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At least 595 records · Page 33

Evidence of Microfossils in Carbonaceous Chondrites

Investigations have been carried out on freshly broken, internal surfaces of the Murchison, Efremovka and Orgueil carbonaceous chondrites using Scanning Electron Microscopes (SEM) in Russia and the Environmental Scanning Electron Microscope (ESEM) in the United States. These independent studies on different samples of the meteorites have resulted in the detection of numerous spherical and ellipsoidal bodies (some with spikes) similar to the forms of uncertain biogenicity that were designated "organized elements" by prior researchers. We have also encountered numerous complex biomorphic microstructures in these carbonaceous chondrites. Many of these complex bodies exhibit diverse characteristics reminiscent of microfossils of cyanobacteria such as we have investigated in ancient phosphorites and high carbon rocks (e.g. oil shales). Energy Dispersive Spectroscopy (EDS) analysis and 2D elemental maps shows enhanced carbon content in the bodies superimposed upon the elemental distributions characteristic of the chondritic matrix. The size, distribution, composition, and indications of cell walls, reproductive and life cycle developmental stages of these bodies are strongly suggestive of biology' These bodies appear to be mineralized and embedded within the meteorite matrix, and can not be attributed to recent surface contamination effects. Consequently, we have interpreted these in-situ microstructures to represent the lithified remains of prokaryotes and filamentous cyanobacteria. We also detected in Orgueil microstructures morphologically similar to fibrous kerite crystals. We present images of many biomorphic microstructures and possible microfossils found in the Murchison, Efremovka, and Orgueil chondrites and compare these forms with known microfossils from the Cambrian phosphate-rich rocks (phosphorites) of Khubsugul, Northern Mongolia.

Hoover, Richard B.↗

Robust Informatics Infrastructure Required For ICME: Combining Virtual and Experimental Data

With the increased emphasis on reducing the cost and time to market of new materials, the need for robust automated materials information management system(s) enabling sophisticated data mining tools is increasing, as evidenced by the emphasis on Integrated Computational Materials Engineering (ICME) and the recent establishment of the Materials Genome Initiative (MGI). This need is also fueled by the demands for higher efficiency in material testing; consistency, quality and traceability of data; product design; engineering analysis; as well as control of access to proprietary or sensitive information. Further, the use of increasingly sophisticated nonlinear, anisotropic and or multi-scale models requires both the processing of large volumes of test data and complex materials data necessary to establish processing-microstructure-property-performance relationships. Fortunately, material information management systems have kept pace with the growing user demands and evolved to enable: (i) the capture of both point wise data and full spectra of raw data curves, (ii) data management functions such as access, version, and quality controls;(iii) a wide range of data import, export and analysis capabilities; (iv) data pedigree traceability mechanisms; (v) data searching, reporting and viewing tools; and (vi) access to the information via a wide range of interfaces. This paper discusses key principles for the development of a robust materials information management system to enable the connections at various length scales to be made between experimental data and corresponding multiscale modeling toolsets to enable ICME. In particular, NASA Glenn's efforts towards establishing such a database for capturing constitutive modeling behavior for both monolithic and composites materials

Mutli-scale models↗

Computer vision models and advanced TEM imaging for microstructures of irradiated AM316 stainless steels

Advancements were made in automating microscopy-based material characterization, particularly in studying irradiation effects on additively manufactured (AM) materials using machine learning (ML) and computer vision (CV). These automation efforts address the challenges of analyzing complex microstructures, accelerating the detection of irradiation-induced defects. Two CV models were developed at Argonne National Laboratory (ANL) to enhance transmission electron microscopy (TEM) analysis of irradiated AM 316 stainless steel. The first model focused on the detection of irradiation-induced dislocation loops, which contribute to material hardening and embrittlement. These loops, categorized as faulted or perfect, were automatically detected and classified using a Mask R-CNN model trained on TEM images from both in-situ and ex-situ ion irradiation experiments. The model achieved high accuracy, with precision, recall, and F1 scores of 0.839, 0.734, and 0.776, respectively, demonstrating its effectiveness in analyzing dislocation loops in irradiated AM materials. The second CV model was developed to analyze the size and wall thickness of dislocation cells in laser powder bed fusion (LPBF) 316 stainless steel. Using a U-Net++ architecture with EfficientNet as the encoder, the model was trained on TEM images to segment and measure cell size and wall thickness.

