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At least 577 records · Page 32

Coordinated Analysis of an Experimentally Space Weathered Carbonaceous Chondrite

The surfaces of airless bodies experience solar wind irradiation and micrometeorite impacts, a process collectively known as space weathering. These mechanisms alter the chemical composition, microstructure, and optical properties of surface materials and considerable work has been done to understand this phenomenon in lunar and ordinary chondritic materials. However, ongoing sample return missions Hayabusa2 to asteroid Ryugu and OSIRIS-REx to asteroid Bennu have prompted the need to study the effects of space weathering on hydrated, organic-rich materials, especially in the context of early results. Understanding space weathering of these samples is critical for properly interpreting remote sensing data during asteroid encounters, for sample site selection, and for the eventual study of returned samples. We can better understand space weathering of carbonaceous materials by simulating these processes in the laboratory. Recent experiments have shown that the changes in spectral characteristics of carbonaceous chondrites are not consistent among experiments, suggesting additional work is needed before these results can inform our understanding of spectral variations on asteroidal surfaces. Similarly, substantial work remains to characterize the chemical and microstructural effects of these processes in order to correlate these features with spectral changes. Here, we build on our previous work, presenting new results of the pulsed laser irradiation of the Murchison (CM2) meteorite to simulate micrometeorite impacts and the progressive space weathering of carbonaceous surfaces.

Thompson, M. S.↗

Analysis of radially resolved thermal conductivity in high burnup mixed oxide fuel and comparison to thermal conductivity correlations implemented in fuel performance codes

The thermal diffusivity and thermal conductivity of high burnup (19 % FIMA) mixed oxide (U, Pu)O 2 nuclear fuel has been measured along the radial direction using a thermoreflectance-based method. Measured thermal conductivity exhibits a notable radial variation consistent with the expectations that a large temperature gradient across the annular fuel pellet leads to a heterogeneous microstructure. A common fuel performance model of thermal conductivity, the Lucuta-Inoue model, is used to analyze the measured thermal conductivity profile. Further, this model adequately captures the radial dependence of thermal conductivity except in the periphery. The analysis suggests that the characteristic radial shape of the thermal conductivity profile follows the burnup profile within the fuel pin. In the periphery, the high burnup structure is formed and the conductivity model, not capturing this effect, likely overestimates the thermal conductivity.

36 MATERIALS SCIENCE↗

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗

A microstructural lattice model for strain oriented problems: A combined Monte Carlo finite element technique

A specialized, microstructural lattice model, termed MCFET for combined Monte Carlo Finite Element Technique, was developed which simulates microstructural evolution in material systems where modulated phases occur and the directionality of the modulation is influenced by internal and external stresses. In this approach, the microstructure is discretized onto a fine lattice. Each element in the lattice is labelled in accordance with its microstructural identity. Diffusion of material at elevated temperatures is simulated by allowing exchanges of neighboring elements if the exchange lowers the total energy of the system. A Monte Carlo approach is used to select the exchange site while the change in energy associated with stress fields is computed using a finite element technique. The MCFET analysis was validated by comparing this approach with a closed form, analytical method for stress assisted, shape changes of a single particle in an infinite matrix. Sample MCFET analytical for multiparticle problems were also run and in general the resulting microstructural changes associated with the application of an external stress are similar to that observed in Ni-Al-Cr alloys at elevated temperature.

Gayda, J.↗

Microstructural Coarsening Kinetics and Mechanical Property Changes in Long-Term Aged Sn–Pb–Sb Solder Joints

