Characterization and modeling of three-dimensional self-healing shape memory alloy-reinforced metal-matrix composites
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An in-situ nanowire Nb/TiNiCu composite is fabricated based on the concept of strain under-matching between a phase transforming matrix and high strength nanomaterials. The deformation behavior of the Nb nanowire was investigated by means of in-situ synchrotron X-ray diffraction when the TiNiCu matrix underwent different deformation modes. The maximum lattice strain of the Nb nanowires was about 5% when the matrix deformed via martensitic transformation or 1% when deforming plastically by dislocation slip. As a result, the Nb nanowires showed a lattice strain of 3.5% when the matrix deformed in the mixed mode of plastic deformation and martensitic transformation, which means that the occurrence of plastic deformation does not impede load transfer from the matrix to the nanowires.
Cold embrittlement is one of the primary concerns challenging the usage of steels in infrastructures like pipelines and ocean platforms. This challenge is also compounded by the limited selection of materials for application in a cold and corrosive environment. Inspired by recent progresses in developing gradient structured materials with extraordinary properties, in this paper we report a class of stainless steels with gradient phase structures achieving a superb combination of strength (1753 MPa) and tensile ductility (>25%) at the cryogenic temperature of 77 K. A set of cylindrical steel samples acquire a graded mixture of hard martensitic and soft austenitic phases through pre-torsion, which results in an optimal stress partition in the material - the hard martensitic structures showing a positive density gradient from core to edge carry higher stress near the edge, while the soft austenitic phase showing a negative density gradient from core to edge serves to retain substantial tensile ductility. Finally, the phase-transformation at low temperature in gradient structures and the resulted work-hardening could be adopted to enhance the ductility and strength of widely used engineering materials for their applications in harsh environment.
We report there are abundant studies on deformation mechanisms in metallic materials dominated by grain boundaries and twin boundaries. In comparison, the influence of stacking faults on deformation mechanisms of materials remains less well understood. Recent studies have shown that when the density of stacking faults increases sharply, their influence on mechanical behavior of metallic or ceramic materials becomes prominent, and in fact, dominates in some cases. This article reviews recent research progress on how nanoscale stacking faults impact the mechanical behavior of metallic and ceramic materials. We primarily focus on studies that reveal the formation of pre-existing stacking faults, their interactions with dislocations, and phase transformations during plastic deformation as evidenced by experiments and simulations. The aim of this review is to highlight the potential opportunities in using stacking faults to tailor the deformation mechanisms of advanced materials.
Substantial residual tensile stress tends to accumulate in currently available high-Cr ferritic martensitic steels that are subjected to cyclical heat treatment, which leads to premature brittle fracture. By tailoring the alloy composition, this thermal cycling can be exploited to induce a high number density of nanoprecipitates and phase transformations countering residual tensile stresses. In this work, three new variants of ferritic-martensitic steels have been designed with computational thermodynamics to meet the goals of mitigating residual tensile stresses by lowering martensite start temperatures and of enhancing mechanical strength and irradiation sink strength by increasing the number density of nanoprecipitates. Furthermore, ctenast materials were subjected to cyclical heat treatment. The thermally cycled samples were evaluated with mechanical testing and microstructural analysis to identify the optimal composition in which figures of merit include low residual stress and a high density of nanoscale MX (M = metal, X = C/N) precipitates, leading to high yield strength with reasonable ductility. The noticeably higher density of nanoprecipitates in the optimal alloy favor its higher yield strength, which is supported by the microstructure-derived yield strength calculation and precipitation kinetics simulation.