36 MATERIALS SCIENCE↗

Micro-Raman Analysis of Irradiated Diamond Films

Owing to its unique and robust physical properties, diamond is a much sought after material for use in advanced technologies, even in Microelectromechanical Systems (MEMS). The volume and weight savings promised by MEMS-based devices are of particular interest to spaceflight applications. However, much basic materials science research remains to be completed in this field. Results of micro-Raman analysis of proton (10(exp 15) - 10(exp 17) H(+)/sq cm doses) irradiated chemical vapor deposited (CVD) films are presented and indicate that their microstructure is retained even after high radiation exposure.

Newton, Robert L.↗

Materials Examination of the Vertical Stabilizer from American Airlines Flight 587

The first in-flight failure of a primary structural component made from composite material on a commercial airplane led to the crash of American Airlines Flight 587. As part of the National Transportation Safety Board investigation of the accident, the composite materials of the vertical stabilizer were tested, microstructure was analyzed, and fractured composite lugs that attached the vertical stabilizer to the aircraft tail were examined. In this paper the materials testing and analysis is presented, composite fractures are described, and the resulting clues to the failure events are discussed.

Fox, Matthew R.↗

Dynamic Scaling Analysis of Accelerated Irradiation Testing on Additive Manufacturing Materials by Positron Annihilation

The timely applications of Additive Manufacturing (AM) materials in nuclear environments require accelerated irradiation tests, mainly ion irradiation to enable rapid prototyping. Low dose ion irradiation would cause sub-nanostructure changes by generation of lattice defects, vacancies, vacancy clusters and voids and void swelling caused by cellular dislocations. Positron Annihilation Lifetime (PAL), a novel technology, sensitive towards sub-nanostructure morphology with high accuracy (about 10-7 vacancy per atom), supported by Transition Electron Microscope (TEM) would be applied to identify the type and total size of the defects. The subsequent PAL measurements and TEM surface studies would be followed by PAL analysis that includes sophisticated trapping model. The PAS results would become an input to dynamic scaling analysis (that predicts radiation effects from low dose studies for high dose effects), which incorporate mean-field theory model. The final effect is an in-depth understanding of the microstructure evolution of AM materials under ion irradiation which can be extrapolated to the studies of neutron irradiation, since ion-irradiation takes less time and do not cause the irradiation hazard. The working hypothesis is that PAL technology, that have excellent sensitivity to low-defect concentration would help to identify ion-induced material damage on the atomic and nano-scale level, which then could be extrapolated to understand the neutron damage better.

accelerated irradiation testing↗

Tuning Microstructure of Mesophase Pitch Carbon Fiber by Altering the Carbonization Ramp Rate

The microstructure of mesophase pitch carbon fibers (CFs) are tuned by varying ramp rates from 1 to 50 °C min –1 up to 1000 °C to study the effect of ramp rate on CFs’ microstructure, thermal and mechanical properties with the goal of offsetting the cost by decreasing cycle time. The ramp rates represent carbonization times ranging from 16.4 to 1.17 h, not including cool down. Differential scanning calorimetry, thermogravimetric analysis, and derivative thermogravimetry are used to investigate the impact ramp rate has on the thermal properties of mesophase pitch. It is found that lower ramp rates are endothermic in nature with a lower temperature onset and maximum weight loss. Higher ramp rates possess an exothermic nature with higher temperatures resulting in maximal weight loss over a smaller range of temperatures. Mechanical testing shows varying CF strengths and moduli dependent on ramp rate and an optimized process is developed to produce the strongest CF. Furthermore, microstructural characterization revealed that faster ramp rates lead to smaller interplanar spacings and larger crystallites but possessed greater disorder.

