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At least 1,099 records · Page 61

Study of Material Densification of In718 in the Higher Throughput Parameter Regime

Selective Laser Melting (SLM) is a powder bed fusion additive manufacturing process used increasingly in the aerospace industry to reduce the cost, weight, and fabrication time for complex propulsion components. Previous optimization studies for SLM using the Concept Laser M1 and M2 machines at NASA Marshall Space Flight Center have centered on machine default parameters. The objective of this project is to characterize how heat treatment affects density and porosity from a microscopic point of view. This is performs using higher throughput parameters (a previously unexplored region of the manufacturing operating envelope for this application) on material consolidation. Density blocks were analyzed to explore the relationship between build parameters (laser power, scan speed, and hatch spacing) and material consolidation (assessed in terms of density and porosity). The study also considers the impact of post-processing, specifically hot isostatic pressing and heat treatment, as well as deposition pattern on material consolidation in the higher energy parameter regime. Metallurgical evaluation of specimens will also be presented. This work will contribute to creating a knowledge base (understanding material behavior in all ranges of the AM equipment operating envelope) that is critical to transitioning AM from the custom low rate production sphere it currently occupies to the world of mass high rate production, where parts are fabricated at a rapid rate with confidence that they will meet or exceed all stringent functional requirements for spaceflight hardware. These studies will also provide important data on the sensitivity of material consolidation to process parameters that will inform the design and development of future flight articles using SLM.

Cordner, Samuel↗

Synthesis of platinum single-site centers through metal-ligand self-assembly on powdered metal oxide supports

Developing single-site metal catalysts has been regarded as a promising strategy to improve activity and selectivity in heterogeneous catalysis. Here, we report a metal-ligand self-assembly method to create Pt single-site centers on powdered oxide supports. Impregnating Pt and a ligand 3,6-di-2-pyridyl-1,2,4,5- tetrazine (DPTZ) simultaneously (one-step) creates Pt-DPTZ single-sites on powdered MgO, Al 2 O 3 , and CeO 2 . MgO has the most uniform single-sites due to a strong, non-competitive support-ligand interaction, and a support-metal interaction of appropriate strength. Pt(II) centers are stabilized between the N binding pockets of DPTZ, with minimal metallic nanoparticle formation. This system was characterized by XAS, XPS, TEM, XRD, and CO adsorption. Sequential impregnation of Pt and DPTZ (two-step) was also tested on Al 2 O 3 and CeO 2 , but is not as effective as the one-step method due to limited Pt accessibility and mobility. These oxide-supported Pt-DPTZ single-sites were found to be effective catalysts in hydrosilylation reactions. In conclusion, this work demonstrates a metal-ligand self-assembly strategy to create metal singlesite centers on high surface area catalyst supports.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructure and mechanical behavior of laser remelted amorphous Al-Ni-La welds

To explore the feasibility of using laser powder bed fusion systems to print bulk amorphous Al alloys, a single autogenous weld produced by laser remelting on a cast Al-5La-9Ni (at.%) alloy was studied for its microstructure and mechanical behavior. The solidification rates experienced by material within the welds were high enough to produce entirely amorphous regions within the welds. Welds were characterized using SEM, STEM, and APT and were found to contain Ni-rich amorphous clusters. Micropillar compression tests were used to assess mechanical properties of the welds and found that all of the amorphous regions exhibited yield strengths around 1 GPa. In conclusion, these results are discussed in the context of diffusivity of Ni and rare earth elements in liquid, glass forming ability, thermodynamic driving force for phase formation during solidification, free volume concentrations in bulk metallic glasses, and cluster-related softening.

APT↗

Characterization of shielding materials used in neutron scattering instrumentation

The nuclear cross-sections of certain isotopes make some materials excellent candidates for neutron shielding. We have performed a series of measurements examining the transmission, reflection, and nuclear Bragg scattering of a series of common materials used for neutron shielding. Here, we concentrate on characterizing the materials most likely to be used in neutron scattering instrumentation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Microstructural features underpinning the mechanical behavior of powder metallurgy Cr-based alloys

