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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Engineering new limits to magnetostriction through metastability in iron-gallium alloys

Magnetostrictive materials transduce magnetic and mechanical energies and when combined with piezoelectric elements, evoke magnetoelectric transduction for high-sensitivity magnetic field sensors and energy-efficient beyond-CMOS technologies. The dearth of ductile, rare-earth-free materials with high magnetostrictive coefficients motivates the discovery of superior materials. Fe 1- x Ga x alloys are amongst the highest performing rare-earth-free magnetostrictive materials; however, magnetostriction becomes sharply suppressed beyond x = 19% due to the formation of a parasitic ordered intermetallic phase. Here, we harness epitaxy to extend the stability of the BCC Fe 1- x Ga x alloy to gallium compositions as high as x = 30% and in so doing dramatically boost the magnetostriction by as much as 10x relative to the bulk and 2x larger than canonical rare-earth based magnetostrictors. A Fe 1- x Ga x - [Pb(Mg 1/3 Nb 2/3 )O 3 ] 0.7 -[PbTiO 3 ] 0.3 (PMN-PT) composite magnetoelectric shows robust 90° electrical switching of magnetic anisotropy and a converse magnetoelectric coefficient of 2.0 × 10 -5 s m -1 . When optimally scaled, this high coefficient implies stable switching at ~80 aJ per bit.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Additive Manufacturing Flaw Assessment Methodology

An evolution fatigue data and flaw tolerance of components produced using the Powder Bed Fusion (PBF) Additive Manufacturing (AM) process is documented in this report. Initial differences in fatigue data for AM components compared to smooth bar fatigue data indicated a need for a more detailed analysis of AM data available in technical literature. The investigation was initiated to support the development of a fatigue analysis methodology for AM components to support the of codification of AM technology for pressure equipment. The project was initiated to collect and analyze stainless steel 304L and 316L AM fatigue test data and corresponding process and quality information to develop S-N and E-N based fatigue data representation. Additional AM fatigue test data including Inconel Ti-6-4 and aluminum alloys were also considered for comparison purposes Metallic AM parts tend to contain various forms of defects distributed throughout the part. If an AM part is subjected to fatigue loading in service, a fatigue analysis needs to be performed during the design process to ensure an acceptable service life for the part. Post-process machining and polishing do not to improve fatigue resistance in any significant degree. The low cycle fatigue regime is of particular interest to this project in support of flaw acceptance criteria currently under development by ASME’s BPTCS/BNCS. Internal defects become exposed as external surface defects during machining for the machining of the AM part to final dimensions. This implies that as long as inherent AM defects are within a controlled limit in terms of both size and distribution characteristics, the corresponding fatigue test data in terms of either S-N (stress life) or E-N (strain life) can be investigated and characterized to establish fatigue properties of AM parts for design and fatigue evaluation purposes. The resulting S-N or E-N curves and their scatter bands can be used to derive fatigue design allowable stress values by capturing the effects of distributed discontinuities within an acceptable limit.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Combining synchrotron X-ray diffraction, mechanistic modeling and machine learning for in situ subsurface temperature quantification during laser melting

Laser melting, such as that encountered during additive manufacturing, produces extreme gradients of temperature in both space and time, which in turn influence microstructural development in the material. Qualification and model validation of the process itself and the resulting material necessitate the ability to characterize these temperature fields. However, well established means to directly probe the material temperature below the surface of an alloy while it is being processed are limited. To address this gap in characterization capabilities, a novel means is presented to extract subsurface temperature-distribution metrics, with uncertainty, from in situ synchrotron X-ray diffraction measurements to provide quantitative temperature evolution data during laser melting. Temperature-distribution metrics are determined using Gaussian process regression supervised machine-learning surrogate models trained with a combination of mechanistic modeling (heat transfer and fluid flow) and X-ray diffraction simulation. The trained surrogate model uncertainties are found to range from 5 to 15% depending on the metric and current temperature. The surrogate models are then applied to experimental data to extract temperature metrics from an Inconel 625 nickel superalloy wall specimen during laser melting. The maximum temperatures of the solid phase in the diffraction volume through melting and cooling are found to reach the solidus temperature as expected, with the mean and minimum temperatures found to be several hundred degrees less. The extracted temperature metrics near melting are determined to be more accurate because of the lower relative levels of mechanical elastic strains. However, uncertainties for temperature metrics during cooling are increased due to the effects of thermomechanical stress.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Imaging the magnetic nanowire cross section and magnetic ordering within a suspended 3D artificial spin-ice

