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At least 865 records · Page 48

Uncertainty Quantification and Sensitivity Analysis in Process-Structure-Property Simulations for Laser Powder Bed Fusion Additive Manufacturing

Process variations and process-induced defects like porosity cause significant uncertainty in the microstructure and mechanical behavior of additively manufactured metals. Establishing process-structure-property (PSP) relationships and quantifying uncertainty using experiments alone is costly, especially for structural applications where mechanical allowables must be established for qualification and certification. This work presents a PSP simulation framework for laser powder bed fusion with a focus on uncertainty quantification through probabilistic calibration and multi-fidelity uncertainty propagation. Motivated by phenomenological input parameters related to grain nucleation and growth that are difficult to characterize, a global sensitivity analysis (GSA) is completed. Through GSA, the most important input parameters are identified based on their influence on the statistical distributions of microstructural metrics that influence mechanical behavior, including grain size, morphology, and crystallographic texture. The results provide insight on what experiments are necessary to quantify and control PSP uncertainties, particularly those associated with the more challenging input parameters.

additive manufacturing↗

Structural and optical analysis of Fe doped NiO nanoparticles synthesized by chemical precipitation route

Highlights: • The Fe doped NiO nanoparticles were synthesized by chemical precipitation route. • XRD analysis reveals cubic rock-salt fcc structure of the synthesized nanoparticles. • The Ni-O and Fe-O bonding were confirmed through FTIR spectroscopy. • Existence of nickel or interstitial oxygen vacancies indicates p-type nature of nanoparticles. - Abstract: The Ni{sub 1-x}Fe{sub x}O (x = 0.00, 0.02, 0.04 and 0.06) nanoparticles are synthesized by chemical precipitation route using polyvinyl-pyrrolidone (PVP) and nitrate metal salts. The results of thermogravimetric analysis (TGA) of the synthesized dried hydroxide powders showed that thermal decomposition occurs up to 500 °C so as to form pure Ni{sub 1-x}Fe{sub x}O. Therefore, all synthesized samples were calcined at 500 °C for 4 h and then used for further characterization. Energy dispersive X-ray spectroscopy (EDS) of all the samples showed the presence of Ni, O and Fe without any other impurities. From X-ray diffraction (XRD) and transmission electron microscopy (TEM) we could prove that the samples are polycrystalline in nature and are in single phase. The different vibrational modes in Ni{sub 1-x}Fe{sub x}O (x = 0.00, 0.02, 0.04 and 0.06) nanoparticles were studied by Raman spectroscopy and Fourier transform infrared spectroscopy (FTIR). Further, we analyzed the optical response from ultraviolet-visible spectra and Photoluminescence (PL) spectra.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Progress in Additively Manufactured Copper-Alloy GRCop-84, GRCop-42, and Bimetallic Combustion Chambers for Liquid Rocket Engines

Additive Manufacturing (AM) has significantly evolved over the last decade for use in the aerospace industry, particularly for liquid rocket engines. AM offers a considerable departure from traditional manufacturing to rapidly fabricate components with complex internal features. High performance liquid rocket engine combustion chambers that operate in a high heat flux environment are fabricated using a copper-alloy liner with a series of integral coolant channels. Copper-alloys provide the necessary conductivity and material strength for adequate design margins offering high performance without the need for film coolant. Copper-alloys present unique challenges to properly melt the powder in laser-based AM processes due to their high reflectivity and conductivity. Starting in 2014, NASA’s Marshall Space Flight Center (MSFC) and Glenn Research Center (GRC) have developed a process for AM of GRCop (Copper- Chrome-Niobium) alloys using Selective Laser Melting (SLM). GRCop, originally developed at GRC, is a high conductivity, high-strength, dispersion strengthened copper-alloy for use in high-temperature, high heat flux applications. NASA has completed significant material characterization and testing, along with hot-fire testing, to demonstrate that GRCop-42 and GRCop-84 alloys are suitable for use in combustion chambers. Additional development and testing has been completed on AM bimetallic chambers using GRCop-84 liners and superalloy jackets, fabricated using two Directed Energy Deposition (DED) processes: Electron Beam Freeform Fabrication (EBF³) and Blown Powder DED. NASA completed hot-fire testing on various AM chambers using GRCop-84, GRCop-42, and bimetallic chambers in Liquid Oxygen (LOX)/Hydrogen, LOX/Methane, and LOX/Kerosene propellants.