Refractory materials such as Cr-based alloys offer the potential of enhanced elevated temperature performance but have been limited by their poor formability. However, powder metallurgy has been shown to be a viable pathway to fabricate these alloys. Nanophase separation sintering (NPSS) in particular has been used in the literature to accelerate the densification of powder metallurgy Cr- and W-based alloys. Here, we explore microstructure evolution during NPSS in a binary Cr 85 Ni 15 alloy consolidated via (i) cold pressing & pressureless sintering and (ii) hot isostatic pressing followed by hot extrusion & hot upsetting, and the role of these different processing routes on resulting material properties. The alloy lacked room temperature tensile ductility regardless of consolidation process, with multi-length scale characterization, including scanning electron microscopy, transmission electron microscopy, atom probe tomography, X-ray diffraction, and uniaxial tensile testing, revealing that brittleness was due to intrinsically poor Cr grain boundary cohesion. Tensile testing conducted at 760 °C showed marked strength reduction for the extruded & upset (94 %) condition compared to the pressed & sintered (18 %). The formation of orthorhombic CrNi 2 intermetallics functioned as precipitate strengtheners and prevented elevated temperature softening in the pressed and sintered condition. The findings offer foundational insights into aiding the future development of Cr-based alloys.

36 MATERIALS SCIENCE↗

Deformation and fracture characteristics of Al6092/SiC/17.5p metal matrix composite sheets due to heat treatments

Highlights: • Al{sub 2}Cu, Al{sub 4}Cu{sub 2}Mg{sub 8}Si{sub 7} and MgAl{sub 2} precipitations are formed between Al-matrix and SiC particle interface after T6-treatement • O-condition annealing decrease Al{sub 2}Cu intermetallic compound and increase elongation to fracture • 6092Al/SiCp composite at O-condition annealing is more sensitive to strain rate than the one heat treated by T6-treatment • Dimple density in the fracture surface of Al/SiCp composite varies as a function of heat treatment and strain rate - Abstract: In metal matrix composite (MMC) materials, the reaction between the metal matrix and reinforcement particles could change the composition of the matrix and the interface and lead to interfacial compounds. These intermetallic compounds may have either a deleterious effect to the mechanical properties or beneficial effect in enhancing the toughness and ductility of the composite. An aluminium 6092 alloy with 17.5% volume fraction silicon carbide (SiC) particles sheet manufactured by means of powder metallurgical method, heat treated to T6 condition, is used to obtain a fundamental understanding of the heat treatment effect on the fracture mechanism, the microstructural changes and the interface between the Al-matrix and SiC particles. Changes in the microstructure of the Al/SiCp and the topography of the fracture are investigated using scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM) to characterize the precipitate and intermetallic compounds formed at the Al/Sic interface. X-ray diffraction (XRD) is utilized to characterize the phase formation and to give confidence in the results of TEM and EDS. Tensile tests with different strain rates (8 × 10{sup −5}, 8 × 10{sup −4}, 8 × 10{sup −3}, 8 × 10{sup −2} and 0.16 s{sup −1}) were carried out to study the toughness and to find a correlation between the strain rate and heat treatment. Under T6 condition, the results show that the mechanical property of this MMC is less ductile due to the formation of precipitations as a result of either the interaction between the Al and SiCp or from hardening precipitation treatment, e.g. Al{sub 2}Cu, Al{sub 4}Cu{sub 2}Mg{sub 8}Si{sub 7} and MgAl{sub 2}. O-condition annealing can reduce the detrimental effect of the intermetallic compounds in the interface region and improve the toughness and ductility of the material by decreasing the intermetallic compound (Al{sub 2}Cu). However, the Al/SiC sheet treated with O-condition annealing is more sensitive to the strain rate than the one treated with T6.

36 MATERIALS SCIENCE↗

Excitation spectrum and low-temperature magnetism in the disordered defect-fluorite Ho2⁢Zr2⁢O7

In this work, we report on the thermomagnetic characterization and crystalline-electric field (CEF) energy scheme of the disordered defect-fluorite Ho2⁢Zr2⁢O7. This structural phase is distinguished by the coexistence of magnetic frustration and extensive disorder, with Ho3+ and Zr4+ sharing randomly the same 4⁢𝑎 site with even 50% occupancy, and an average 1/8 oxygen vacancy per unit cell. AC magnetic susceptibility measurements performed on powder samples down to 0.5 K revealed signs of slowing spin dynamics without glassy behavior, including a frequency dependent peak at ∼1K. Yet, no evidence for long-range magnetic order is found down to 200 mK in the specific heat. Inelastic neutron scattering measurements show a weak, low-lying CEF excitation around 2 meV, accompanied by a broad level centered at 60 meV. To fit our observations, we propose an approach to account for structural disorder in the crystal-field splitting of the non-Kramers Ho3+. Our model provides an explanation to the broadening of the high-energy, single-ion excitations and suggests that the zirconate ground-state wavefunction has zero magnetic moment. Through the breaking of local symmetry, structural disorder enables the magnetic response observed in Ho2⁢Zr2⁢O7, allowing the mixing of low-lying states at finite temperatures. Finally, we show that this scenario is in good agreement with the bulk properties reported in this work.

