M, and 5M→7M→L1{sub 0} with decreasing temperature. The L1{sub 0} non-modulated structure is most stable at low temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Texture evolution during nitinol martensite detwinning and phase transformation

Nitinol has been widely used to make medical devices for years due to its unique shape memory and superelastic properties. However, the texture of the nitinol wires has been largely ignored due to inherent complexity. In this study, in situ synchrotron X-ray diffraction has been carried out during uniaxial tensile testing to investigate the texture evolution of the nitinol wires during martensite detwinning, variant reorientation, and phase transformation. It was found that the thermal martensitic nitinol wire comprised primarily an axial (1{sup ¯}20), (120), and (102)-fiber texture. Detwinning initially converted the (120) and (102) fibers to the (1{sup ¯}20) fiber and progressed to a (1{sup ¯}30)-fiber texture by rigid body rotation. At strains above 10%, the (1{sup ¯}30)-fiber was shifted to the (110) fiber by (21{sup ¯}0) deformation twinning. The austenitic wire exhibited an axial (334)-fiber, which transformed to the near-(1{sup ¯}30) martensite texture after the stress-induced phase transformation.

36 MATERIALS SCIENCE↗