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At least 397 records · Page 22

Laser‐Powder Melt Pool Solidification Dynamics and Microstructural Engineering of Ti‐5553 Microlattices

The fine geometric and topological control afforded by additive manufacturing technologies has enabled the manufacture of architected materials across length scales, and enabling tunable mechanical performance as a function of local and global design. Progress has been made to tune the mechanical response of architected materials through geometry, but understanding how the geometry and processing conditions will inform the microstructure remains a challenge due to the rapid solidification in laser powder bed fusion. This study uses in situ X-ray imaging and electron backscatter diffraction microscopy to demonstrate that the melt pool size, microstructure morphology, and elastic strain distribution is influenced by a combination of lattice geometry and laser processing conditions. These results indicate that within larger melt pools the local thermal gradients are sufficient to enable a columnar-to-equiaxed transition across the melt pool. Furthermore, the solidification mechanisms producing these microstructures are examined across the first 5 ms of melting and solidification, described via in situ high-speed X-ray imaging and mirrored via multiphysics simulation.

additive manufacturing↗

High-pressure high-temperature melting and recrystallization of nanolamellar high-entropy alloys

Additively manufactured (AM) High Entropy Alloys (HEAs) are notable for their exceptional high-yield strength and large tensile ductility. The nanolamellar Eutectic HEA (EHEA) AlCoCrFeNi 2.1 was fabricated by laser powder bed fusion (L-PBF) in the as-printed form (EHEA1) and subsequently annealed at 1000oC (EHEA2) and 600oC (EHEA3) to achieve a broad range of mechanical properties. EHEA2 and EHEA3 samples were studied using Scanning transmission electron microscopy (STEM), energy dispersive X-ray diffraction (EDXRD) at high-pressures and high temperatures, nanoindentation hardness and modulus measurements. According to EDXRD EHEA2 and EHEA3 are composed of B2 and L1 2 phases. High-pressure high-temperature EDXRD studies show melting for EHEA2 at 1698 ± 25 K at a pressure of 6.5 GPa and melting for EHEA3 at 1598 ± 25 K at a pressure of 5.8 GPa. Post-melt and recrystallized samples were recovered at ambient conditions, and XRD analysis showed retention of B2 and L1 2 phases, although a new σ phase appeared for both EHEA2 and EHEA3 samples due to high-pressure and high-temperature melting and recrystallization experiment. SEM analysis also demonstrated the preservation of the nanolamellar morphology. Nanoindentation studies revealed that recrystallized EHEAs retain their original mechanical property hierarchy, with EHEA3 being 47% harder than EHEA2, largely related to higher content of B2-phase and retention of nanolamellar morphology. We also present Pressure-Volume-Temperature (P-V-T) data for 3-D printed and annealed eutectic high entropy alloys and extract mechanical and thermal properties data.

36 MATERIALS SCIENCE↗

Advanced Functional Membranes for Noble Gas Management: Fabrication and Testing of Membranes on Porous Support

We selected several porous materials including PNW-24, CC3, SAPO-34, SAPO-56 and PNW-6, as the basis for fabricating membranes for Kr/Xe separation. Initially, we synthesized powder samples of the candidates and confirmed their crystallinity and morphology with X-ray diffraction and microscopy. In the case of PNW-24 and PNW-6, we further confirmed its Xe selectivity through Xe and Kr adsorption experiments, while we relied on literature reports for CC3, SAPO-34 and SAPO-56. We subsequently proceeded to fabricate membranes on porous alumina supports using techniques such as seeded-assisted secondary growth, in-situ growth and solution-processed method. PXRD on the membranes verified that the structures were well-grown on the surface of alumina support, while SEM provided visual confirmation of particle morphology. Importantly, defects were not visually observed in the fabricated membranes, which was further verified with pressure retention tests. We analyzed the separation performance of the synthesized membranes using a dilute gas mixture comprising of xenon, krypton and argon. We focused on PNW-6 to optimize the synthesis reaction time and study the effects of time on gas separation. While more research is necessary to reach a comprehensive conclusion, in alignment with our milestones, we have successfully achieved our goals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Mechanical and Tribological Performance of Additively Manufactured Nanocrystalline Aluminum via Cryomilling and Cold Spray