Tin-lead-antimony (50Sn–47Pb–3Sb wt.%) soldered assemblies were mechanically tested approximately 30 years after initial production and found to have solder joints of reduced strength. The microstructure of this solder alloy exhibits a ternary eutectic structure with Sn-rich, Pb-rich, and SnSb phases. Accelerated aging was performed to evaluate solder microstructural coarsening and associated strength of laboratory solder joints to correlate these properties to the “naturally aged” solder joints. Isothermal aging was conducted at room temperature, 55, 70, 100, and 135 °C and aging times that ranged from 0.1 to 365 days. The coarsening kinetics of the Pb-rich phase were determined through optical microscopy and image analysis methods established in previous studies on binary Sn–Pb solder. A kinetic equation was developed with time exponent n of 0.43 and activation energy of 24000 J/mol, suggesting grain boundary diffusion or other fast diffusion pathways controlling the microstructural evolution. Compression testing and Vickers microhardness showed significant strength loss within the first 20–30 days after soldering; then, the microstructure and mechanical properties changed more slowly over long periods of time. Further, by combining accelerated aging data and the microstructure-based kinetics, strength predictions were made that match well with the properties of the actual soldered assemblies naturally aged for 30 years. However, aging at the highest temperature of 135 °C produced anomalous behavior suggesting that extraneous aging mechanisms are active. Therefore, data obtained at this temperature or higher should not be used. Overall, the combined microstructural and mechanical property methods used in this study confirmed that the observed reduction in strength of ~ 30-year-old solder joints can be accounted for by the microstructural coarsening that takes place during long-term solid-state aging.

36 MATERIALS SCIENCE↗

Linking microstructure to creep behavior in vertically and horizontally built LPBF Haynes 282 compared with wrought material via θ -projection

Laser Powder Bed Fusion (LPBF) has emerged as a promising route for fabricating intricate geometries in high-performance alloys. Haynes 282 (H282) is a strong candidate for applications such as heat exchangers or engines due to its excellent creep strength and thermal stability; however, the long-term creep behavior of LPBF-processed H282 remains poorly understood. In this study, the θ -projection method is used to analyze and extrapolate the creep behavior of vertically built LPBF, horizontally built LPBF, compared to wrought H282 tested at 816 °C. Vertically built LPBF H282 exhibits the lowest minimum creep rate (MCR), while the horizontally built condition shows a higher MCR comparable to that of wrought H282. Despite these differences, both LPBF conditions exhibit significantly shorter rupture life and reduced rupture strain than the wrought material, with the most severe degradation observed in the horizontal builds, consistent with an earlier onset of tertiary creep and accelerated strain-rate evolution. Microstructural characterization reveals that both LPBF and wrought H282 exhibit abundant twin-related boundary character; however, their grain boundary topologies differ markedly. The wrought alloy contains a higher fraction of low-angle grain boundaries and continuous twin lamellae, whereas the LPBF microstructure is characterized by a suppressed low-angle boundary population and fragmented twin-related boundaries embedded within irregular high-angle grain boundary networks. Fractographic analysis further reveals predominantly intergranular cracking in LPBF H282, accompanied by grain-boundary-decorated carbides, Al 2 O 3 inclusions, and high-aspect-ratio pores. These results demonstrate that grain boundary topology, rather than minimum creep rate alone, plays a critical role in governing creep damage accumulation and rupture behavior in LPBF and wrought H282.

Creep↗

Microstructure and mechanical properties of bulk yttria-partially-stabilized zirconia

A commercially available bulk 4.5 mole percent yttria-Y2O3)-partially-stabilized zirconia (PSZ) was studied by light microscopy, X-ray analysis, microhardness measurement, and fracture toughness testing. The growth of the precipitates and the phase transformations were studied as a function of aging in air at 1500 C. Aging cuves were constructed for both the as-received and the solution-annealed-and-quenched materials; the curves showed hardness peaks at 1397 and 1517 kg/sq mm, respectively. A total of twelve different types of tetragonal precipitates were found. The rectangular plate-shaped tetragonal precipitates were found to have a (110) habit plane. Grinding of the Y2O3 PSZ into powder did not cause a significant amount of metastable tetragonal precipitates to transform into the monoclinic phase, thus indicating that transformation toughening is not a significant mechanism for the material. The fracture toughness of the aged and of the unaged solution-annealed-and-quenched PSZ was found to be between 2 and 3 MN/cu m/2.