Multi-principal-element alloys (also known as medium and high entropy alloys) offer a much larger and richer design space than conventional alloys, providing opportunities for discovering new functionalities and their governing physics. Some of these alloys exhibit an outstanding combination of high strength and ductility, linked to the activation of various deformation modes triggered by low-energy stacking faults. However, a pressing question remains: Is the plasticity of medium- and high-entropy alloys governed only by stacking fault energy, or does atomic short-range order (SRO) play a role? Here, to answer this, we investigated how SRO affects the deformation in single-crystalline NiCoCr, with previous contradictory findings. First, we established unique experimental evidence for SRO formation in bulk single crystals using high-energy synchrotron transmission X-Ray Diffraction. By tuning the degree of SRO by aging at high temperatures, twinning density and strain-induced martensitic phase transformation can be significantly increased in the [110] and [111] orientations under tension, increasing the tensile ductility; yet, no increase was observed along the [001] orientation due to lack of TWinning-Induced Plasticity (TWIP) or TRansformation-Induced Plasticity (TRIP), indicating a strong crystallographic orientation dependence. Our first-principles thermodynamic calculations unequivocally show SRO exists and governs the observed microstructural evolution and deformation hardening behavior. Here we find direct proof that SRO triggers a simultaneous TWIP and TRIP in NiCoCr, a rare microstructural evolution path. Our findings establish that the interplay of SRO and plasticity could be exploited to alter deformation modes and yield unprecedented mechanical response in medium- and high-entropy alloys.
This study investigates the influence of an applied magnetic field on the microstructural evolution and mechanical properties of hypoeutectoid steels subjected to heat treatment. Tensile tests and microstructural analysis were performed on samples processed under varying magnetic field strengths (0 T, 5 T, and 9 T) and different austenitization incubation times. The results indicate that the application of a magnetic field alters the fraction of proeutectoid ferrite phase without changing the cooling rates and heat treatment process. Additionally, pearlite microstructural features such as lamellar spacing and misorientation angles exhibit variations under different field strengths. While the pearlite nodule diameter remains largely unaffected, an increase in percentage elongation and strength is observed in the 5 T treated sample, attributed to changes in microstructural features with the magnetic field. Additionally, the percentage elongation is reduced in the samples heat treated with reduced austenitization incubation times. The study further demonstrates that low-angle misorientations increased in the samples taken parallel to the magnetic field direction, influencing the mechanical response. These findings suggest that applying a magnetic field during heat treatment provides an additional driving force for phase transformations, offering a manufacturing process for tailoring microstructures and optimizing mechanical properties. Moreover, integrating magnetic fields in heat treatment processes has potential benefits in energy efficiency.
The feasibility of depositing a thin film of highly concentrated alloy on zircaloy-4 substrates at low temperatures was investigated. Electron microscopy characterisation at micro and nanoscales showed that the deposited thin film is near-equiatomic, single-phase and with all alloying elements uniformly distributed throughout the microstructure. Heavy-ion irradiations carried out in situ within a transmission electron microscope displayed the generation of both defect clusters and inert gas bubbles at around 1.5 × 10 16 ions·cm –2 (15.4 dpa). Post-irradiation characterisation demonstrated that the thin film preserved its solid solution and that, under the studied conditions, no elemental segregation or phase transformations were observed, indicating a high radiation tolerance.
This feasibility study examines the additive manufacturing of Ti–48Al–2Cr–2Nb preforms in a quest to make more complex engine components from this promising but hard to machine, brittle material. The preforms are built using the electron beam melting technique; hot isostatic pressing (HIP) was performed as the only post-process. Microstructural characterizations were carried with scanning electron microscopy techniques, X-ray diffraction and X-ray computed tomography while mechanical properties were obtained via tensile testing. We exploited computational thermodynamic modeling (widely known as CALPHAD) approach to investigate the phase stability pertinent to Nb and Cr modified TiAl. Defect-free structures were obtained in the HIPed condition with mechanical behavior comparable to/better than traditionally manufactured counterparts. Equiaxed duplex microstructures were achieved in the as-built condition that were sustained post-HIP. The effect of the build conditions and phase transformation kinetics on the observed microstructures is discussed. Furthermore, the microstructure-mechanical behavior relationship is also discussed.