36 MATERIALS SCIENCE↗

The Hollow Spheres of the Orgueil Meteorite: A Re-Examination

In 1971, Rossignol-Strick and Barghoorn provided images and a description of a number of spherical hollow microstructures showing well-defined walls in acid macerated extract of the Orgueil CI carbonaceous meteorite. Other forms such as membranes and spiral shaped structures were also reported. The carbon-rich (kerogen) hollow spheres were found to be in a narrowly constrained distribution of sizes (mainly 7 to 10 microns in diameter). Electron microprobe analysis revealed that these spheres contained Carbon, possibly P, N, and K. It was established that these forms could not be attributed to pollen or other recent terrestrial contaminants. It was concluded that they most probably represented organic coatings on globules of glass, olivine or magnetite in the meteorite. However, recent studies of the Orgueil meteorite have been carried out at the NASA/Marshall Space Flight Center with the S-4000 Hitachi Field Emission Scanning Electron Microscope (FESEM). These investigations have revealed the presence of numerous carbon encrusted spherical magnetite platelets and spherical and ovoidal bodies of elemental iron in-situ in freshly fractured interior surfaces of the meteorite. Their size range is also very narrowly constrained (typically approximately 6 to 12 microns) in diameter. High resolution images reveal that these bodies are also encrusted with a thin carbonaceous sheath and are surrounded by short nanofibrils that are shown to be composed of high purity iron by EDAX elemental analysis. We present Secondary and Backscatter Electron FESEM images and associated EDAX elemental analyses and 2D X-ray maps of these forms as we re-examine the hollow spheres of Orgueil and attempt to determine if they are representatives of the same population of indigenous microstructures.

Hoover, Richard B.↗

Corrosion Response of Ni-19Cr-5Fe in Molten NaCl-MgCl 2 Salt

Ni-based alloys are strong candidates for use in high-temperature molten salt reactors due to their superior corrosion resistance and mechanical stability compared to stainless steels. In this study, the static corrosion behavior of a Ni-19Cr-5Fe model alloy was systematically evaluated in a purified molten NaCl-MgCl 2 salt at 700°C for 30, 240, and 500 h. Post-exposure analyses were conducted to assess microstructural evolution, corrosion depth, and elemental depletion profiles. Corrosion rates, quantified by chromium depletion depth, followed an inverse power-law trend with increasing exposure time, indicating diffusion-limited kinetics. This trend is attributed to limitations in mass transport in the static salt and to the progressive local depletion of reactive chromium species. Coupled electron backscatter diffraction and energy dispersive X-ray spectroscopy analysis further revealed that the grain boundary character significantly influences corrosion susceptibility: high-angle grain boundaries exhibited pronounced Cr depletion and pitting, while low-angle and Σ3 boundaries remained comparatively resistant. These results offer valuable insight into the role of microstructure in corrosion processes and reinforce the importance of time-dependent material evaluation in molten salt environments relevant to advanced reactor designs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Spin Testing of Superalloy Disks With Dual Grain Structure

This 24-month program was a joint effort between Allison Advanced Development Company (AADC), General Electric Aircraft (GEAE), and NASA Glenn Research Center (GRC). AADC led the disk and spin hardware design and analysis utilizing existing Rolls-Royce turbine disk forging tooling. Testing focused on spin testing four disks: two supplied by GEAE and two by AADC. The two AADC disks were made of Alloy 10, and each was subjected to a different heat treat process: one producing dual microstructure with coarse grain size at the rim and fine grain size at the bore and the other produced single fine grain structure throughout. The purpose of the spin tests was to provide data for evaluation of the impact of dual grain structure on disk overspeed integrity (yielding) and rotor burst criteria. The program culminated with analysis and correlation of the data to current rotor overspeed criteria and advanced criteria required for dual structure disks.

Hefferman, Tab M.↗

Investigation of residual stress distribution in wire-arc directed energy deposited refractory molybdenum alloy utilizing numerical thermo-mechanical analysis and neutron diffraction method