Gradl, Paul R.↗

SR19016 - Characterization of AM Materials for SRTE Service

This project addresses several issues and challenges for the use of AM produced components in the tritium facility. It will evaluate the effect of low level hydrogen and tritium exposure on the mechanical and chemical characteristics of Arcam A2X Electron Beam Powder Bed Fusion Produced (EPBF) Ti-6AI-4V by printing tensile samples and testing them in the as printed, machined, and hydrogen exposed conditions. Hydrogen uptake will be measured using an Eltra Hydrogen-Oxygen- Nitrogen analyzer. Hydride response will be measured using a Seiffert's apparatus and determining the effects of various surface treatments on the hydriding susceptibility. Tools, fixtures, and other objects will be deigned and printed for use in the AM lab and tritum facility and for other groups that support the tiritum mission.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Testing techniques for mechanical characterization of rapidly solidified materials

Mechanical property testing techniques are reviewed for rapidly solidified materials. Mechanical testing of rapidly solidified materials is complicated by the fact that in most cases at least one dimension of the material is very small (less than 100 microns). For some geometries, i.e., powder or thin surface layers, microhardness is the only feasible mechanical test. The ribbon geometry which is obtained by the melt-spinning method, however, has been used for a variety of mechanical property measurements including elastic properties, tensile properties, fracture toughness, creep, and fatigue. These techniques are described with emphasis placed on the precautions required by the restricted geometry of rapidly solidified specimens.

Koch, C. C.↗

Phase Stability of Yttrium Titanium Oxide

This proposed study aims at elevating Idaho National Laboratory (INL)’s portfolio in nuclear material research on two major fronts: 1) expanding INL’s material characterization capabilities to provide holistic microstructural and microchemical characterization ranging from atomic scale to millimeter scale, and 2) filling the knowledge gap on the effect of microstructural evolution on material phase stability at extreme conditions resembling those inside nuclear reactors, using Yttrium-Titanium-Oxide (YTO) as a model material. Previous research indicated the kinetics of phase transition of YTO materials varies between bulk samples and powder samples, suggesting that microstructural characteristics such as defect, micro-strain, and crystallite size could play a significant role in phase transition. The effect of crystallite size on the thermodynamics of phase transition has been well documented for other ceramic materials at nanometer crystallite size, with potential impacts from surface and strain energy and defects. In this proposed study, we will perform microstructural (micro-strain, crystallite size, defects, phase) and microchemical (elemental mapping) analyses through in-situ high temperature measurements using X-ray diffraction (XRD; at millimeter scale for powder and bulk samples) and transmission electron microscopy (TEM, at nanometer scale and atomic scale for powder and thin foil samples), to provide a comprehensive view of the effect of microstructural and microchemical evolution on phase transition and phase stability of YTO materials. These findings will also establish a roadmap and provide new insights on the phase stability of other materials that are critical to nuclear energy and other renewable energy infrastructure. Besides advancing our understanding of this fundamental material science question, this project will also enable the development of state-of-the-art material characterization capabilities at INL/MFC for microstructural and microchemical analysis at high temperature conditions. The new collaboration between the High-Resolution Materials Characterization group at INL and the Electron Microscopy group at the University of Florida (UF) in this project will open the possibilities for more fruitful and synergetic cutting-edge nuclear material research in the future.

36 MATERIALS SCIENCE↗

Microstructural diversity and digestion yields of select bituminous and subbituminous coals as raw material candidates for carbon fiber precursor production

Here, this work investigates the use of coals as raw materials for carbon fiber precursor production as a new alternative to coal utilization. Coal being a highly complex and heterogeneous material with different macerals and minerals complicates this task. Extensive microstructural characterization as well as preliminary digestion studies are performed on three bituminous coals (Herrin and Springfield from the Illinois Basin and the Blue Gem from the Central Appalachians) and one subbituminous coal from the Powder River Basin (Monarch), as raw material candidates. The subbituminous coal was richer in oxygen, lower in sulfur, and had a higher volatile matter yield. Microstructural investigations were performed using X-ray diffraction, X-ray/neutron computed tomography, scanning electron microscopy with energy dispersive spectroscopy, and petrology. Mild solvent extraction studies were conducted using creosote and decant oil as solvents in microreactors. The extraction yield was sensitive to temperature and time (350 to 450 °C between 30 and 120 mins.) for both creosote and decant oil digestions. While the Blue Gem coal had more desirable microstructural properties with less mineral content and cleaner macerals, it had the lowest coal conversion to quinoline soluble ‘liquid’ (of the bituminous coals). The lower coal conversion yield was hypothesized to be connected to the lack of FeS2 which could act as a catalyst when Fe is liberated from the structure under solvent extraction conditions. The Herrin and Springfield coals revealed similar microstructures and coal conversion efficiencies (higher than Blue Gem). These coals were the most promising candidates for further examination from this first approximations study. The subbituminous Monarch coal, however, was deemed less suitable due to poor coal conversion and less desirable microstructures. Additionally, the presented results with combined microstructural data from multiple length scales established a framework necessary for a first approximations study in this new coal utilization approach.

