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At least 469 records · Page 26

TEM Observation of the Ti Interlayer Between SiC Substrates During Diffusion Bonding

Diffusion bonding was carried out to join SiC to SiC substrates using titanium interlayers. In this study, 10 m and 20 m thick physical vapor deposited (PVD) Ti surface coatings, and 10 and 20 m thick Ti foils were used. Diffusion bonding was performed at 1250 C for PVD Ti coatings and 1200 C for Ti foil. This study investigates the microstructures of the phases formed during diffusion bonding through TEM and selected-area diffraction analysis of a sample prepared with an FIB, which allows samples to be taken from the reacted area. In all samples, Ti3SiC2, Ti5Si3Cx and TiSi2 phases were identified. In addition, TiC and unknown phases also appeared in the samples in which Ti foils were used as interlayers. Furthermore, Ti3SiC2 phases show high concentration and Ti5Si3Cx formed less when samples were processed at a higher temperature and thinner interlayer samples were used. It appears that the formation of microcracks is caused by the presence of intermediate phase Ti5Si3Cx, which has anisotropic thermal expansion, and by the presence of an unidentified Ti-Si-C ternary phase with relatively low Si content.

Tsuda, Hiroshi↗

Tomography Analysis of Orion Artemis 1 Heatshield Sample

The Orion spacecraft, under NASA's Artemis program, is an integral step in humanity's ambitions of deep space exploration, including our return to the Moon and subsequent mission to Mars. The performance of Orion's heatshield is central to ensuring the safety and success of such missions. This presentation offers a comprehensive overview of the process used in and findings derived from tomography scans of an Artemis 1 heatshield sample executed at the Lawrence Berkeley National Laboratory's Advanced Light Source. These tomography scans captured high-resolution X-Ray images of the heatshield's microstructure, allowing advanced imaging to be employed for 3D image segmentation and visualization of the sample. The Porous Media Analysis (PuMA) software stands central to our analysis, offering robust computational algorithms and methodologies to digitally compute properties of the heatshield material. The presentation discusses the following derived metrics: - Volume fractions, representing the spatial distribution and amounts of various components throughout the heatshield’s depth. - Porosity and crack distributions, offering insights into the void space within the material, critical for understanding the heatshield's structural integrity. - Fiber orientation, detailing the alignment and arrangement of fibers, significant for material orthotropy. - Permeability estimates, quantifying the passage of gas through the material, relevant for re-entry conditions and pyrolysis gasses. One distinctive feature of this study is the comparative evaluation against data obtained from tomography scans of the Exploration Flight Test-1 (EFT-1) heatshield. Such a comparison offers multiple insights, including evaluation of the consistency and repeatability of manufacturing processes as well as understanding of any evolutionary changes in heatshield design or material properties.

Micro-tomography↗

Benchmarking machine learning strategies for phase-field problems

Abstract We present a comprehensive benchmarking framework for evaluating machine-learning approaches applied to phase-field problems. This framework focuses on four key analysis areas crucial for assessing the performance of such approaches in a systematic and structured way. Firstly, interpolation tasks are examined to identify trends in prediction accuracy and accumulation of error over simulation time. Secondly, extrapolation tasks are also evaluated according to the same metrics. Thirdly, the relationship between model performance and data requirements is investigated to understand the impact on predictions and robustness of these approaches. Finally, systematic errors are analyzed to identify specific events or inadvertent rare events triggering high errors. Quantitative metrics evaluating the local and global description of the microstructure evolution, along with other scalar metrics representative of phase-field problems, are used across these four analysis areas. This benchmarking framework provides a path to evaluate the effectiveness and limitations of machine-learning strategies applied to phase-field problems, ultimately facilitating their practical application.

36 MATERIALS SCIENCE↗

Experimental and Theoretical Thermokinetic Analysis of the Na 3 VO 4 –CO 2 Reaction System under Different Physicochemical Conditions