Artificial spin-ice systems are patterned arrays of magnetic nanoislands arranged into frustrated geometries and provide insight into the physics of ordering and emergence. The majority of these systems have been realized in two-dimensions, mainly due to the ease of fabrication, but with recent developments in advanced nanolithography, three-dimensional artificial spin ice (ASI) structures have become possible, providing a new paradigm in their study. Such artificially engineered 3D systems provide new opportunities in realizing tunable ground states, new domain wall topologies, monopole propagation, and advanced device concepts, such as magnetic racetrack memory. Direct imaging of 3DASI structures with magnetic force microscopy has thus far been key to probing the physics of these systems but is limited in both the depth of measurement and resolution, ultimately restricting measurement to the uppermost layers of the system. In this work, a method is developed to fabricate 3DASI lattices over an aperture using two-photon lithography, thermal evaporation, and oxygen plasma exposure, allowing the probe of element-specific structural and magnetic information using soft x-ray microscopy with x-ray magnetic circular dichroism (XMCD) as magnetic contrast. The suspended polymer–permalloy lattices are found to be stable under repeated soft x-ray exposure. Analysis of the x-ray absorption signal allows the complex cross section of the magnetic nanowires to be reconstructed and demonstrates a crescent-shaped geometry. Measurement of the XMCD images after the application of an in-plane field suggests a decrease in magnetic moment on the lattice surface due to oxidation, while a measurable signal is retained on sub-lattices below the surface.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanoscale imaging of phonon dynamics by electron microscopy

Spatially resolved vibrational mapping of nanostructures is indispensable to the development and understanding of thermal nanodevices, modulation of thermal transport and novel nanostructured thermoelectric materials. Through the engineering of complex structures, such as alloys, nanostructures and superlattice interfaces, one can significantly alter the propagation of phonons and suppress material thermal conductivity while maintaining electrical conductivity. There have been no correlative experiments that spatially track the modulation of phonon properties in and around nanostructures due to spatial resolution limitations of conventional optical phonon detection techniques. Here we demonstrate two-dimensional spatial mapping of phonons in a single silicon–germanium (SiGe) quantum dot (QD) using monochromated electron energy loss spectroscopy in the transmission electron microscope. Tracking the variation of the Si optical mode in and around the QD, we observe the nanoscale modification of the composition-induced red shift. We observe non-equilibrium phonons that only exist near the interface and, furthermore, develop a novel technique to differentially map phonon momenta, providing direct evidence that the interplay between diffuse and specular reflection largely depends on the detailed atomistic structure: a major advancement in the field. Our work unveils the non-equilibrium phonon dynamics at nanoscale interfaces and can be used to study actual nanodevices and aid in the understanding of heat dissipation near nanoscale hotspots, which is crucial for future high-performance nanoelectronics.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Tribological Behavior of Structural Materials in High Temperature Helium Gas-Cooled Reactor Environments