Advancing a mechanistic understanding of the colloidal to solid-phase transformations of silica allows us to tune these meso-scale structures. In this study, we probe the structural transformations associated with the formation of mesoporous silica particles, SBA-15 using in-operando Small Angle X-ray Scattering (SAXS) and Grazing Incidence-Small Angle X-ray Scattering (GI-SAXS). The chemical transformations associated with the hydrolysis and condensation of silica particles is investigated using Attenuated Total Reflection – Fourier Transform Infrared Spectroscopy (ATR-FTIR) measurements. Fast polymerization of Si-O-Si species to form mesoporous silica is noted when SBA-15 is synthesized in the presence of nitrate salts, due to the “salting-in” effect or enhanced solubility of polymers. However, aging the silica particles resulted in plate-like morphologies in the absence of the nitrate salt and spherical morphologies in the presence of nitrate salt. Early onset of nucleation of silica particles in the presence of nitrate salts was captured using GI-SAXS measurements. These studies show that the rational basis for developing new synthesis routes for accelerated kinetics or specific meso-scale structures can be informed by detailed characterization of the evolution in chemistry and meso-scale structure of these materials.
Alkali metal ion intercalation into layered transition-metal dichalcogenide structures is a promising approach to make next generation rechargeable batteries for energy storage. It has been noted that the number of Na-ions which can be reversibly intercalated and extracted per MoS 2 is limited, and the chemical and electrochemical processes/mechanisms remain largely unknown, especially for nano-sized materials. Here, in this study, sodiation of MoS 2 nanosheets are studied by in-situ electron diffraction and the phase transformations in sodiation are identified with the aid of DFT calculations to reveal the reaction mechanism. Several thermodynamically stable/metastable structures are identified in the sodiation pathway of MoS 2 nanosheets, previously unnoticed in bulk MoS 2 . The gradual reduction of Mo 4+ upon Na-ion intercalation leads to a transition of the Mo-S polyhedron from a trigonal prism to an octahedron around 0.375 Na per MoS 2 inserted (i.e. Na 0.375 MoS 2 ). When the intercalated Na-content is larger than 1.75 per MoS 2 structural unit (i.e. Na 1.75 MoS 2 ), the MoS 2 layered structure collapses and the intercalation reaction is replaced by an irreversible conversion reaction with the formation of Na 2 S and metal Mo nanoparticles. The calculated sodiation pathways reproduce the experimental sodiation voltages. The current observations provide useful insights in developing sodium-ion batteries with high cycling stability.
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Here, the layered NaTMO 2 (TM = Ni, Fe, Mn) materials with the O3-type structure are attractive as positive electrodes for sodium ion batteries because of their high theoretical capacity. Additionally, Li doping in these materials has been shown to offer substantial enhancements to their electrochemical properties by promoting the formation of intergrowth structures, which are combinations of specific phases. However, the mechanism by which the intergrowth modifies the electrochemical properties is often unclear. Systematic variation of Li content in Na x Li y Ni 0.4 Fe 0.2 Mn 0.4 O 2 (NFM-Li y ) was conducted to identify its role in structural modification and electrochemical performance. Li contents of 0.15 and greater generate a layered/layered Na-O3/Li-O’3 intergrowth structure. 7 Li and 23 Na nuclear magnetic resonance and x-ray absorption spectroscopy identify that when the total solubility for alkali ions in the layered structure is exceeded, Li continues to form the Li-O’3 phase while the excess Na forms residual sodium compounds such as Na 2 O. Higher Li content is associated with improved capacity retention in the initial cycles from the superior stability of the mechanically linked NaO3/Li-O’3 structure that suppresses the P3 to OP2 phase transition during charge. However, high Li contents are associated with increased rates of parasitic side reactions that reduce long-term cycling stability. These side reactions are associated with the instability of the cathode-electrolyte interphase, which can be partially mitigated by atomic layer deposition (ALD) coating with alumina, which significantly enhances the capacity retention and Coulombic efficiency over many cycles. Overall, we find that the layered/layered Na-O3/Li-O’3 intergrowth structure is able to provide structural stability and suppress undesired phase transformations but is overwhelmed by the increased reactivity of the surface if not protected by surface coating.