Directed energy deposition (DED), a metal additive manufacturing (AM) technique, offers higher deposition rates and energy efficiency, making it suitable for fabricating components from refractory molybdenum alloys, such as molybdenum-titanium-zirconium (TZM). However, large thermal gradients and non-equilibrium thermal cycles in DED could generate high residual stress in the component, potentially deteriorating quality and performance. Thus, this study aims to investigate residual stress generation and its distribution in wire-arc DED of TZM thin-wall, utilizing thermo-mechanical analysis and high-fidelity neutron diffraction (ND) method. Two interpass temperatures (50°C and 200°C) have been considered to investigate their impact on residual stress formation. During experiments, in-situ thermal data has been recorded using thermocouples, which have been utilized for calibrating the thermal model. Thermocouple data shows a good agreement with the simulation results, having a difference of less than 10 %. Post-deposition part deformation has been observed, which is measured using a coordinate measuring machine, showing maximum values of 0.93 mm and 0.78 mm for interpass temperatures of 50°C and 200°C, respectively. Numerical predictions of distortion deviated by less than 15% from the experimental results. ND measurement and simulation results indicate that residual stress magnitude and evolution vary across the TZM deposits, revealing microstructural anisotropy in both conditions. Notably, lower interpass temperatures resulted in higher residual stresses, confirmed by experimental and simulation data. Further, this study demonstrated that an integrated experimental and thermo-mechanical analysis can potentially reveal the temperature history, part deformation, and residual stress formation in wire-arc DED TZM alloy.

36 MATERIALS SCIENCE↗

Single particle impact explorations on the role of powder heat treatments in cold spray: Effects of strength and oxide structure

In cold spray, the optimization of the powder feedstock for improving the final properties of the coating and for improving the process itself are two different objectives. This paper explores the latter, studying the relationship between powder pre-heat treatment and the kinetic bonding between the individual particles and the substrate. Using a laser-induced particle impact test (LIPIT), we investigate the effect of different heat treatments on the critical adhesion velocity of Al 6061. Although heat treatments change the strength of the powders as well as the thickness of the native oxide layer each by as much as ∼50 %, the critical adhesion velocity remains constant to within only ∼10 %. A deeper analysis reveals that these two factors change in somewhat complementary ways for the heat treatments explored here, leading to counteracting effects. By quantitatively evaluating these two microstructural factors in tandem, we find that they are roughly equally important in determining the critical adhesion velocity. These observations thus provide insight for the development of new heat treatment regimens that might lower the adhesion velocity.

Al 6061↗

Elevated temperature crack growth in aluminum alloys: Tensile deformation of 2618 and FVS0812 aluminum alloys

Understanding the damage tolerance of aluminum alloys at elevated temperatures is essential for safe applications of advanced materials. The objective of this project is to investigate the time dependent subcritical cracking behavior of powder metallurgy FVS0812 and ingot metallurgy 2618 aluminum alloys at elevated temperatures. The fracture mechanics approach was applied. Sidegrooved compact tension specimens were tested at 175, 250, and 316 C under constant load. Subcritical crack growth occurred in each alloy at applied stress intensity levels (K) of between about 14 and 25 MPa/m, well below K (sub IC). Measured load, crack opening displacement and displacement rate, and crack length and growth rate (da/dt) were analyzed with several continuum fracture parameters including, the C-integral, C (sub t), and K. Elevated temperature growth rate data suggest that K is a controlling parameter during time dependent cracking. For FVS0812, da/dt is highest at 175 C when rates are expressed as a function of K. While crack growth rate is not controlled by C (sub t) at 175 C, da/dt appears to better correlate with C (sub t) at higher temperatures. Creep brittle cracking at intermediate temperatures, and perhaps related to strain aging, is augmented by time dependent transient creep plasticity at higher temperatures. The C (sub t) analysis is, however, complicated by the necessity to measure small differences in the elastic crack growth and creep contributions to the crack opening displacement rate. A microstructural study indicates that 2618 and FVS0812 are likely to be creep brittle materials, consistent with the results obtained from the fracture mechanics study. Time dependent crack growth of 2618 at 175 C is characterized by mixed transgranular and intergranular fracture. Delamination along the ribbon powder particle boundaries occurs in FVS0812 at all temperatures. The fracture mode of FVS0812 changes with temperature. At 175 C, it is characterized as dimpled rupture, and at 316 C as mixed matrix superplastic rupture and matrix-dipersoid debonding.

Leng, Yang↗

Effect of Surface Treatments on Electron Beam Freeform Fabricated Aluminum Structures

Electron beam freeform fabrication (EBF3) parts exhibit a ridged surface finish typical of many layer-additive processes. This, post-processing is required to produce a net shape with a smooth surface finish. High speed milling wire electrical discharge machining (EDM), electron beam glazing, and glass bead blasting were performed on EBF3-build 2219 aluminum alloy parts to reduce or eliminate the ridged surface features. Surface roughness, surface residual stress state, and microstructural characteristics were examined for each of the different surface treatment to assess the quality and effect of the surface treatments on the underlying material. The analysis evaluated the effectivenes of the different surface finishing techniques for achieving a smooth surface finish on an electron beam freeform fabricated part.