The High-Temperature Gas-cooled Reactor (HTGR) is a Generation IV concept designed to produce electricity and hydrogen at high efficiencies via high operating temperatures (700 °C or higher). Helium, the primary coolant for HTGRs, contains impurities (e.g., CO, H2O and CH4) that can induce corrosion reactions at high temperatures such as oxidation and (de)carburization, which in turn can affect the tribological behavior of components. Incoloy® 800HT (Ni-Fe-Cr austenitic solid-solution alloy) and Inconel® 617 (Ni-Cr-Co-Mo solid-solution alloy) are two high-temperature superalloys currently selected as candidate structural materials for the HTGR. The objective of this study is to evaluate the high-temperature tribological performance of these two candidate alloys after conditioning them in HTGR environments. Four regimes of corrosion were considered: a non-conditioned regime (Regime I), an oxidizing regime (Regime II), a carburizing and oxidizing regime (Regime III), and a carburizing regime (Regime IV). To simulate oxidation in HTGR, samples were conditioned for 22 days at elevated temperatures in a once-through helium loop with 4 ppmv H2O. Carburization of the samples was achieved by the commercial process, Kolsterising®. In addition, two surface treatments – shot peening and aluminization – were considered as potential routes of improving the alloys’ wear resistance. Surface-treated samples were tested both before and after conditioning in Regime II. Tribological testing of the samples was performed via a pin-on-disk tribometer at elevated temperatures in ambient environment – 650 and 750°C for 800HT; 850 and 900°C for 617 – with applied loads of 1N, 2N and 5N. The wear behavior of the alloys was assessed via wear volume and friction coefficient measurements, supported by morphological, structural and compositional analyses of the wear tracks. Conditioning the samples in Regime II led to the formation of a chromium oxide on both alloys. This protective scale increased the wear resistance compared to that of as-received samples (Regime I) due to the formation of a compacted ‘glaze’ oxide layer during sliding, rendering the wear track nearly undistinguishable from the unworn background and resulting in wear volumes below the detection limits of the measurement technique. The variability of the friction coefficients of the conditioned samples was also considerably reduced compared to that of the as-received samples due to the glaze layer. Additionally, the initial friction coefficients of the samples conditioned in Regime II were reduced by 45% and 54% compared to those of as-received samples for alloys 800HT and 617, respectively. Carburizing the samples (Regime IV) hardened the surfaces of both alloys and promoted the formation of an iron oxide on 800HT during tribological testing, thereby increasing the wear resistance and decreasing the initial friction coefficient by a factor of two compared to those of as-received 800HT. Alloy 617 exhibited an enhanced wear resistance but similar initial friction coefficient compared to those of as-received samples due to the increased surface hardness. The Mn-Cr oxide developed during Regime III conditioning of 800HT did not develop a glaze layer during tribotesting, even at lower loads. Thus, it was not as protective as the oxide produced during conditioning of Regime II samples, leading to lower wear resistance of 800HT in Regime III compared to that measured in the Regime II condition. 800HT benefited from the aluminization surface treatment, particularly before conditioning in Regime II, due to the promotion of a wear-resistant aluminum oxide layer during testing and the increase in surface hardness due to the presence of a FeAl intermetallic phase. The presence of this phase caused an order-of-magnitude reduction in wear volumes compared to those of as-received 800HT. Aluminization of 617 decreased its wear resistance, particularly after conditioning in Regime II, due to significant wear of the aluminum oxide via a ceramic wear mechanism. This aluminum oxide was removed during sliding, causing the wear volumes to increase by a factor of five compared to those of 617 conditioned in Regime II. Shot-peened 800HT exhibited a tribological behavior similar to that of as-received 800HT, despite an enhancement in the rate of chromium oxide formation. Shot-peened 800HT conditioned in Regime II showed lower wear resistance compared to that of 800HT conditioned in Regime II due to the poor adhesion between the oxide and the underlying metal, preventing the formation of the glaze layer during sliding. Shot peening of 617 increased its wear resistance at higher load, reducing worn volumes by 60% compared to that measured with as-received 617. Tribotesting of shot-peened 617 in Regime II revealed that the glaze-oxide layer was formed at every load, resulting in negligible wear, similar to what was observed from testing 617 after conditioning in Regime II. Overall, alloy 617 exhibited tribologically superior behavior compared to that of alloy 800HT, as demonstrated by its lower friction coefficients and its order-of-magnitude lower wear volumes when measurable.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Thermodynamic modeling of the Pd–Zn system with uncertainty quantification and its implication to tailor catalysts