Sodium vanadate (Na 3 VO 4 ) was synthesized, structural and microstructurally characterized as well as tested as possible carbon dioxide (CO 2 ) captor through thermodynamic calculations in addition to thermogravimetric dynamic and isothermal analyses. Ceramic structural characterization evidenced the formation of the Na 3 VO 4 crystal phase, while microstructural features evidenced dense agglomerates with a poor specific surface area, although synthesis temperature (600 °C) was not as high as that for other sodium ceramics. Na 3 VO 4 was investigated for the CO 2 capture process through dynamic and isothermal experiments, in the presence or absence of oxygen. All these experiments showed that Na 3 VO 4 possesses interesting CO 2 capture properties in a specific temperature range (520 and 600 °C). Isothermal products characterization allowed to elucidate the reaction pathway, implying the Na 4 V 2 O 7 formation, as possible reactive intermediate. In fact, reaction path evolution was supported with theoretical thermodynamic data. Moreover, the kinetic analysis, performed using the Avrami-Erofeev mathematical model and subsequent thermodynamic data obtention, probed the positive influence of the temperature, in both CO 2 superficial and bulk chemical sorption processes, while oxygen addition did not enhance the superficial process. Additionally, as it would be expected, kinetics were enhanced as a function of the CO 2 concentration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Scaling effects of defects in fiber-reinforced composites

Material defects may be introduced willingly or unwillingly during material manufacturing and structural component fabrication stages. Their presence in the material plays a dominant role in determining the material's strength and the associate failure mechanisms. In the sense that the size and the number of defects may increase with the volume of the material, the effect of dimensional scaling may manifest itself in the dependence of material strength on volume. Or, alternatively, there may exist a scaling effect of material defects. In fiber-reinforced composites, manufacturing or fabrication defects may come in several forms: matrix voids, matrix microcracks, fiber misalignment, broken fibers, or interface disbonds, just to mention a few. These are interacting and competing defects in the sense that one type of defect may become dominant under one stress condition and another type of defect may become dominant under a different stress condition. This happens because the fiber reinforcement network, together with the distribution of defects, constitutes the prime microstructure of the composite, and there exist continued interactions between the evolving microstructure and the distribution of defects. In the process, the scaling effects of defects are complicated by this interaction. In this presentation, the scaling effects of defects in fiber-reinforced composites will be briefly discussed with the introduction of the concept of effective defects. It is then shown with the aid of some actual experimental and analysis results that the scaling effects are very much present, but they are regulated by the characteristic dimension of the composite microstructure due to the aforementioned microstructure-defect interaction effect.

Wang, A. S. D.↗

Influence of cobalt, tantalum, and tungsten on the microstructure and mechanical properties of superalloy single crystals

The influence of Co, Ta, and W on the microstructure and mechanical properties of nickel base super-alloy single crystals was investigated. A matrix of alloys was based on Mar-M 247 stripped of C, B, Zr, and Hf. The microstructures of the alloys were examined using optical and electron microscopy, phase extraction, X-ray diffraction, and differential thermal analysis. Tensile and creep-rupture tests were performed at 1000 C. An increase in tensile and creep strength resulted when Co was removed from alloys containing high refractory metal contents, but Co effects were negligible for alloys with lower refractory metal levels. In the composition range studied, W was more effective than Ta in increasing the creep resistance. The mechanical properties are discussed in relation to the microstructures of the alloys.

Nathal, M. V.↗

Thin-sectioning and microanalysis of individual extraterrestrial particles

A long standing constraint on the study of micrometeorites has centered on difficulties in preparing them for analysis. This is due largely to their small dimensions and consequent practical limitations on sample manipulation. Chondritic micrometeorites provide a good example; although much has been learned about their chemistry and mineralogy almost nothing was known about such basic properties as texture and petrographic associations. The only way to assess such properties is to examine microstructure indigenous to the particles. Unfortunately, almost all micrometeorites, out of necessity, have been crushed and dispersed onto appropriate substances prior to analysis, and most information about texture and petrography was lost. Recently, thin-sections of individual extraterrestrial particles have been prepared using an ultramicrotome equipped with a diamond knife. This procedure has been applied to stratospheric micrometeorites and Solar Max impact debris. In both cases the sections have enabled observation of a variety of internal particle features, including textures, porosity, and petrographic associations. The sectioning procedure is described and analysis results for chondritic micrometeoroids and select particles from Solar Max are presented.

Bradley, J. P.↗

Theoretical analysis of segmented Wolter/LSM X-ray telescope systems

The Segmented Wolter I/LSM X-ray Telescope, which consists of a Wolter I Telescope with a tilted, off-axis convex spherical Layered Synthetic Microstructure (LSM) optics placed near the primary focus to accommodate multiple off-axis detectors, has been analyzed. The Skylab ATM Experiment S056 Wolter I telescope and the Stanford/MSFC nested Wolter-Schwarzschild x-ray telescope have been considered as the primary optics. A ray trace analysis has been performed to calculate the RMS blur circle radius, point spread function (PSF), the meridional and sagittal line functions (LST), and the full width half maximum (PWHM) of the PSF to study the spatial resolution of the system. The effects on resolution of defocussing the image plane, tilting and decentrating of the multilayer (LSM) optics have also been investigated to give the mounting and alignment tolerances of the LSM optic. Comparison has been made between the performance of the segmented Wolter/LSM optical system and that of the Spectral Slicing X-ray Telescope (SSXRT) systems.