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Post-irradiation examination of coated particle fuel from the AGR-1 experiment is in progress at Idaho National Laboratory and Oak Ridge National Laboratory. In this paper a brief summary of results from characterization of microstructures in the coating layers of selected irradiated fuel particles with burnup of 11.3% and 19.3% FIMA will be given. The main objectives of the characterization were to study irradiation effects, fuel kernel porosity, layer debonding, layer degradation or corrosion, fission-product precipitation, grain sizes, and transport of fission products from the kernels across the TRISO layers. Characterization techniques such as scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, and wavelength dispersive spectroscopy were used. A new approach to microscopic quantification of fission-product precipitates is also briefly demonstrated. Microstructural characterization focused on fission-product precipitates in the SiC-IPyC interface, the SiC layer and the fuel-buffer interlayer. The results provide significant new insights into mechanisms of fission-product transport. Although Pd-rich precipitates were identified at the SiC-IPyC interlayer, no significant SiC-layer thinning was observed for the particles investigated. Characterization of these precipitates highlighted the difficulty of measuring low concentrations of Ag in precipitates with significantly higher concentrations of Pd and U. Different approaches to resolving this problem are discussed. An initial hypothesis is provided to explain fission-product precipitate compositions and locations. No SiC phase transformations were observed and no debonding of the SiC-IPyC interlayer as a result of irradiation was observed for the samples investigated. Lessons learned from the post-irradiation examination are described and future actions are recommended.
The stiffness of wellbore cement fracture surfaces was measured after exposing to the advective flow of nitrogen, silicone oil, and medium sweet dead crude oil for different exposure periods. The test specimens were extracted from fractured cement cylinders, where the cement fracture surfaces were exposed to the different fluids up to 15 weeks. A nanoindenter with a Berkovich indenter tip was used to measure load-indentation depth data, which was used to extract the elastic modulus (E) and nano-hardness (H) of the cement fracture surfaces. A reduction in the elastic modulus compared with an unexposed specimen were observed in all the specimens. Both elastic modulus and nano-hardness for the specimens exposed to silicone oil were lower than specimens exposed to nitrogen gas and varied with the period of exposure. The elastic modulus and nano-hardness of the specimens exposed to crude oil were the lowest with a significant decrement with the exposure period. The frequency distribution of the nanoindentation measurements shows that the volume-fraction ratio of the two types of cement hydrated nanocomposites for both the unexposed and test specimens is about 70:30%. Phase transformation beneath the indenter is observed for all of the specimens, with more obvious plastic deformation in specimens exposed to crude oil. Analytical measurements (SEM, EDS, FT-IR, and XRD) on exposed cement fracture surfaces reveal different levels of physical and chemical alteration that are consistent with the reduction in stiffness measured by nanoindentation. Furthermore, the study suggests that cement stiffness will decrease due to crude oil exposure, and the fracture will be sensitive to stress and pore pressure with time.
Laser-induced breakdown spectroscopy (LIBS) and Raman spectroscopy are complementary techniques providing respectively chemical and structural information on the sample target. These techniques are increasingly used in Earth and Planetary sciences, and often together. LIBS is locally destructive for the target, and the laser-induced effects due to LIBS laser shots on the structure and on the Raman fingerprint of a set of geological samples relevant to Mars exploration are here investigated by Raman spectroscopy and electron microscopy. Experiments show that the structure of samples with low optical absorption coefficients is preserved as well as the structural information carried by Raman spectra. By contrast, minerals with high optical absorption coefficient can be severely affected by LIBS laser shots with local amorphization, melting and/or phase transformation. Thermal modeling shows that the temperature can reach several thousands of degrees at the surface for such samples during a LIBS laser shot, but decreases rapidly with time and in space. In 2020, NASA Mars 2020 mission will send a rover equipped with a combined LIBS/Raman instrument for remote analysis (SuperCam) as well as proximity science instruments at fine scale for X-ray fluorescence called PIXL for Planetary Instrument for X-ray Lithochemistry, and deep UV Raman spectroscopy called SHERLOC for Scanning Habitable Environments with Raman & Luminescence for Organics & Chemicals. Here, we discuss the implications of our results for the operation of these instruments and show that (i) the SuperCam analytical footprint for Raman spectroscopy is many times larger than the LIBS crater, minimizing any effects and (ii) SHERLOC and PIXL analysis may be affected if they analyze within a LIBS crater created by SuperCam LIBS.
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