Pd–Zn intermetallic catalysts show encouraging combinations of activity and selectivity on well-defined active site ensembles. Thermodynamic description of the Pd–Zn system, delineating phase boundaries and enumerating site occupancies within intermediate alloy phases, is essential to determining the ensembles of Pd–Zn atoms as a function of composition and temperature. Combining the present extensive first-principles calculations based on density functional theory (DFT) and available experimental data, the Pd–Zn system was remodeled using the CALculation of PHAse Diagrams (CALPHAD) approach. High throughput modeling tools with uncertainty quantification, i.e., ESPEI and PyCalphad, were incorporated in the phase analysis. Here, the site occupancies across the γ phase composition region were given special attention. A four-sublattice model was used for the γ phase owing to its four Wyckoff positions, i.e., the outer tetrahedral (OT) site 8c, the inner tetrahedral (IT) site 8c, the octahedral (OH) site 12e, and the cuboctahedral (CO) site 24g. The site fractions of Pd and Zn calculated from the present thermodynamic model show the occupancy preference of Pd in the OT and OH sublattices in agreement with experimental observations. The force constants obtained from DFT-based phonon calculations further supports the tendency of Pd occupying the OH sublattice compared with the IT and CO sublattice. The catalytic ensembles changing from Pd monomers (Pd 1 ) to trimers (Pd 3 ) on the surface of γ phase are attributed to the increase of Pd occupancy in the OH sublattice.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Developing of nano sized fibrous eutectic silicon in hypereutectic Al–Si alloy by laser remelting

Laser surface melting followed by rapid solidification is an effective means to produce very fine microstructures with desirable surface properties because of the high rates of cooling associated with it. In the present study, the effect of rapid cooling on the silicon particle size, distribution, and morphology of hypereutectic Al–17wt.%Si and Al–20wt.%Si alloys have been investigated. A continuous-wave CO2 laser of wavelength 10.6 μm and a Trumpf Yb-YAG disk laser of wavelength 1.030 μm were used with a beam diameter of 1 mm and scanning speeds ranging from 5 to 100 mm/s. Rapid solidification increased the solubility of silicon in aluminum to approximately 5wt% and induced non-equilibrium hypoeutectic microstructures comprising large volume fractions of primary α-Al dendrites and ultrafine Al–Si eutectic of lamellar morphology. Both α-Al dendrites and the silicon particle sizes were significantly reduced from micron to nanoscale level. The morphology of silicon particles is modified from massive polygonal and plate-like to a mixture of fine fakes with round corners, feathery and fibrous, or a coral-like and thread-like structure. The eutectic silicon size and the interlamellar spacing were reduced to 30 and 10 nm, respectively. Furthermore, most of the silicon crystals in the eutectic region and the aluminum dendrites contained a significant number of twins which were considered as an essential contributor to the mechanism of growth and branching. Microhardness values increased two to threefold due to the refinement of the microstructural constituent.

42 ENGINEERING↗
DOE OSTI2022

A laser powder bed fusion system for operando synchrotron x-ray imaging and correlative diagnostic experiments at the Stanford Synchrotron Radiation Lightsource