Shealy, D. L.↗

Microstructural transitions during containerless processing of undercooled Fe-Ni alloys

In order to identify the possible hierarchy of microstructural pathways and transitions, a systematic evaluation of the microstructural evolution in undercooled Fe-Ni alloys was performed on uniformly processed samples covering seven orders of magnitude in volume. At appropriate undercooling levels, alternate solidification pathways become thermodynamically possible and metastable product structures can result from the operation of competitive solidification kinetics. For thermal history evaluation, a heat flow analysis was applied and tested with large Fe-Ni alloy particles (1 to 3 mm) to assess undercooling potential. Alloy powders (10 to 150 microns), with large liquid undercoolings, were studied under the same composition and processing conditions to evaluate the solidification kinetics and microstructural evolution, including fcc/bcc phase selection and the thermal stability of a retained metastable bcc phase. The identification of microstructural transitions with controlled variations in sample size and composition during containerless solidification processing was used to develop a microstructure map which delineates regimes of structural evolutions and provides a unified analysis of experimental observations in the Fe-Ni system.

Thoma, D. J.↗

STUDIES ON PIPELINE POLYETHYLENES IN HYDROGEN GAS ENVIRONMENTS USING IN-SITU AND EX-SITU CHARACTERIZATION METHODS

Polymeric materials are commonplace in the natural gas infrastructure as distribution pipes, coatings, seals, and gaskets. Under the auspices of the U.S. Department of Energy HyBlend program, one of the means to reduce greenhouse gas emissions is with replacing natural gas, either partially or completely, with hydrogen. This approach makes it imperative that we conduct near-term and long-term materials compatibility research in these relevant environments. Insights into the effects of hydrogen and hydrogen gas blends on polymer integrity can be gained through both ex-situ and in-situ analytical methods. Our work represented here highlights a study of the behavior of pipeline polyethylene (PE) materials, including HDPE (Dow 2490 and GDB50) and MDPE (Ineos and legacy Dupont Aldyl A), when exposed to hydrogen by means of in-situ X-ray scattering and ex-situ Raman spectroscopy techniques. Samples were tested in ex-situ hydrogen and argon gas environments and in-situ hydrogen environments to identify differences due to permeation and solubility of these gases. These methods complemented each other because Raman spectroscopy could capture permanent effects after materials were removed from gaseous environments, and in-situ X-ray scattering analysis collected real-time data to elucidate the impact of the gas environment on polymer microstructure. Data collected revealed that the aforementioned polymers did not show significant changes in crystallinity and microstructure under the exposure conditions tested. Our findings from these studies will help establish real-time effects caused by hydrogen gas transport through pipeline polyethylenes by way of its influence on polymer structure and chemistry, which is directly related to pipeline mechanical strength and longevity of service.

Hydrogen materials compatibility, Natural gas pipe↗

Status Report on Characterization of High Burnup Fuel with Advanced Nondestructive Pulsed Neutron PIE

Characterizing irradiated or spent nuclear fuels with pulsed neutron techniques provides microstructural data such as phase fractions as well as crystallographic data, e.g. lattice parameters, from diffraction analysis. Diffraction characterization is complemented by spatially resolved mapping of isotope densities from energy-resolved neutron imaging, in particular neutron absorption resonance imaging, and overall bulk isotope assay with better sensitivity for minority isotopes from neutron absorption resonance spectroscopy without spatial resolution. Furthermore, after characterization at ambient condition, heating of irradiated or spent fuel will allow to characterize differences of e.g. lattice thermal expansion or phase transition temperature and kinetics compared to fresh fuel as well as enable the study of disappearance of irradiation defects. This data enables benchmarking of predictions of properties of irradiated fuels for which otherwise experimental data is sparse. The effort described here strives to characterize a section cut from a high-burnup fuel. Volumes smaller than entire fuel pellets or rodlets as proposed here, e.g. sections cut from a fuel pellet, to pave the way to characterize entire pellets or rodlets in the future.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ferromagnetic phase-mass equivalence and lunar sample magnetic remanence

Man-made alloy spheres simulating the compositions of particles found in the lunar soil and weighting approximately 10 mg are shown to be equivalent, insofar as remanence intensity and demagnetization stability are concerned, to more than about 10 billion submicrometer spherical iron particles. The large particles not only contain large stable magnetic remanence, but when the polished surfaces of these particles are etched and carefully studied, they provide useful petrogenetic information, imply the mechanism of magnetization, the time-temperature history, and outline the format for possible paleointensity analysis. The intensity and stability of the remanence in these large spheres is related to the microstructure developed during rapid cooling.