In this study, nanocrystalline (NC) aluminum (Al) and magnesium (Mg)-doped Al bulk components were fabricated using a hybrid manufacturing process that combines cryomilling and high-pressure cold spray (HPCS) additive deposition techniques. Yttria-stabilized zirconia (YSZ) was also added during the HPCS process to improve deposition efficiency and build-up thickness via peening. The evolution of morphology, crystallite size, and elemental composition of both cryomilled powders and cold-sprayed (CS’ed) components was systematically characterized using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). Mechanical characterization was performed using Vickers microhardness and uniaxial tensile testing, while the tribological behavior was assessed using sliding wear tests under dry/lubricated conditions. XRD analysis revealed that increased cryomilling duration led to significant crystallite refinement, which directly correlated with enhanced hardness and strength. This mechanical strengthening was accompanied by an increase in coefficient of friction (COF) and lower wear rates. The results also showed that the Mg-doped Al exhibited superior hardness, tensile strength, and tribological performance compared to pure Al. The study further explores the underlying mechanisms responsible for these enhancements, highlighting the potential of solute-assisted grain boundary stabilization in tailoring high-performance NC Al alloys.

36 MATERIALS SCIENCE↗

Residual strain and microstructure evolution in 316L stainless steel fabricated by hybrid additive/subtractive manufacturing

The extreme thermal gradients in additive manufacturing (AM) result in residual strains. Subsequent machining operations can relieve the AM strains but can introduce additional strains. AM and machining on the same platform, also called interleaving, during hybrid manufacturing has been shown to improve productivity. However, the impacts of these operations on the resulting residual strains are not well understood. In this investigation, neutron diffraction was used to measure residual strains in hybrid manufactured 316L stainless steel where blown-powder laser directed energy deposition (DED), and machining operations were interleaved in 1-inch intervals. We observe that the dominant texture developed during AM, resulting from different spot sizes and deposition parameters, significantly affects residual strain evolution. A dominant <011> texture along the build direction does not show any strain localization during interleaved deposition and machining whereas a dominant <001> texture shows strong tensile strain localization consistent with the pauses for machining at the end of AM step. Using coolant during machining can further alter the residual strain evolution. Our work shows that a combination of AM parameters and machining strategy can be used to influence the nature and magnitude of residual strains in components fabricated using convergent manufacturing technologies.

Hybrid manufacturing↗

Synthesis and thermal evolution of structure in alkoxide-derived niobium pentoxide gels

Niobium pentoxide gels in the form of transparent monoliths and powder have been synthesized from the controlled hydrolysis and polycondensation of niobium pentaethoxide under different experimental conditions using various mole ratios of Nb(OC2H5)5:H2O:C2H5OH:HCl. Alcohol acted as the mutual solvent and HCl as the deflocculating agent. In the absence of HCl, precipitation of colloidal particles was encountered on the addition of any water to the alkoxide. The gels were subjected to various thermal treatments and characterized by differential thermal analysis, thermogravimetric analysis, x-ray diffraction, and infrared spectroscopy. After drying at 400 C, the gels were amorphous to x-rays. The amorphous powder crystallized into the low-temperature orthorhombic form of Nb2O5 at approximately 500 C, which transformed irreversibly into the high-temperature monoclinic alpha-Nb2O5 between 900 to 1000 C. The kinetics of crystallization of the amorphous niobium pentoxide have been investigated by non-isothermal differential scanning calorimetry. The crystallization activation energy was determined to be 399 kJ/mol.

Bansal, Narottam P.↗

Elucidating texture and grain morphology contributions to the micromechanical response of additively manufactured Inconel 625

Microstructural variation of additively manufactured (AM) metal components in comparison to wrought counterparts makes certification for critical applications a challenge. Microscale simulations leveraging modern computational tools may be used to supplement testing of AM microstructures, thus accelerating certification by reducing the number of experiments needed. However, as micromechanical response is closely tied to critical properties like fatigue-life and fracture, utilization of these simulations with macroscale experimental data alone is insufficient. One means to attain microscale experimental data is in situ diffraction data collected from synchrotron X-ray sources. In this work, such data were collected during in situ compression of AM Inconel 625 superalloy. Interpretation of experimental results was assisted by massive (8M element) complementary micromechanical simulations performed on sets of virtual microstructures generated using cellular automata. Together, micromechanical data from diffraction experiments and simulations were used to probe the effects of textured “track” microstructures generated during laser powder bed fusion and directional strength-to-stiffness on micromechanical response. Though fiber-averaged directional strength-to-stiffness ratios were expected to dominate given the high elastic anisotropy of the material, the combination of small variations in texture and specific grain configurations unique to AM microstructures lead to significant variability in micromechanical response after yield. The findings emphasize the importance of high-fidelity microstructural representation that captures key texture components and AM-specific morphology for property prediction of AM metals.