Gardner, Jason [ORNL] (ORCID:0000000278234072)↗

Optimizing Process Parameters to Produce Single Phase YBa2Cu3O7 Powder

Process parameters such as temperature and time are varied to obtain single phase (pure) YBa2Cu307 powders. X-ray diffraction patterns of superconducting and nonsuperconducting powders are observed in situ in normal and elevated temperature environments to confirm known strong peaks that are unique to YBa2Cu307. Peaks vary in magnitude as a result of superconducting - nonsuperconducting phase transitions. Known strong peaks serve as our basis in monitoring transitional changes. Peak isotherms obtained experimentally are correlated with theoretical models to identify the weighting factor that characterizes the optimum isotherm. By isolating the parameters under which 100% peak growth occurs most rapidly, we obtain the optimum isotherm. The choices made for firing temperature and atmosphere were determined to be the primary factors necessary to ensure sample purity.

Hurley, J. S.↗

Effect of Processing Route on Strain Controlled Low Cycle Fatigue Behavior of Polycrystalline NiAl

The present investigation examines the effects of manufacturing process on the total axial strain controlled low cycle fatigue behavior of polycrystalline NiAl at 1000 K, a temperature above the monotonic Brittle-to-Ductile Transition Temperature (BDTT). The nickel aluminide samples were produced by three different processing routes: hot isostatic pressing of pre- alloyed powders, extrusion of prealloyed powders, and extrusion of vacuum induction melted ingots. The LCF behavior of the cast plus extruded material was also determined at room temperature (below the BD77) for comparison to the high temperature data. The cyclic stress response, cyclic stress-strain behavior, and strain-life relationships were influenced by the alloy preparation technique and the testing temperature. Detailed characterization of the LCF tested samples was conducted by optical and electron microscopy to determine the variations in fracture and deformation modes and to determine any microstructural changes that occurred during LCF testing. The dependence of LCF properties on processing route was rationalized on the basis of starting microstructure, brittle-to-ductile transition temperature, deformation induced changes in the basic microstructure, deformation substructure, and synergistic interaction between the damage modes.

Rao, K. Bhanu Sankara↗

Thermal Performance Testing of Cryogenic Insulation Systems

Efficient methods for characterizing thermal performance of materials under cryogenic and vacuum conditions have been developed. These methods provide thermal conductivity data on materials under actual-use conditions and are complementary to established methods. The actual-use environment of full temperature difference in combination with vacuum-pressure is essential for understanding insulation system performance. Test articles include solids, foams, powders, layered blankets, composite panels, and other materials. Test methodology and apparatus design for several insulation test cryostats are discussed. The measurement principle is liquid nitrogen boil-off calorimetry. Heat flux capability ranges from approximately 0.5 to 500 watts per square meter; corresponding apparent thermal conductivity values range from below 0.01 up to about 60 mW/m- K. Example data for different insulation materials are also presented. Upon further standardization work, these patented insulation test cryostats can be available to industry for a wide range of practical applications.

Fesmire, James E.↗

Bulk nanocrystalline Al alloys with hierarchical reinforcement structures via grain boundary segregation and complexion formation

Grain size engineering, particularly reducing grain size into the nanocrystalline regime, offers a promising pathway to further improve the strength-to-weight ratio of Al alloys. Unfortunately, the fabrication of nanocrystalline metals often requires non-equilibrium processing routes, which typically limit the specimen size and require large energy budgets. In this study, multiple dopant elements in ternary Al alloys are deliberately selected to enable segregation to the grain boundary region and promote the formation of amorphous complexions. Three different fully dense bulk nanocrystalline Al alloys (Al-Mg-Y, Al-Fe-Y, and Al-Ni-Y) with small grain sizes were successfully fabricated using a simple powder metallurgy approach, with full densification connected directly to the onset of amorphous complexion formation. All the compositions demonstrate densities above 99% with grain sizes <60 nm following consolidation via hot pressing at 585 °C. The very fine grain structure results in excellent mechanical properties, as evidenced by nanoindentation hardness values in the range of 2.2-2.8 GPa. Detailed microstructural characterization verifies the segregation of all dopant species to grain boundaries as well as the formation of amorphous complexions, which suggests their influential role in aiding effective consolidation and endowing thermal stability in the alloys. Moreover, nanorods with a core-shell structure are also observed at the grain boundaries, which likely contribute to the stabilization of the grain structure while also strengthening the materials. Lastly, intermetallic particles with sizes of hundreds of nanometers form in all systems. As a whole, the results presented here demonstrate a general alloy design strategy of segregation and boundary evolution pathway that enables the fabrication of multiple nanocrystalline Al alloys with hierarchical microstructures and improved performance.