01 COAL, LIGNITE, AND PEAT↗

Adsorption of Iodine on Metal Coupons in Humid and Dry Environments

In this study, five different metal coupons were evaluated for gaseous iodine [I2(g)] adsorption including two stainless steels (i.e., SS304 and SS316), two Inconel® alloys (i.e., 625 and 718) and pure Ni (i.e., Ni-200) within a dynamic flow-through system where temperature, iodine concentration, flow rate, atmosphere, and relative humidity were controlled. Humidity was shown to be critical to iodine adsorption on SS304 and SS316 and Ni-200 at ambient temperatures. The results presented herein suggest that a moisture mediated reaction is occurring. However, higher humidity levels decrease the adsorption, suggesting an ideal range of humidity for highest corrosion. A comparison of the five metal substrates showed the highest I2(g) adsorption in the following descending order Ni-200 > SS304 > SS316 >718>625.The 625 and 718 Inconel alloys were fairly inert to iodine adsorption under the conditions tested. Characterization by scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction of the Ni-200 coupon indicates that NiI2 is formed and flakes off the surface as a black powder. The SS304 and SS316 coupons showed evidence of extensive reactions with I2(g) and formed a much more deliquescent corrosion product, which reacted with air when removed from the flow-through system for weighing on the analytical balance. These findings assist in predicting iodine adsorption behavior on a variety of metal surfaces under various conditions.

Beck, Chelsie L.↗

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗

Structural Insights into the Vapochromic Behavior of Pt- and Pd-Based Compounds

Anionic complexes having vapochromic behavior are investigated: [K(H 2 O)][M(ppy)(CN) 2 ], [K(H 2 O)][M(bzq)(CN) 2 ], and [Li(H 2 O) n ][Pt(bzq)(CN) 2 ], where ppy = 2-phenylpyridinate, bzq = 7,8-benzoquinolate, and M = Pt(II) or Pd(II). These hydrated potassium/lithium salts exhibit a change in color upon being heated to 380 K, and they transform back into the original color upon absorption of water molecules from the environment. The challenging characterization of their structure in the vapochromic transition has been carried out by combining several experimental techniques, despite the availability of partially ordered and/or impure crystalline material. Room-temperature single-crystal and powder X-ray diffraction investigation revealed that [K(H 2 O)][Pt(ppy)(CN) 2 ] crystallizes in the Pbca space group and is isostructural to [K(H 2 O)][Pd(ppy)(CN) 2 ]. Variable-temperature powder X-ray diffraction allowed the color transition to be related to changes in the diffraction pattern and the decrease in sample crystallinity. Water loss, monitored by thermogravimetric analysis, occurs in two stages, well separated for potassium Pt compounds and strongly overlapped for potassium Pd compounds. Furthermore, the local structure of potassium compounds was monitored by in situ pair distribution function (PDF) measurements, which highlighted changes in the intermolecular distances due to a rearrangement of the crystal packing upon vapochromic transition.

36 MATERIALS SCIENCE↗

Pressure-Stabilized MnSb2 with Complex Incommensurate Magnetic Order

Marcasite-type compounds have been proposed as promising hosts of exotic magnetic quantum states, yet experimental realizations in stoichiometric, disorder-free systems remain limited. Here, we report the high-pressure stabilization and magnetic characterization of MnSb2, a marcasite-type compound that is thermodynamically metastable under ambient pressure. Single crystals were synthesized using a cubic multianvil press at 3.3 GPa and 490 °C for 24 h, and powder and single-crystal X-ray diffraction confirm the orthorhombic Pnnm structure. These crystals are stable at ambient pressure for a long time up to between 450 and 500 K. Heat-capacity measurements reveal phase transitions at approximately T0 ∼ 118 K and T1 ∼ 220 K. Neutron diffraction uncovers an unconventional magnetic state below T1 ∼ 220 K. Magnetic powder neutron diffraction refinements reveal possible multiple magnetic configurations that provide comparably acceptable fits to the experimental data. While most solutions are consistent with a spin-density-wave (SDW) description, helical models systematically yield inferior agreement factors. Across a broad range of models, the Mn ordered moment reaches a maximum value of approximately 2 μB and remains predominantly collinear, with minimal canting along the c-axis. At 200 K, the magnetic propagation vector is q = (0, 0.3975, 0.3783); upon cooling, the b component increases toward 0.5, reflecting a temperature-dependent evolution of the modulation. The need for modification of the magnetic model between high and low temperatures further highlights the complex and strongly temperature-dependent nature of the magnetic order in this system. These results establish MnSb2 as a pressure-stabilized marcasite magnet with a tunable, complex magnetic state and a compelling stoichiometric platform for exploring unconventional magnetic behavior, including potential altermagnetism.