36 MATERIALS SCIENCE↗

The First X-ray Diffraction Patterns of Clay Minerals from Gale Crater

The Mars Science Laboratory (MSL) Rover, Curiosity spent approx 150 sols at Yellowknife Bay (YKB) studying a section of fluvio-lacustrine sedimentary rocks (with potential indications of volcanic influence), informally known as the Yellowknife Bay formation. YKB lies in a distal region of the Peace Vallis alluvial fan, which extends from the northern rim of Gale Crater toward the dune field at the base of Mt Sharp. Sedimentological and stratigraphic observations are consistent with the Yellowknife Bay formation being part of a distal fan deposit, which could be as young as middle Hesperian to even early Amazonian in age (approx 3.5 to 2.5 Ga). The Yellowknife Bay formation hosts a unit of mudstone called the Sheepbed member. Curiosity obtained powdered rock samples from two drill holes in the Sheepbed Member, named John Klein and Cumberland, and delivered them to instruments in Curiosity. Data from CheMin, a combined X-ray diffraction (XRD)/X-ray fluorescence instrument (XRF), has allowed detailed mineralogical analysis of mudstone powders revealing a clay mineral component of approx 20 wt.% in each sample. The clay minerals are important indicators of paleoenvironmental conditions and sensitive recorders of post-depositional alteration processes. The XRD pattern of John Klein reveals a 021 band consistent with a trioctahedral phyllosilicate. A broad peak at approx 10A with a slight inflexion at approx 12A indicates the presence of 2:1 type clay minerals in the John Klein sample. The trioctahedral nature of the clay minerals, breadth of the basal reflection, and presence of a minor component with larger basal spacing suggests that John Klein contains a trioctahedral smectite (probably saponite), whose interlayer is largely collapsed because of the low-humidity conditions. The XRD patterns show no evidence of corrensite (mixed-layer chlorite/smectite) or chlorite, which are typical diagenetic products of trioctahedral smectites when subjected to burial and heating >60degC in the presence of water. Given estimated geothermal gradients on Mars temperatures <60 degC might still be consistent with (but do not require) moderate burial. However, our ability to identify interstratified minerals is greatly limited by the lack of access to traditional treatments methods used in the lab (e.g., ethylene glycol solvation). Our preferred explanation for the origin of trioctahedral smectites in Sheepbed mudstone is in situ production via reaction of olivine, water and Si-bearing amorphous material, an important mudstone component detected by XRD. Elevated levels of magnetite in the Sheepbed and the trioctahedral monomineralic nature of the clay minerals support this model. These observations, combined with previous studies of olivine stability, support the persistence of circum-neutral hydrous conditions for thousands of years at YKB.

Bristow, Thomas↗

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

Additive Manufacturing of Oxide Dispersion Strengthened Multi Principle Element Alloys for Future Aerospace Applications

Oxide Dispersion Strengthened (ODS) materials have long been of interest for their high temperature applications, and additive manufacturing enables their manufacturing viability. The ODS multi-principle element alloy NiCoCr was prepared using powder metallurgy techniques, additively manufactured, and evaluated for its processingmicrostructure-property relationships. The high temperature foundations of nickel-base superalloys and ODS materials were combined with the manufacturing advantages of 3D printing and the chemical simplicity of NiCoCr to inspire this work, which was divided into powder and printed material assessments. The project was achieved through multiple iterative project loops to assess the processing parameters’ impact on the microstructure and mechanical properties of the feedstock powder and printed material. The powder investigations (Chapter 3) focused on understanding the oxide coating that formed on the metal powder following acoustic mixing. Time of Flight Secondary Ion Mass Spectrometry was used to semi-quantitatively assess the amount of yttrium on the surface of the mixed powders, and indicated that a combination of higher mixing condition energy and moderate mixing time resulted in the most oxide coating on the NiCoCr powder. The results were supported by a qualitative assessment of scanning electron images of coated powder particles. Following mixing, the ODS NiCoCr was consolidated by Laser Powder Bed Fusion. The evaluations of the printed material (Chapter 4) frst considered screening experiments including Archimedes’ density, porosity, and grain size and number metrics from electron backscatter diffraction data. After the ideal additive manufacturing parameters were identifed, both the oxide homogeneity and yield strength were discussed for the idealized printed material. Overall, the project suggests that the combined use of qualitative or semi-quantitative powder surface analysis with Archimedes’ density analyses can be a valid high-throughput technique which can lead to process optimization of Laser Powder Bed Fusion additively manufactured ODS material.