36 MATERIALS SCIENCE↗

A Road Map for the Advanced Manufacturing of Ferritic-Martensitic Steels

Advanced manufacturing (AM) is a disruptive manufacturing process often referred to as “the next industrial revolution” because of its ability to fabricate components with complex geometries and site-specific materials and properties. While other industries, like automotive, aerospace, and fossil-fired power companies, are adopting and evaluating AM processes, the nuclear industry, including the fusion materials community, has been somewhat slow to capitalize on the seemingly beneficial aspects of AM. To address this gap, Oak Ridge National Laboratory is evaluating candidate AM techniques to fabricate nuclear-relevant materials including ferritic-martensitic (FM) steels. This paper discusses the development of a road map for AM approaches for FM steels. Specifically, the connection among alloy composition, additive processes, processing conditions, and postprocessing and the resulting microstructure using both wire-based and powder-based directed energy deposition techniques is detailed. Lastly, strategies to develop specialized alloys for additive manufacturing are outlined.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Temperature-dependent diffuse reflectance measurements of ceramic powders in the near- and mid-infrared spectra

Radiative properties are critical to quantify radiative energy fluxes between surfaces and in participating media. However, there is limited experimental data on temperature-dependent radiative properties of materials. Herein, this work focuses on experimentally measuring temperature-dependent diffuse reflectance in the near- and mid-infrared spectra (1–20 μm) for ceramic particles with applications as heat-transfer and thermal-storage media in concentrated solar power (CSP) plants. Specifically, a commercially available sintered bauxite proppant, ACCUCAST ID80, and its primary chemical constituents—alumina (Al 2 O 3 ) and silica (SiO 2 )—are measured in powder form using a Fourier transform infrared spectrometer (FTIR) coupled with a specialized diffuse reflectance accessory and a heated stage. Room-temperature diffuse reflectance measurements show increased absorption in tests with greater mass fractions of the ceramic samples. There is a strong correlation in the measured reflectance spectra of ACCUCAST with alumina and silica in the spectral range 2000–500 cm –1 (5–20 μm). Whereas, for shorter wavelengths (< 5 μm), the absorptance for ACCUCAST is greater than the absorptance for alumina and silica, indicating contributions from other chemical species present in the composite material. For the first time, temperature-dependent diffuse reflectance measurements are reported for ACCUCAST up to 1000 °C. These results are compared against those of alumina and silica through the calculation of a thermal emittance. All three materials exhibit a calculated emittance of ~0.9 at room temperature. However, this value decreases to ~0.6 for ACCUCAST and drops to less than 0.4 for alumina and silica at 1000 °C. Thermal cycling in air at 1000 °C resulted in a visible color change from dark grey to light orange for ACCUCAST and a subsequent larger increase in reflectance for wavelengths less than 5 μm as compared to ACCUCAST thermally cycled at 1000 °C in vacuum. Alumina and silica spectra proved to be largely unaffected by thermal cycling under atmospheric conditions. Overall, this study establishes a powerful technique for the characterization of radiative properties of particulate materials as a function of temperature and presents a detailed case study of ACCUCAST, a candidate for next-generation particle-based CSP.

14 SOLAR ENERGY↗

Laser metal deposition of refractory high-entropy alloys for high-throughput synthesis and structure-property characterization

Progress in materials development is often paced by the time required to produce and evaluate a large number of alloys with different chemical compositions. This applies especially to refractory high-entropy alloys (RHEAs), which are difficult to synthesize and process by conventional methods. To evaluate a possible way to accelerate the process, high-throughput laser metal deposition was used in this work to prepare a quinary RHEA, TiZrNbHfTa, as well as its quaternary and ternary subsystems by in-situ alloying of elemental powders. Compositionally graded variants of the quinary RHEA were also analyzed. Our results show that the influence of various parameters such as powder shape and purity, alloy composition, and especially the solidification range, on the processability, microstructure, porosity, and mechanical properties can be investigated rapidly. The strength of these alloys was mainly affected by the oxygen and nitrogen contents of the starting powders, while substitutional solid solution strengthening played a minor role.