Wasilewski, P. J.↗

Quantitative characterization of spatial distribution of particles in materials: Application to materials processing

Most engineering materials contain second phase particles or fibers which serve to reinforce the matrix phase. The effect of reinforcements on material properties is usually analyzed in terms of the average volume fraction and spacing of reinforcements, quantities which are global microstructural characteristics. However, material properties can also depend on local microstructural characteristics; for example, on how uniformly the reinforcing phase is distributed in the material. The analysis method will then be applied to a materials processing problem to discover how processing parameters can be selected to maximize redistribution of the reinforcing phase during processing. Several mathematical analysis methods could be adapted to the problem of characterizing the distribution of particles in materials. A tessellation-based method was selected. In the first phase of the investigation, a software package was written to automate the analysis. Typical results are shown. The analysis technique allows the degree to which particles are clustered together, the size and spacing of particle clusters, and the particle density in clusters to be found. The analysis methods were applied to computer-generated distributions and to a few real particle-containing materials. Methods for analyzing a nonuniform particle distribution in a material can be applied to two broad classes of materials science problems: understanding how the resulting particle distribution affects properties. The analysis method described is applied to a materials processing problem: how to select extrusion conditions to maximize the redistribution of reinforcing particles that are initially nonuniformly distributed. In addition, the tessellation-based method to analyze star distributions in spiral galaxies was adapted, illustrating the diverse types of problems to which the analysis method can be applied.

Parse, J. B.↗

Effect of Environmental Exposures on Fatigue Life of P/M Disk Superalloys

As the temperature capability of Ni-base superalloy powder metallurgy disks is steadily increased, environmental resistance and protection of advanced nickel-based turbine disk components are becoming increasingly important. Localized surface hot corrosion attack and damage from oxidation have been shown to impair disk fatigue life and may eventually limit disk operating temperatures. NASA Research Announcement (NRA) contracts have been awarded to GE Aviation and Honeywell Aerospace to separately develop fatigue resistant metallic and ceramic coatings for corrosion resistance and the corrosion/fatigue results of selected coatings will be presented. The microstructural response of a bare ME3 disk superalloy has been evaluated for moderate (704 C) and aggressive (760-816 C) oxidizing exposures up to 2,020 hours. Cross section analysis reveals sub-surface damage (significant for aggressive exposures) that consists of Al2O3 "fingers", interfacial voids, a recrystallized precipitate-free layer and GB carbide dissolution. The effects of a Nichrome corrosion coating on this microstructural response will also be presented.

Draper, Susan↗

Coupled phase field damage and crystal plasticity analysis of intragranular fracture: The role of crystallographic orientation and voids

Damage evolution in engineering metal alloys at the grain scale exhibits significant microstructural heterogeneity and anisotropy. These heterogeneities create local hotspots for stress and strain localization, leading to void nucleation. Crystal orientation influences the active slip systems around voids, affecting lattice rotation and potentially forming discontinuities. At low triaxiality, voids may change shape due to lower stress, rotation, elongation, and coalescence. At high triaxiality, the correlation between crystal orientation and void growth rate becomes stronger, resembling the behavior observed in isolated single crystals. Therefore, understanding the effects of crystal orientation, heterogeneous strain, and defect evolution is crucial for single crystal fracture characterization. Here, in this work, a coupled phase-field damage (PFD) and crystal plasticity (CP) model is implemented within a finite element framework to analyze crystal deformation and failure. The CP method employs a dislocation density-based constitutive model, while intragranular failure is modeled using an anisotropic PFD method. The PFD model considers both the stored energy due to elastic stretching and the energy release due to defect formation and crack formation. A single crystal Al2219 with an intracrystalline spherical void is chosen to analyze fracture. The study finds that fracture propagation is strongly correlated with crystal orientations. This coupled CP-PFD model provides accurate failure prediction in crystalline materials by incorporating the effects of crystal orientations and existing voids. This study demonstrates how the local microstructure and defects influence plastic deformation and failure mechanisms in metal alloys.