Laura G Wilson↗

Diffraction Measurement of Reaction Products in Shock Compressed TATB on the NIF

The shock-induced reaction of high explosives to gaseous and solid reaction products is a rapid, complex process. Understanding solid reaction product structure and formation kinetics is essential in determining the high-pressure equation of state of these multicomponent systems. We use the National Ignition Facility (NIF) to shock compress ~500-µm thick pressed powder high-explosive TATB samples to 70-135 GPa and collect in situ structural data on detonation byproducts using the TARDIS X-ray diffraction diagnostic. Velocimetry is used to record the transmitted compression wave profile, which is well described by Cheetah hydrocode simulations coupled with a reactive flow model, providing strong evidence of reaction in the TATB sample. While an unambiguous determination of the product phases was not possible owing to the low signal-to-noise quality of the diffraction signal, X-ray diffraction data of the product phases formed within the first 50 ns of the reaction is most consistent with a mixture of amorphous products and crystalline hexagonal diamond.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Smart manufacturing approach to manufacture bulk nanocrystalline aluminum for lightweight applications

In this research, a smart manufacturing approach was used to enhance the mechanical properties of aluminum (Al) for lightweight applications. The smart manufacturing involved cryomilling of Al powders with and without 5 wt.% magnesium (Mg) powders for varying durations followed by a high-pressure cold spray (HPCS) additive manufacturing process to prepare bulk components. The morphological changes, crystallite size, and composition of the cryomilled powders and cold sprayed (CS’ed) components were examined using scanning electron microscopy (SEM), x-ray diffraction (XRD), and transmission electron microscopy (TEM) techniques. The results showed that the crystallite size reduces with an increase in cryomilling time and the addition of Mg dopant. To test the mechanical properties of the bulk CS’ed components, microhardness tests were performed using a Vickers microhardness tester. Uniaxial tensile tests were also carried out to ascertain the material’s tensile properties. The mechanical testing results showed great improvement in the hardness and tensile strength of CS’ed Al–Mg samples as compared to pure Al samples. Subsequently, fractography analysis of the tensile failed samples was carried out to determine the nature of the failure. Here, the research article also discusses the inherent mechanisms for the improvement in mechanical properties of smart manufactured components as a result of Mg doping and cryomilling.

36 MATERIALS SCIENCE↗

Microstructural and Mechanical Characterization of a Dispersion Strengthened Medium Entropy Alloy Produced Using Selective Laser Melting

High entropy alloys (HEAs) are an interesting new class of alloys which have been shown to exhibit both notable strength and ductility for a wide range of temperature and stresses. In addition, the remarkably small difference between the solvus and liquidus temperatures for many face centered cubic HEAs makes them an excellent candidate for selective laser melting fabrication. In this study, the microstructure and mechanical properties of a dispersion strengthened equiatomic NiCoCr alloy successfully produced using selective laser melting are explored. The effect laser speed, laser power, and powder recyclability have on final part density and microstructural segregation are analyzed through both x-ray diffraction and high resolution scanning electron microscopy. These results are further validated and compared to stable phase predictions produced using a commercially available high entropy alloy mobility database. Lastly, the tensile strengths resulting from different heat treatment pathways are detailed.