Valentine, P. G.↗

Analysis of New Composite Architectures

Efficient and accurate specialty finite elements methods to analyze textile composites were developed and are described. Textile composites present unique challenges to the analyst because of the large, complex 'microstructure'. The geometry of the microstructure is difficult to model and it introduces unusual free surface effects. The size of the microstructure complicates the use of traditional homogenization methods. The methods developed constitute considerable progress in addressing the modeling difficulties. The details of the methods and attended results obtained therefrom, are described in the various chapters included in Part 1 of the report. Specific conclusions and computer codes generated are included in Part 2 of the report.

Whitcomb, John D.↗

HOTCFGM-1D: A Coupled Higher-Order Theory for Cylindrical Structural Components with Through-Thickness Functionally Graded Microstructures

The objective of this three-year project was to develop and deliver to NASA Lewis one-dimensional and two-dimensional higher-order theories, and related computer codes, for the analysis, optimization and design of cylindrical functionally graded materials/structural components for use in advanced aircraft engines (e.g., combustor linings, rotor disks, heat shields, blisk blades). To satisfy this objective, a quasi one-dimensional version of the higher-order theory, HOTCFGM-1D, and four computer codes based on this theory, for the analysis, design and optimization of cylindrical structural components functionally graded in the radial direction were developed. The theory is applicable to thin multi-phased composite shell/cylinders subjected to macroscopically axisymmetric thermomechanical and inertial loading applied uniformly along the axial direction such that the overall deformation is characterized by a constant average axial strain. The reinforcement phases are uniformly distributed in the axial and circumferential directions, and arbitrarily distributed in the radial direction, thereby allowing functional grading of the internal reinforcement in this direction.

Pindera, Marek-Jerzy↗

Microstructural stability and mechanical properties of the as-cast and heat-treated newly developed TiNbCrTa refractory complex concentrated alloy

In this study, a TiNbCrTa refractory complex concentrated alloy (RCCA) was prepared using vacuum arc remelting. The microstructural evolution and mechanical properties of both as-cast and heat-treated RCCA samples were analyzed. Heat treatment (HT) was performed at 800–1200 °C for 1 h in a vacuum-sealed environment. These samples exhibited a formation of Cr 2 Nb and Cr 2 Ti Laves phases. A variation in elemental distribution was observed, with interdendritic (ID) regions showing higher fractions of Ti and Cr, while the dendritic regions had a greater concentration of Ta and Nb. Micro-segregation at the IDs was confirmed through energy dispersive x-ray spectroscopy mapping, which inferred the formation of Cr- and Ti-rich phases during HT at 800–1200 °C. High-temperature HT at 1200 °C for 1 h led to the evolution of the hcp omega phase. Prolonged HT at 1200 °C for 96 h resulted in the evolution of a Cr-rich Laves phase (Cr 2 Ta), which was homogeneously distributed within the microstructure, indicating an unstable microstructure. Furthermore, despite prolonged HT, a variation in the elemental distribution persisted due to the presence of dendritic and ID regions. Electron backscattered diffraction analysis revealed the presence of bcc and hcp phases in the dendritic and ID regions, respectively, of the as-cast and HTed samples. The as-cast samples demonstrated a high compressive strength of approximately 2 GPa. Micro-hardness values increased with the HT temperature up to 1000 °C. Further increases under HT conditions did not significantly reduce the microhardness value, whereas prolonged HT at 1200 °C led to an increase in the microhardness value. Overall, the newly developed TiNbCrTa RCCA exhibited high-strength behavior even after the phase transformation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

New oxidation features in NiCrAl-Zr revealed by an Auger microprobe

A NiCrAl-0.5 (wt %) Zr alloy, oxidized in air for 1 h at 1180 C was studied using a 30-nm resolution Auger microprobe. Depth analysis was achieved using crater edge profiling. This first application of AES to these alloys enabled several new observations of the chemical composition of microstructural features in the corrosion layer. The external oxide was rough, about 2-3 microns thick, and contained Ni, Cr, Al, and O. It was discovered that stoichiometric Al2O3 was restricted to a homogeneous layer about 300-nm thick between the oxide and the base metal. The metal immediately beneath this Al2O3 layer was found to be depleted in Al and roughly ten times richer in Zr than the bulk alloy. These observations are compared with the predictions of current models of the oxidation of MCrAl alloys.