Xu, Mingyu [Michigan State University , , , ,; Iow↗

Interfacial transmetallation synthesis of a platinadithiolene nanosheet as a potential 2D topological insulator

The construction of two-dimensional metal complex materials is fascinating because of the structural and functional diversity of these materials. Previously, we have reported the synthesis of electroconductive nickelladithiolene (NiDT) and palladadithiolene (PdDT) nanosheets using benzenehexathiol (BHT). Down the group from Ni, Pd to Pt, there is a distinct positive shift in the reduction potential; as a result, it becomes synthetically more challenging to stabilize Pt 2+ than to form metallic Pt(0) in the presence of BHT as a reducing agent. Herein, a novel synthetic strategy for the preparation of platinadithiolene nanosheet (PtDT) using a dibutyltin-protected BHT ligand is reported, leading to transmetallation in the presence of dioxygen. Both free-standing stacked sheets and atomic layer sheets were obtained and characterized by microscopic techniques such as AFM, SEM, and TEM. To study the morphology of the sheets and determine their charge neutrality, X-ray photoelectron (XP) and infrared (IR) spectroscopic techniques were used. Powder X-ray diffraction analysis of the multilayer PtDT indicates a half-way slipped hexagonal configuration in the P 3¯1 m space group. The band structure of this PtDT exhibits a band gap at the Fermi level, which is different from that of NiDT in the staggered configuration, and a Dirac gap, indicating the possibility of 2D topological insulation at room temperature. PtDT is insulating but chemically activated by oxidation with I 2 to increase the conductivity by more than 106 folds up to 0.39 S cm –1 . The MDT sheets exhibit electrocatalytic activity for the hydrogen evolution reaction, and the activity order is NiDT < PdDT < PtDT.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Relationship of Chemical Composition and Moisture Sensitivity in LiNi x Mn y Co 1-x-y O 2 for Lithium-Ion Batteries

Chemical composition–moisture sensitivity relationship of LiNi x Mn y Co 1-x-y O 2 (NMC) cathode materials was investigated by exploring crystal structures, surface properties, and electrochemical performance behaviors of various commercial NMC powders: LiNi 1/3 Mn 1/3 Co 1/3 O 2 (NMC111), LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532), LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), and LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811). The NMC powders were stored in different moisture conditions: moisture-free, humidified air, or immersed in water. Rietveld refinement analysis of X-ray diffraction (XRD) data and scanning electron microscopy (SEM) were used to characterize the crystal structure changes and the evolution of particle surfaces morphologies. The effect of moisture contamination on the electrochemical properties of NMC cathodes was studied by galvanostatic cycling and electrochemical impedance spectroscopy (EIS). The moisture contamination resulted in either structural disorder or unwanted surficial deposition products, which increased a charge-transfer impedance and consequent performance degradation of battery cells. The results showed that NMC’s moisture vulnerability increased with Ni content (x) despite protective coatings on commercial particles, which stressed the necessity of alternative surface passivation strategies of Ni-rich NMC for broad applications such as electric vehicles and electrified aircraft propulsion.

25 ENERGY STORAGE↗

Program for plasma-sprayed self-lubricating coatings

A method for preparing composite powders of the three coating components was developed and a procedure that can be used in applying uniform coatings of the composite powders was demonstrated. Composite powders were prepared by adjusting particle sizes of the components and employing a small amount of monoaluminum phosphate as an inorganic binder. Quantitative microscopy (image analysis) was found to be a convenient method of characterizing the composition of the multiphase plasma-sprayed coatings. Area percentages and distribution of the components were readily obtained by this method. The adhesive strength of the coating to a nickel-chromium alloy substrate was increased by about 40 percent by a heat treatment of 20 hours at 650 C.