additive manufacturing↗

Melt Pool characteristics on surface roughness and printability of 316L stainless steel in laser powder bed fusion

Purpose Surface quality and porosity significantly influence the structural and functional properties of the final product. This study aims to establish and explain the underlying relationships among processing parameters, top surface roughness and porosity level in additively manufactured 316L stainless steel. Design/methodology/approach A systematic variation of printing process parameters was conducted to print cubic samples based on laser power, speed and their combinations of energy density. Melt pool morphologies and dimensions, surface roughness quantified by arithmetic mean height (Sa) and porosity levels were characterized via optical confocal microscopy. Findings The study reveals that the laser power required to achieve optimal top surface quality increases with the volumetric energy density (VED) levels. A smooth top surface (Sa < 15 µm) or a rough surface with humps at high VEDs (VED > 133.3 J/mm 3 ) can serve as indicators for fully dense bulk samples, while rough top surfaces resulting from melt pool discontinuity correlate with high porosity levels. Under insufficient VED, melt pool discontinuity dominates the top surface. At high VEDs, surface quality improves with increased power as mitigation of melt pool discontinuity, followed by the deterioration with hump formation. Originality/value This study reveals and summarizes the formation mechanism of dominant features on top surface features and offers a potential method to predict the porosity by observing the top surface features with consideration of processing conditions.

Engineering↗

Controlling microstructure in deposits fabricated using powder blown direct energy deposition technique

The overall goal of this collaboration is to develop technologies to control grain morphology and microstructures of Inconel 718 components additively manufactured through the Direct Energy Deposition (DED) process (Identical to the LENS (laser engineered net shaping) processes) and to achieve equiaxed or near equiaxed grain structures. The phase1 technical collaboration was used to fabricate Inconel 718 builds with different process parameters, pre heat and scan strategies. The results were then rationalized using computational heat transfer and solidification models. Microstructural characterization showed that the aspect ratio of the grains can be reduced to less than 1.5, and that control of the grain sizes to within 50-100 μm could be potentially obtained by using an external source to preheat the substrate to 400 ̊C. Heat transfer models coupled with solidification models were used to rationalize the results which show that preheating lowered the temperature gradient thereby resulting in moving towards the equiaxed region of the columnar to equiaxed transition (CET) curve. The results demonstrate that higher preheat temperatures could be potentially used to obtain a truly equiaxed structure.

36 MATERIALS SCIENCE↗

Colloidal characterization of silicon nitride and silicon carbide

The colloidal behavior of aqueous ceramic slips strongly affects the forming and sintering behavior and the ultimate mechanical strength of the final ceramic product. The colloidal behavior of these materials, which is dominated by electrical interactions between the particles, is complex due to the strong interaction of the solids with the processing fluids. A surface titration methodology, modified to account for this interaction, was developed and used to provide fundamental insights into the interfacial chemistry of these systems. Various powder pretreatment strategies were explored to differentiate between true surface chemistry and artifacts due to exposure history. The colloidal behavior of both silicon nitride and carbide is dominated by silanol groups on the powder surfaces. However, the colloid chemistry of silicon nitride is apparently influenced by an additional amine group. With the proper powder treatments, silicon nitride and carbide powder can be made to appear colloidally equivalent. The impact of these results on processing control will be discussed.

Feke, Donald L.↗

Describing the Influence of Ball-milling on the Amorphization of Flubendazole Using the PDF and RMC Methods with X-ray Powder Diffraction Data

Flubendazole (FBZ) is a poorly water-soluble drug, and different methodologies have been proposed to improve its oral bioavailability. Obtaining the amorphous drug phase is an alternative to improve its water solubility. Several techniques for drug amorphization, such as spray drying, lyophilization, melt quenching, solvent-evaporation, and ball milling, can yield various types of structural disorder and possibly render variations in physicochemical properties. Herein, we focus on evaluating the influence of the ball-milling process on the amorphization of FBZ. The characterization of the average global and local structures before, during, and after the milling process is described by sequential Rietveld refinements, pair distribution function analysis, and the Reverse Monte Carlo method. In conclusion, we show that preserving the local structure (nearest molecules) can be responsible for avoiding the fast structure recrystallization commonly observed when using the solvent-evaporation process for the studied drug.

60 APPLIED LIFE SCIENCES↗