Taminger, Karen M. B.↗

Phase-field model of alloy solidification far from chemical equilibrium at the solid-liquid interface

We further develop a recently introduced phase-field model of far-from-equilibrium alloy solidification under additive manufacturing conditions [K. Ji et al., Phys. Rev. Lett. 130, 026203 (2023)]. This model utilizes enhanced solute diffusivity within the spatially diffuse interface region to quantitatively capture solute trapping with a larger interface width, thereby making simulations on experimentally relevant length and timescales computationally feasible. The main developments presented here include testing the robustness of different variational formulations, extending the model to concentrated alloys by incorporating solid and liquid free energies from thermodynamic databases, as illustrated for hypoeutectic Al-Ag alloys with CALPHAD, extending convergence tests as a function of interface width to 3D, and carrying out simulations in both 2D and 3D to examine existing theories of microstructure development. Our results indicate that the simplest variational formulation that interpolates the bulk free-energy density between its solid and liquid forms is the most robust. Remarkably, for hypoeutectic Al-Ag alloys, this formulation yields a high-velocity nonequilibrium phase diagram that is independent of interface width, thereby demonstrating that the framework of enhanced solute diffusivity can be nontrivially extended to concentrated alloys. Other variational formulations have restricted ranges of materials or processing parameters that can be reliably modeled. We use 2D simulations to construct high-velocity microstructure selection maps for dilute Al-Cu alloys. The results validate the important role of latent heat rejection at the interface and extend the limited predictions of linear stability analysis [A. Karma and A. Sarkissian, Phys. Rev. E 47, 513 (1993)] and sharp-interface 1D simulations to fully nonlinear regimes. Furthermore, 3D simulations, carried out using a computationally tractable axisymmetric cellular/dendritic interface shape, demonstrate a good convergence similar to that observed in 2D as a function of interface width. Full 3D simulations, in turn, reveal that the standard theory of absolute stability is a good predictor of the upper critical velocity beyond which steady-state growth becomes unstable, despite the different morphological manifestations of this instability in 2D and 3D.

36 MATERIALS SCIENCE↗

Multiscale and Machine Learning Modeling for Process-informed Microstructure Prediction in Additively Manufactured Materials Using MALAMUTE

Advanced Materials and Manufacturing Technologies (AMMT) program under the Department of Energy Office of Nuclear Energy, aims to develop and qualify additively-manufactured materials for nuclear applications. The key challenges to these efforts are the microstructural variabilities observed on the AM products and their impact on the properties and performance of the material in extreme environments. AMMT is using a combination of high-through-put experimental and modeling techniques to accelerate the qualification efforts. Conventionally, in-situ and ex-situ characterizations and testing are performed to correlate different aspects of the AM process to the final product and its performance. However, adopting a trial-and-error approach to experimentally evaluate the vast range of process parameters required to capture the microstructural variabilities is cost-prohibitive. Modeling and simulation provide a comparatively inexpensive way to understand and correlate the microstructural evolution to the processing conditions. The modeling and simulation work-packages within the AMMT program aims to use physics-based and machine learning modeling capabilities to develop a digital twin for AM that can correlate the process conditions to the final product and establish a process-structure-property-performance (PSPP) correlation for AM materials. The melting and subsequent solidification that occurs during the AM process is a complex phenomenon that requires multiscale multiphysics analysis. Idaho National Laboratory’s (INL) Multiphysics Object-Oriented Simulation Environment (MOOSE), specifically the MOOSE Application Library for Advanced Manufacturing UTilitiEs (MALAMUTE) software, provides an ideal platform for developing the multiphysics multiscale model to explore the intricacies of the microstructural evolution during the AM processes within a single framework. Furthermore, given that such full-fidelity simulations can be computationally intensive, reduced order models are necessary to explore the PSPP space for AM materials in an efficient, reliable, and cost-effective way. This work package focuses on understanding the role of process variabilities on the various microstructural characteristics of the AM materials. Microstructures unique to AM materials, such as compositional micro-heterogeneity and dislocation cells, are of particular interest here since they can influence the creep properties and radiation performance. In fiscal year (FY) 24, we significantly advanced upon our work in the last fiscal year, both on physics-based and ML models. The alloy solidification model available in MOOSE has been extended to incorporate the thermodynamic properties and free energy relevant to 316SS. The model demonstrates the Cr segregation that occurs during solidifcation. It is demonstrated that rate of solidification and solute segregation is primarily influence by the cooling rate dictating the level of freezing. This work captures the microstructural variabilities at the subgrain level that are often missing in the part-scale models. With an aim to connect the microstructural evolution model to realistic process conditions, a reduced order model is developed for predicting the thermal conditions around meltpool from high-fidelity process simulations. Furthermore, machine learning approach is used to accelerate the temperature prediction during the AM process. In the following years, MALAMUTE will be used to connect different aspects of the models and quantitatively predict the microstructural evolution. The developed ML-based surrogate model will consider the process conditions as the input to predict the microstructural features in a cost-effective way. The generated microstructures can be used by other work packages under AMMT to evaluate the properties and environmental response of the material at the mesoscale. Thus, this work help identify the key microstructural features at the subgrain level that are significant in property/performance prediction of the AM products. This work will provide inputs to the large-scale process variability models to reevaluate and validate assumptions/simplifications made in the part-scale models. Furthermore, through active learning this work will help identify the data need from both modeling and experimental sides for development of a robust digital twin for AM.