Larson, L. A.↗

A study of aluminum-lithium alloy solidification using acoustic emission techniques

Physical phenomena associated with the solidification of an aluminum lithium alloy was characterized using acoustic emission (AE) techniques. It is shown that repeatable patterns of AE activity may be correlated to microstructural changes that occur during solidification. The influence of the experimental system on generated signals was examined in the time and frequency domains. The analysis was used to show how an AE signal from solidifying aluminum is changed by each component in the detection system to produce a complex waveform. Conventional AE analysis has shown that a period of high AE activity occurs in pure aluminum, an Al-Cu alloy, and the Al-Li alloy, as the last fraction of solid forms. A model attributes this to the internal stresses of grain boundary formation. An additional period of activity occurs as the last fraction of solid forms, but only in the two alloys. A model attributes this to the formation of interdendritic porosity which was not present in the pure aluminum. The AE waveforms were dominated by resonant effects of the waveguide and the transducer.

Henkel, Daniel P.↗

RESIDUAL DEFORMATION ANALYSIS IN COMPOSITE SHELL STRUCTURES MANUFACTURED USING AUTOMATED FIBER PLACEMENT

The manufacturing of composites typically produces residual stresses that can significantly affect the final shape of the structure. The process of automated fiber placement (AFP) has become a prominent manufacturing technique in developing layups with tailored, variable stiffness morphology. The steered patterns of fiber tows with and without overlaps produce residual deformations that are distinctive from traditional layups. Digital image correlation was used to measure the AFP lamina coefficients of thermal expansion, which were incorporated into finite element analyses (FEA) to model the cooling phase of the cure cycle. The effects of nonlinear analysis and temperature-dependent lamina properties calculated using self-consistent field micromechanics, on the resulting residual deformation of shells, were also modeled. The predicted residual deformation was analyzed by considering out-of-roundness in cylindrical shells and compared to the experimental results. The shell FEA results were well-correlated with the overall deformed shape of the AFP cylinder with overlaps, while the shell FEA model of the AFP cylinder without overlaps did not show as good of qualitative match of the deformation pattern. Analytical correlation with measured results were insensitive to material softening at elevated temperatures, geometric nonlinearities, and variations in measured lamina thermal properties. To improve the accuracy of the residual deformation analysis, these results suggest that the thermo-chemical shrinkages preceding the cooldown should be considered, as well as possible variations in ply level microstructure due to the presence of the embedded fiber tow gaps and overlaps.

Composites↗

Microstructure and mechanical properties of bulk and plasma-sprayed y2O3-partially stabilized zirconia

Bulk 8.0 weight percent yttria partially stabilied zirconia (PSZ) was studied by light microscopy, transmission electron microscopy, X-ray analysis, microhardness testing, and fracture toughness testing. The as received PSZ contained spheroidal and grain boundary precipitates up to 4 micrometers in size. Spheroids up to 1.26 micrometers were metastable tetragonal; large spheroids were monoclinic. Grinding the PSZ into powder did not cause a significant amount of tetragonal to transform to monoclinic. This indicates that transformation toughness is not a significant mechanism in PSZ. Aging the PSZ at 1500 C caused the fine tetragonal precipitates to grow from 0.06 to 0.12 micrometers, in 250 minutes. A peak hardness of 1400 kg/sq mm was attained after 50 minutes. Solution annealing and quenching the as received PSZ eliminated the large precipitates, but fine tetragonal precipitates reformed on quenching. Aging at 1500 C caused the fine 0.02 micrometers tetragonal precipitates to grow into plates about 0.10 by 0.50 micrometers. A peak hardness of 1517 kg/sq mm was obtained after 250 minutes. On further aging, monoclinic percipitates formed along grain boundaries. The fracture toughness of the aged and unaged solution annealed and quenched PSZ was found to be between 2 and 3 MN /square root of m cubed. This range of fracture toughness is consistent with PSZ's that do not undergo transformation toughening.