Smith, T. M.↗

Experimental and computational studies on high-entropy carbide MoNbTaVWC 5 under high pressures

High-entropy carbide, MoNbTaVWC 5 , was synthesized from oxide precursors of the constituent metals, mixed with graphite powder in a microwave-generated hydrogen plasma at 26.66 kPa and 2100 °C. Ambient x-ray diffraction analysis confirms the full conversion of oxide precursors into a single-phase, face-centered cubic structure with a lattice parameter a = 4.3309 Å. Nanoindentation measured a hardness of 24.5 ± 1.3 GPa and an elastic modulus of 386 ± 22 GPa. The synthesized sample, mixed with a copper pressure marker, was studied by the radial x-ray diffraction technique with beryllium gasketing in a diamond anvil cell up to 70 GPa. The experimentally measured pressure–volume curve and shear strength were compared with theoretical predictions using the special quasi-random structure technique and density functional theory. MoNbTaVWC 5 achieved a 12% volume compression at 70 GPa and exhibited a high shear strength of 6.6 GPa. The present study demonstrates that the high-entropy carbide MoNbTaVWC 5 exhibits exceptional incompressibility and high strength under extreme conditions.

36 MATERIALS SCIENCE↗

Fast and Accurate Pixel Calibration of Tof Neutron Diffractometers with Machine Learning

At a spallation neutron source, neutron pulses of varying energies are generated, and the detection of neutrons by instrument detectors is recorded as time-of-flight from the emission of the neutron pulse to its arrival at specific detector pixels with high time resolution. The flight path of neutrons from the moderator to the sample and then to the detector must be precisely calibrated at the detector-pixel level using standard powders, so the neutron events from all pixels can be time-focused to produce high-resolution diffraction patterns. Modern time-of-flight neutron diffractometers at spallation neutron sources are equipped with two-dimensional detectors with millimeter-scale pixelations. The number of pixels in a diffraction instrument can reach millions, which makes a single-pixel-level calibration process time-consuming or even impossible with conventional refinement or fitting approaches. Here we present a machine-learning-aided calibration process using a train-and-predict approach, in which machine learning models are trained on the relationship between an individual pixel time-of-flight diffraction pattern and its diffraction constant. These models use a portion of the available pixels for training, and a good model then predicts the diffraction constants precisely and rapidly for large sets of pixel diffraction patterns.

detector pixel calibration↗

The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50μm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

CheMin↗

Crystal Growth of Quaternary Rare Earth Selenosilicates by Using the Flux-Assisted Boron Chalcogen Mixture Method: Investigation of Their Magnetic and Optical Properties

A series of rare earth magnesium selenosilicates, RE3Mg 0.5 SiSe 7 (RE = Ce, Pr, Nd, Sm, Gd, Tb, Dy) were obtained as single crystal using the flux assisted boron chalcogen mixture (BCM) method. The structures of the crystals were determined by single-crystal X-ray diffraction. The RE3Mg 0.5 SiSe 7 series crystallizes in the hexagonal crystal system in the space group P6 3 . Polycrystalline powders were synthesized to perform physical property measurements. Magnetic measurements over the 2–300 K temperature range reveal that Ce 3 Mg 0.5 SiSe 7 and Gd 3 Mg 0.5 SiSe 7 exhibit paramagnetic behavior with negative Weiss constants (θ W = −14.50, θ W = −6.13 K, respectively). The optical properties of RE 3 Mg 0.5 SiSe 7 (RE = Ce, Pr, Nd, Sm, Gd) were measured by ultraviolet–visible (UV–vis) diffuse reflectance. Density functional theory (DFT) electronic structure calculations were performed. Furthermore, a second harmonic generation measurement was performed on a polycrystalline powder of Ce 3 Mg 0.5 SiSe 7 and was found to be SHG active with an efficiency of 0.11 times the standard potassium dihydrogen phosphate (KDP).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Protonic Conduction of BaCe0.85YO. 1503 Doped with SrTiO3

Reformers based on ceramic membrane technology potentially offer hydrogen production that is comparable to the cost of fossil fuels. Protonic conducting ceramic with the chemical formula AB03 offers the promise of highly selective hydrogen separation at intermediate temperature (400-800 C). Among different perovskite-type oxides, BaCe03 and SrCe03 based compositions show high protonic conductivities but strong resistance to densification. X-ray diffraction studies on sintered specimens of BaCe0.85Y0.1503-6 show multi-phase formation which was found to show dependence upon powder synthesis method. Doping with SrTiO3 suppresses multi-phase formation and enhances grain growth. Conductivity measurements in temperature range of 200 to 1000 C were performed by ac impedance spectroscopy under dry and wet conditions. Sintering behavior, phase formation and conductivity results will be reported.

Dynys, Frederick W.↗