36 MATERIALS SCIENCE↗

Microstructural characterization of the HRSI thermal protection system for space shuttle

Components of the space shuttle high temperature reusable surface insulation (HRSI) system were microscopically characterized, both separately and as a system, to obtain information needed for stress analysis models of the thermal protection system. A tension specimen of the HRSI system was loaded in steps and was microscopically observed at each load condition to demonstrate the tension failure mode associated with strain isolation pad (SIP) behavior. A local failure occurred which should be associated with transfer of load through transverse fibers in the SIP. Stress concentrations attributed to the SIP behavior necessitated strengthening of the HRSI by densification of the RSI at the bondline. An HRSI tile was microscopically characterized after the densification process. The densified surface layer blended into the RSI which caused a gradual change in density. The gradation in density does not appear to represent a sharp discontinuity in elastic modulus between the densified layer and the parent material.

Ransone, P. O.↗

Harvesting Reactor Pressure Vessel Beltline Material from the Decommissioned Zion Nuclear Power Plant Unit 1

The decommissioning of the Zion Nuclear Power Plant (NPP) provided a unique opportunity to harvest and study service-aged reactor pressure vessel (RPV) beltline materials. This work, conducted through the U.S. Department of Energy’s Light Water Reactor Sustainability (LWRS) Program, aims to improve the understanding of radiation-induced embrittlement to support extended nuclear plant operations. Material segments containing the Linde 80 flux, wire heat 72105 (WF-70) beltline weld and the A533B Heat B7835-1 base metal, obtained from the intermediate shell region with a peak fluence of 0.7 × 10 19 n/cm 2 (E > 1.0 MeV), were extracted, cut into blocks, and machined into test specimens for mechanical and microstructural characterization. The segmentation process involved oxy-propane torch-cutting, followed by precision machining using wire saws and electrical discharge machining (EDM). A chemical composition analysis confirmed the expected variations in alloying elements, with copper levels being notably higher in the weld metal. The harvested specimens enable a detailed evaluation of through-wall embrittlement gradients, a comparison with the existing surveillance data, and the validation of predictive embrittlement models. This study provides critical data for assessing long-term reactor vessel integrity, informing aging-management strategies, and supporting regulatory decisions to extend the life of nuclear plants. This article is a revised and expanded version of a paper entitled, “Current Status of the Characterization of RPV Materials Harvested from the Decommissioned Zion Unit 1 Nuclear Power Plant”, PVP2017-65090, which was accepted and presented at the ASME 2017 Pressure Vessels and Piping Conference, Waikoloa, HI, USA, 16–20 July 2017.

harvesting beltline material↗