Walther, G. C.↗

Matrix effects for reflectivity spectra of dispersed nanophase (superparamagnetic) hematite with application to Martian spectral data

The effect of the matrix on the reflectivity spectra of nanophase (superparamagnetic) hematite (np-Hm) dispersed within the matrix was investigated in four series of powder samples containing np-Hm dispersed within discrete powder particles (of two size ranges) of silica gel and activated alumina. The spectral data show that matrix effects are large. Samples with the same Fe2O3 content can have np-Hm absorption edges characterized by very different positions and curvature and slope indices, while samples with equivalent absorption edges can have very different Fe2O3 concentrations. Thus, quantitative relationships between the positions of ferric absorption edges and Fe2O3 concentrations are unreliable without knowledge of matrix properties of the system. It is shown that it was possible to match the Fe2O3 concentration, magnetic properties, and spectral data for Martian surface material with a laboratory mixture whose only ferric-bearing phase was hematite.

Morris, Richard V.↗

Reactive Additive Manufacturing for Fourth Industrial Revolution Exploration Systems (Ramfire) Aluminum 6061-Ram2 Nozzle Testing

The NASA Marshall Space Flight Center (MSFC) has applied various forms of metallic additive manufacturing (AM) in liquid rocket engine component design, development, and testing since 2010. These AM techniques reduce hardware cost, shorten fabrication schedules, increase reliability by reducing the number of joints, and improve hardware performance by allowing unconventional design. The RAMFIRE project, funded under Space Technology Mission Directorate (STMD) Game Changing Development (GCD) Program, has furthered the use of novel AM liquid rocket nozzles in collaboration with Elementum 3D. The project advanced novel large-scale AM aluminum material technology for significant weight savings in rocket engines and launch vehicles. Previously, aluminum alloys were difficult to weld and print using additive manufacturing. Elementum 3D’s patented Aluminum 6061-RAM2 alloy allows for aluminum alloys to be printed using various AM techniques and at various scales. The alloy can be leveraged for welding wire, showing drastic improvements in aluminum weldability. The RAMFIRE project focuses on five key areas: 1) Laser Powder Directed Energy Deposition (LP-DED) AL6061-RAM2 feedstock specification and verification, 2) LP-DED process development and validation, 3) LP-DED printed AL6061-RAM2 microstructural and mechanical property characterization, 4) Hot-fire test a 7k-lbf thrust class regeneratively cooled nozzle, 5) Print large scale regeneratively cooled nozzle. Hot-fire testing demonstrates potential of advanced space technologies to NASA and potential users by providing the relevant environments to advance TRL levels to the 5/6 range.

Al6061-RAM2↗

RIMS analysis of isotopically tagged uranium particles with application to Intentional Forensics

Traditional nuclear forensics approaches leverage isotopic measurements for characterizing nuclear forensics signatures in fuel cycle materials. To aid in provenance assessment, isotopically perturbed transition metal taggants can be added to fuel cycle materials. We present a case study for examining natural uranium oxide powder that was tagged with isotopically perturbed Mo before and after irradiation using resonance ionization mass spectrometry. In conclusion, this method accurately and precisely measures taggant and uranium compositions, rapidly enabling the ability to clearly discriminate between tagged particles and other material with application for robust assessment of material provenance.

Forensic Anthropology↗

Synthesis and Characterization of Aluminum Matrix Composites Reinforced with (Ni,Cu){sub 3}Al Intermetallic Particles via Mechanical Milling Technique

This study investigates the dispersion of (Ni,Cu){sub 3}Al intermetallic particles in an aluminum matrix via low-energy mechanical milling as an alternative to conventional stir casting. The precursor powders consisted in (Ni,Cu){sub 3}Al and reactive-grade Al particles with an average size of 15 and 3 microns, respectively. The concentrations used were 3, 5, 8 and 10 wt.% of the intermetallic powders. After 4 h of milling, the obtained powders were compacted in a unidirectional press with a pressure of 930 MPa and the obtained green compacts were sintered at 500 °C in a controlled atmosphere oven for 2 h. Result showed that the bulk composites displayed an increase in the Vickers microhardness as well as an increase in compressive strength and stiffness as the percentage of dispersed particles increased. The Al-8 wt.%(Ni,Cu){sub 3}Al sample achieved the best performance and is related to the findings in SEM micrographs that showed that higher reinforcement concentration increased the formation of microporosities that reduce the decohesion of the bulk sample and impact heavily on the mechanical performance of the material.

36 MATERIALS SCIENCE↗