Laser powder bed fusion (LPBF) is a highly dynamic multi-physics process used for the additive manufacturing (AM) of metal components. Improving process understanding and validating predictive computational models require high-fidelity diagnostics capable of capturing data in challenging environments. Synchrotron x-ray techniques play a vital role in the validation process as they are the only in situ diagnostic capable of imaging sub-surface melt pool dynamics and microstructure evolution during LPBF-AM. In this article, a laboratory scale system designed to mimic LPBF process conditions while operating at a synchrotron facility is described. The system is implemented with process accurate atmospheric conditions, including an air knife for active vapor plume removal. Significantly, the chamber also incorporates a diagnostic sensor suite that monitors emitted optical, acoustic, and electronic signals during laser processing with coincident x-ray imaging. The addition of the sensor suite enables validation of these industrially compatible single point sensors by detecting pore formation and spatter events and directly correlating the events with changes in the detected signal. Experiments in the Ti–6Al–4V alloy performed at the Stanford Synchrotron Radiation Lightsource using the system are detailed with sufficient sampling rates to probe melt pool dynamics. X-ray imaging captures melt pool dynamics at frame rates of 20 kHz with a 2 µm pixel resolution, and the coincident diagnostic sensor data are recorded at 470 kHz. Furthermore, this work shows that the current system enables the in situ detection of defects during the LPBF process and permits direct correlation of diagnostic signatures at the exact time of defect formation.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Optimal Geometry for Focused Ion Beam-Milled Samples for Direct-Pull Micro-Tensile Testing Performed In Situ in a Scanning Electron Microscope

A thorough procedure was developed to efficiently manufacture dogbone samples using focused ion beam (FIB) milling for micro-tensile testing. A Bruker PI 89 PicoIndenter, Billerica, MA, USA, was used as a case study, although the analysis and results are applicable to other micro-mechanical testing systems capable of mounting a standard, Ø12.7 mm × Ø3.2 mm pin, scanning electron microscopy (SEM) pin stub (Ted Pella, Redding, CA, USA). Nine dogbones were made from an Fe-45Cu alloy additively manufactured using powder-fed laser-directed energy deposition (DED-LB). Testing showed that fracture was confined to the gauge section for all dogbones and that the fracture mode, ductile vs. brittle, was entirely dependent on the grain orientation relative to the loading direction. The analysis showed that the measured plastic strain to failure can vary from >11% (optimal geometry) to <1% (non-optimal geometry) in micro-tensile testing of high-tensile-strength (>1 GPa) metallic materials. Subsequently, a finite element analysis (FEA) was conducted to identify the improved dogbone geometries. A total of ten thousand dogbone geometries were tested, and their dimensions were defined by a set of four adjustable parameters (corner radius, load surface angle, load surface length, and dogbone head length). The gauge width and gauge length were fixed to 4 µm and 10 µm, respectively. Three-dimensional surface plots of the stress concentration as a function of two parameters were used to identify the optimal ranges of parameter values. The addition of maximum width and length constraints, measuring 25 µm and 30 µm, respectively, allowed us to identify an optimal geometry at load surface angles of 30° and 45°. Their respective dimensions (corner radius, load surface length, and dogbone head length) are, in µm, 12, 6, and 7 and 10, 7, and 7. Testing these two optimal geometries with a range of gauge lengths from 4 to 20 µm showed that smaller gauge lengths only slightly reduced the detrimental stress concentration outside the gauge section. However, smaller gauge lengths will notably improve the FIB surface polishing step as tapering is reduced with smaller dogbone lengths.

Chemistry↗
DOE OSTI2022

Synergistic effect of microstructure and defects on the initiation of fatigue cracks in additively manufactured Inconel 718

Fatigue cracks in additively manufactured (AMed) Inconel 718 (IN-718) in machined surface condition often initiate from persistent slip bands (PSBs) unlike other popular AM alloys such as 17-4 PH stainless steel or Ti-6Al-4V, where fatigue crack initiation is exclusively from volumetric defects; therefore, a competition between PSB- vs. defect- mediated crack initiation clearly exists. To shed light on the factors governing the competition, this study investigates the characteristics of cyclic strain localization, PSB formation, and crack initiation via crystal plasticity (CP) modeling of cyclic loading on polycrystalline aggregates which are then validated by experiments. In this work, a physics-based, free slip distance (FSD) dependent slip strength evolution law is proposed, which is shown to enable the CP model to simulate the heterogeneous strain distribution in IN-718. Implementing a crack initiation criterion based on strain contrast, the locations and lives for crack initiation can also be calculated. It is shown that both FSD and resolve shear stress influence the strain localization and crack initiation behaviors. The distribution of a localization parameter calculated based on the multiplication of FSD and Schmid factor within a grain is found to correlate well with the locations of PSBs. The maximum values of the localization parameters within a microstructure are shown to correlate well with the experimentally obtained crack initiation lives. The presence of volumetric defects in IN-718 generally do not impact strain localization behavior unless their size is large compared to the grain size.