Valentine, P. G.↗

Optimization of residual stresses in MMC's through the variation of interfacial layer architectures and processing parameters

The objective of this work was the development of efficient, user-friendly computer codes for optimizing fabrication-induced residual stresses in metal matrix composites through the use of homogeneous and heterogeneous interfacial layer architectures and processing parameter variation. To satisfy this objective, three major computer codes have been developed and delivered to the NASA-Lewis Research Center, namely MCCM, OPTCOMP, and OPTCOMP2. MCCM is a general research-oriented code for investigating the effects of microstructural details, such as layered morphology of SCS-6 SiC fibers and multiple homogeneous interfacial layers, on the inelastic response of unidirectional metal matrix composites under axisymmetric thermomechanical loading. OPTCOMP and OPTCOMP2 combine the major analysis module resident in MCCM with a commercially-available optimization algorithm and are driven by user-friendly interfaces which facilitate input data construction and program execution. OPTCOMP enables the user to identify those dimensions, geometric arrangements and thermoelastoplastic properties of homogeneous interfacial layers that minimize thermal residual stresses for the specified set of constraints. OPTCOMP2 provides additional flexibility in the residual stress optimization through variation of the processing parameters (time, temperature, external pressure and axial load) as well as the microstructure of the interfacial region which is treated as a heterogeneous two-phase composite. Overviews of the capabilities of these codes are provided together with a summary of results that addresses the effects of various microstructural details of the fiber, interfacial layers and matrix region on the optimization of fabrication-induced residual stresses in metal matrix composites.

Pindera, Marek-Jerzy↗

Influence of rolling reduction and annealing on recrystallization and grain structure in Ta-2.5W alloys

The microstructural evolution of wrought Tantalum - 2.5 wt% Tungsten (Ta-2.5W) alloys during thermomechanical processing is critical for optimizing their mechanical reliability in demanding applications such as aerospace, chemical processing, and nuclear technology. Despite the widespread use of Ta-W alloys, a comprehensive understanding of how rolling reduction, annealing temperature, and elemental inhomogeneity interact to determine recrystallization behavior and grain refinement remains incomplete. Here, in this study, we systematically investigate the effects of cold rolling and subsequent annealing on the microstructure of Ta-2.5W, with particular attention to grain orientation, stored energy, and elemental banding. Our results demonstrate that higher rolling reduction rates lower the onset and completion temperatures for recrystallization, resulting in finer and more homogeneous grain structures. Electron backscatter diffraction (EBSD) analysis reveals that grains with a 〈111〉 parallel to the plate normal possess higher stored energy and nucleate recrystallization more readily than grains with a 〈001〉 parallel to the plate normal. Elemental mapping shows that tungsten inhomogeneity leads to localized bands of accelerated recrystallization and hardness variation. These findings provide new insights into the mechanisms of microstructure refinement in Ta-2.5W alloys, offering guidance for tailoring processing routes to achieve superior performance in demanding engineering environments.

Annealing↗

Fiber-matrix interphase characterization in composites using ultrasonic velocity data

A nondestructive method is introduced to determine the effective elastic of fiber-matrix interphases from measured composite moduli. The composite moduli are obtained by measuring the angular dependences of ultrasonic longitudinal and transverse phase velocities in planes along and perpendicular to the fibers. Three independent interphase effective moduli are found using micromechanical multiphase models which were applied after averaging composite transverse moduli to account for the composite orthotropy. Sensitivity analysis shows that errors in the calculated interphasial moduli are approximately ten times those in the composite moduli. Experiments are performed on Si3N4 ceramic and Ti-24Al-11Nb intermetallic matrix composites reinforced with carbon coated silicon carbide fibers. The experimental interphasial moduli for the intermetallic composites agree with literature data after accounting for the interphase microstructure. The interphasial moduli for ceramic composites are lower than those for the intermetallic composite due to imperfect mechanical contact between the interphase and the porous matrix. The use of the method to assess the interphase degradation is demonstrated for interphasial oxidation damage. The analysis helps to determine the morphology of the damaged interphase.

Chu, Y. C.↗