Aluminum alloy↗

Microstructural and Defect Characterization in Ceramic Composites Using an Ultrasonic Guided Wave Scan System

In this study, an ultrasonic guided wave scan system was used to characterize various microstructural and flaw conditions in two types of ceramic matrix composites, SiC/SiC and C/SiC. Rather than attempting to isolate specific lamb wave modes to use for characterization (as is desired for many types of guided wave inspection problems), the guided wave scan system utilizes the total (multi-mode) ultrasonic response in its inspection analysis. Several time and frequency-domain parameters are calculated from the ultrasonic guided wave signal at each scan location to form images. Microstructural and defect conditions examined include delamination, density variation, cracking, and pre/ post-infiltration. Results are compared with thermographic imaging methods. Although the guided wave technique is commonly used so scanning can be eliminated, applying the technique in the scanning mode allows a more precise characterization of defect conditions.

Roth, D. J.↗

Mechanical Properties and Microstructure Investigation of Lead Free Solder

While the electronics industry appears to be focusing on Sn-Ag-Cu as the alloy of choice for lead free electronics assembly, ,the exact composition varies by geographic region, supplier and user. Add to that dissolved copper and silver from the printed circuit board traces and surface finish, and there can be significant variation in the final solder joint composition. A systematic study of the mechanical and microstructural properties of Sn-Ag-Cu alloys with Ag varying from 2wt% to 4wt% and Cu varying from 0.5wt% to lSwt%, was undertaken in this research study. Different sample preparation techniques (water quenched, oil quenched and water quenched followed by reflow) were explored and the resulting microstructure compared to that of a typical reflowed lead free chip scale package (CSP) solder joint. Tensile properties (modulus, 0.2% yield strength and the ultimate tensile strength) and creep behavior of selected alloy compositions (Sn-4Ag-1 X u , Sn-4Ag-OSCu, Sn- 2Ag-1 X u , Sn-2Ag-OSCu, Sn-3.5Ag-O.SCu) were determined for three conditions: as- cast; aged for 100 hours at 125OC; and aged for 250 hours at 125OC. There was no significant difference in Young's Modulus as a function of alloy composition. After an initial decrease in modulus after 100 hours at 125"C, there was an insignificant change with further aging. The distribution of 0.2% strain yield stress and ultimate tensile strength as a function of alloy composition was more significant and decreased with aging time and temperature. The microstructures of these alloys were examined using light and scanning electron microscopy (LM and SEM) respectively and SEM based energy dispersive x-ray spectroscopy (EDS). Fracture surface and cross-section analysis were performed on the specimens after creep testing. The creep testing results and the effect of high temperature aging on mechanical properties is presented for the oil quenched samples. In general the microstructure of oil quenched specimen exhibited a eutectic region of Sn with moderately dispersed Ag3Sn intermetallic, surrounded by a dendritic Sn-rich phase. The SEM images of the fracture surface indicated the presence of a tough shear surface at the initial cavity break area and a break line in the middle of specimen along the failure direction. A hyperbolic-sine creep model was adopted and used to fit the creep experiment data. The effect on the mechanical properties by adding the quaternary element bismuth to the Sn-3.5Ag-0.8Cu alloy was measured and compared with the mechanical properties of the ternary alloys. The results of this research study provide necessary data for the modeling of solder joint reliability for a range of Sn-Ag-Cu compositions and a baseline for evaluating the effects of subsequent quaternary additions.

Wang, Qing↗

Forensic characterization of surrogate nuclear explosion debris: radiochemical and spectroscopic strategies for method validation

Surrogate nuclear explosion debris (SNED) has emerged as a critical platform for advancing post-detonation nuclear forensic analysis in the absence of readily accessible historic materials. SNED enables controlled investigation and validation of analytical methodologies used to interrogate the chemical, isotopic, radiological, and microstructural signatures preserved in nuclear explosion debris. This review presents an integrated assessment of destructive and non-destructive analytical techniques commonly employed within decision-driven nuclear forensic workflows. Each technique is discussed individually while highlighting how it contributes to different stages of post-detonation analysis. Core methods – including gamma and alpha spectrometry, ICP-MS, TIMS, SIMS, SEM-EDS, XRF, LIBS, vibrational spectroscopy, and X-ray absorption spectroscopy – are critically evaluated with respect to forensic maturity, information content, and matrix limitations. Emphasis is placed on the role of SNED in benchmarking multi-modal workflows and identifying gaps in reproducing heterogeneity, fractionation, and radiation-driven evolution relevant to forensic attribution.

X-ray spectroscopic methods↗