42 ENGINEERING↗
DOE OSTI2024

Microstructure analysis and machinability of additively manufactured A205 aluminum with heat treatments

A205 aluminum is one of the few high-strength aluminum alloys discovered for additive manufacturing (AM). The microstructure and heat treatment effects of AM A205 vary from those of its cast form, indicating possible differences in machinability during post-processing. Here, the objective of this research is to determine these variations of AM A205 and their effects on machinability using the cast condition as the baseline. As built and two heat-treated conditions (solution treatment and age hardening) were applied and compared in terms of their microstructures, micro-hardness, and machinability including vibration, specific cutting energy, chip morphology, and surface finish. The effects of print orientations on machinability were tested as well and found to be insignificant. AM as built had a higher hardness and slightly better machinability than its cast as built cast counterpart due to a smaller grain size (1 µm vs. 15 µm), eutectic θ-Al 2 Cu lattice and a fine, homogeneous TiB 2 distribution. The solution treatment dissolved this θ-Al 2 Cu lattice and increased the grain size (3 µm) which decreased the hardness, increased the ductility seen in the chips, and reduced the overall machinability. The presence of θ’-Al 2 Cu precipitates improved the machinability of aged AM A205. In addition, it was found that A205 exhibited both ductile and brittle behavior depending on the cutting speed, thus producing different machinability. The speed dependency is related to the material condition and heat treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Gas nitriding behavior of refractory metals and implications for multi-principal element alloy design

Multi-principal element alloys (MPEAs) comprise a large, flexible compositional space that enables tuning of their chemistry, structure, and properties. Here, to facilitate the development of nitriding-based surface-enhancement strategies that harness a broad compositional space, this study examined the gas nitriding behavior of Hf, Mo, Nb, Ta, Ti, and Zr as a function of time, temperature (750 and 1000 °C), and nitriding potential (i.e. ammonia-to-hydrogen ratio). These metals were selected because they have a strong driving force to form nitrides, and appear in many promising refractory MPEA compositions. The nitriding temperatures were selected based on the phase transformation temperature of Ti and Zr, and the nitriding potentials were chosen such that all elements are expected to form nitrides. Mass gain measurements indicate that all six elements follow parabolic kinetics. The microstructure observations and quantitative microchemical analysis show formation of dense and well-adhered compound layers for Mo, Nb, and Ta. Thick diffusion zones appear in Hf, Ta, Ti, and Zr, and diffusion coefficients were fit to the composition profiles. Partial delamination of the compound layer occurred for Ti and Zr. Peak hardness values above 30 GPa are obtained in the dense compound layers, and the solute hardening of the underlying alloy is correlated with the nitrogen content. The results provide insight into the dynamics of nitride compound formation relative to interstitial dissolution of nitrogen, and are discussed in the context of MPEA composition and processing design.

36 MATERIALS SCIENCE↗
DOE OSTI2021

H 2 O-assisted O 2 reduction by H 2 on Pt and PtAu bimetallic nanoparticles: Influences of composition and reactant coverages on kinetic regimes, rates, and selectivities

Hydrogen peroxide (H 2 O 2 ) can replace hazardous oxidants in industrial processes but is currently too expensive for many such applications. While direct synthesis of H 2 O 2 (H 2 + O 2 → H 2 O 2 ) may reduce costs in comparison to incumbent technology, current catalysts lack the requisite stability and selectivity. Here, we examine the direct synthesis of H 2 O 2 on bimetallic Pt 1 Au x (0 ≤ x ≤ 230) and Pt catalysts at steady-state in pure water and relate kinetic parameters for H 2 O 2 and H 2 O formation to possible active site structures informed by complementary characterization methods. X-ray photoelectron spectra show significant Pt surface enrichment compared to the bulk composition. Analysis of infrared spectra of mixed monolayers of 12 CO* and 13 CO* indicate that Pt and Au form substitutional surface alloys. The Pt 1 Au x nanoparticles with the greatest mole fractions of Au predominantly expose Pt monomers (i.e., isolated Pt atoms), yet Pt atoms exposed upon all these nanoparticles possess electronic structures distinct from bulk Pt. Despite these differences, rate measurements are consistent with product formation through proton-electron transfer pathways for all Pt 1 Au x catalysts. In situ XAS indicate that Pt remains metallic during H 2 O 2 synthesis. Under the most oxidizing conditions, selectivities toward H 2 O 2 increase strongly with the Au to Pt ratio from 2% for monometallic Pt to 85% for Pt 1 Au 170 . However, selectivities are similar among all catalysts within reducing conditions. Comparisons of apparent activation enthalpies for the formation of H 2 O 2 and H 2 O across these catalysts and the range of conditions suggest that Pt monomers within Au provide the greatest selectivities for H 2 O 2 formation, because these active sites present high barriers for O-O bond rupture. Further, selectivities decrease with increasing ratios of H 2 to O 2 pressures, because Pt atoms aggregate and form oligomers that readily dissociate dioxygen intermediates. The combined use of spectroscopy, kinetics, and concepts employed in reaching these conclusions take inspiration from the legacy of Prof. Michel Boudart, and specifically his elegant methods for interrogating bimetallic catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

The performance of additively manufactured Haynes 282 in supercritical CO 2

The use of supercritical carbon dioxide (sCO 2 ) as a working fluid is garnering interest in next generation power production systems due to the possibility of increased operational efficiencies and lower associated costs. Its implementation requires alloys with excellent high temperature strength and corrosion resistance, which makes Haynes 282® (H282) a suitable candidate. With increasing adoption of additive manufacturing (AM) in the energy industry, there is a need to investigate long-term sCO2 exposure on AM produced materials. Additively manufactured H282 (AM-H282) samples built using laser powder bed fusion in two different orientations were analyzed through imaging, gravimetric analysis, and room-temperature tensile testing before and after 1000-h exposure to CO 2 at 750 °C and 20 MPa. Performed imaging included observation of the sample surfaces and of the material bulk (cross sections) through means of Scanning Electron Microscopy (SEM) and optical microscopy. In comparison to wrought H282, it was found that the exposed material exhibited a similar Cr 2 O 3 oxide protective layer about 2 μm in thickness with additional top-surface TiO 2 oxide and carbon-rich precipitates. It was also similarly observed that internal oxidation was present but limited to a depth of 20 μm, and a 1–3 μm γ’ denuded region appeared to surround all internal and surface oxidation. Thermal aging effects were noted with the precipitation of needle-like structures in the γ/γ’ matrix and a coarsening of the γ’ precipitates from 28 nm to 73 nm. Mass measurements analyzing oxide precipitation revealed a larger increase compared to wrought, representing an approximate 20% difference. Tensile testing results showed similar behavior to wrought with a slight increase in yield strength and a large reduction in elongation in the exposed samples.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Surface Energy Modulated Self‐Assembly of Percolative Gallium Nanodroplet Films for Stretchable Electronics

Advancements in soft robotics and wearable technologies have led to an increased need for flexible and stretchable electronic systems. Liquid metals like Gallium (Ga) and its alloys offer high potential in the field of stretchable electronics and photonics due to their inherent high conductivity and malleability. However, their high surface tension and native oxide formation hinder uniform wetting and continuous film formation to get conducting films. Here, we report a fabrication strategy to realize electrically conductive Ga thin films with effective thicknesses around 100 nm on polymeric and elastomeric substrates. By enhancing the surface energy of the elastomer, we create uniform Ga nanodroplets capable of sustaining stretchability up to 200% strain. Our devices exhibit electronic conduction primarily through tunneling and display strain tunable piezoresistive characteristics, which are explained using Kirchhoff's resistive network and Simmon's analytical tunneling current model. To showcase the device's capability in fields of stretchable electronics, we demonstrate several functional prototypes, including flexible devices integrated with Light Emitting Diodes (LEDs), curvature and pressure sensors, and soft robotic grippers capable of sensing object curvature. The demonstrated devices highlight the potential of this approach for scalable integration of stretchable electronics in soft robotic and wearable platforms.

42 ENGINEERING↗
DOE OSTI2024

High-Throughput Microstructural Characterization and Process Correlation Using Automated Electron Backscatter Diffraction

The need to optimize the processing conditions of additively manufactured (AM) metals and alloys has driven advances in throughput capabilities for material property measurements such as tensile strength or hardness. High-throughput (HT) characterization of AM metal microstructure has fallen significantly behind the pace of property measurements due to intrinsic bottlenecks associated with the artisan and labor-intensive preparation methods required to produce highly polished surfaces. This inequality in data throughput has led to a reliance on heuristics to connect process to structure or structure to properties for AM structural materials. In this study, we show a transformative approach to achieve laser powder bed fusion (LPBF) printing, HT preparation using dry electropolishing and HT electron backscatter diffraction (EBSD). This approach was used to construct a library of > 600 experimental EBSD sample sets spanning a diverse range of LPBF process conditions for AM Kovar. This vast library is far more expansive in parameter space than most state-of-the-art studies, yet it required only approximately 10 labor hours to acquire. Build geometries, surface preparation methods, and microscopy details, as well as the entire library of >600 EBSD data sets over the two sample design versions, have been shared with intent for the materials community to leverage the data and further advance the approach. Using this library, we investigated process–structure relationships and uncovered an unexpected, strong dependence of microstructure on location within the build, when varied, using otherwise identical laser parameters.

Characterization and Analytical Technique↗
DOE OSTI2020

Dendrite-free Al recycling via electrodeposition using ionic liquid electrolytes: The effects of deposition temperature and cathode surface roughness

In this report, the electrodeposition of Al from aluminum scrap alloys (A2020) on copper cathode substrates with varied surface roughness under different deposition temperatures was studied using low-temperature AlCl 3 -1-butyl-3-methyl-imidazolium chloride (BMIC) ionic liquid electrolytes. The bulk electrodeposition of Al was carried out under a voltage of 1.5 V at a stirring rate of 120 rpm using a fixed ionic liquid electrolyte concentration (molar ratio AlCl 3 : BMIC = 2:1). The effects of deposition temperature (range from 80 °C to 140 °C) and surface roughness of Cu cathode substrates (polished by 320, 600, 800, 1200 grits SiC sandpapers and mirror polishing process) on the morphology of deposited Al, current density, current efficiency and energy consumption, were investigated. The Al deposits were characterized using scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), profilometer, and electrochemical measurements for current density, current efficiency, and energy consumption. It is demonstrated that the deposition temperature and surface roughness of Cu electrodes play a critical role in the nucleation and growth of Al deposits. Higher deposition temperature promotes the diffusion and/or migration of Al 2 Cl 7 - ions and then enhances the current density and efficiency during the electrodeposition of Al. Smoother surface of Cu electrodes is preferred for the formation of dendrite-free Al deposits. Typically, on the mirror polished Cu electrode, no Al dendrite structure was observed, and only plate-like Al deposits were formed at the deposition temperature of 100 °C. Pure metallic Al was successfully deposited on Cu electrodes in AlCl 3 + BMIC ionic liquid electrolytes for all experiments with a current efficiency range from 72% to 99% and energy consumption of 4.6–6.3 kW h/kg Al.

54 ENVIRONMENTAL SCIENCES↗