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At least 307 records · Page 17

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NASA NTRS1990

Preferred orientations in extruded nickel and iron aluminides

A plotting of inverse pole figures is used to characterize the preferred orientations in both powder-extruded and cast-and-extruded NiAl, FeAl, and Ni3Al; the preferred 111 orientation has been noted along the extrusion direction in both powder-extruded and cast-and-extruded NiAl. While powder-extruded FeAl also had a 111 preferred orientation in the as-extruded condition, 110 was observed upon casting and extrusion; this was in turn replaced by a 211 orientation preference upon annealing, although annealing did not change the preferred orientation in either NiAl or in powder-extruded FeAl.

Khadkikar, P. S.↗

NASA NTRS2017

A Novel Solid State Ultracapacitor

Novel dielectric materials were researched to develop an internal barrier layer capacitor that is fully solid state. These materials included reduced nanoparticles of barium titanate that were coated with various atomic layer deposited oxides. The nanoparticle powders were then densified into pellets and characterized using a dielectric test fixture over a frequency range of 20 Hz to 2 MHz. Densification and sintering were evaluated using scanning electron microscopic techniques. Ultimately, the samples showing the most promising electrical characteristics of permittivity, dissipation factor and equivalent series resistance were chosen to manufacture devices for subsequent testing.

Cortes-Pena, A. Y.↗

DOE OSTI2018

New compositional data on ancient mortars and plasters from Pompeii (Campania – Southern Italy): Archaeometric results and considerations about their time evolution

Highlights: • Mortar samples from Pompeii, with different constructive functions, were studied. • Characterization of the materials can be used for preparing compatible mortars. • Analogies and differences were highlighted to identify the constructive phases. • Preliminary statistic models were proposed to discriminate materials and constructive phases. Twenty-six samples of mortar used for various construction applications (joint mortars, floor mortars, filling mortars and plasters) were collected from different areas of the archaeological site of Pompeii (Campania - Sothern Italy). The mortar samples belong to various historical periods covering approximately 2000 years, from the 2nd century BC to the post excavation period (18–19th century). The samples were characterized employing Optical Microscopy (OM), X-ray Powder Diffraction (XRPD), X-ray Fluorescence (XRF), Electron Probe Micro Analysis (EPMA) and Raman Spectroscopy. Moreover, image analysis was carried out using JMicroVision software in order to determine the percentages of binder, macropores and aggregate, in terms of crushed ceramic fragments (cocciopesto), rock fragments and monocrystals. The application of these techniques allowed obtaining a complete chemical and minero-petrographic characterization of the samples, which may prove useful for preparing compatible repair mortars for future restoration works. The archaeometric study provided new data on the production technology of the mortars and the analogies and differences observed among the samples, enabled us to distinguish different constructive phases, thus confirming or rebutting the archaeological hypothesis on the dating of some samples. By combining compositional variables through the discriminant analysis, it was also possible to analyse the time evolution of the materials and to construct preliminary multivariate statistical models, helpful to identify the various typologies of mortars used in the different historical periods.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Nanomechanical Characterization of Additive Manufactured GRCop-42 Alloy Developed by Directed Energy Deposition Methods

Propulsion applications such as combustion chambers and nozzles for liquid rocket engines require the use of unique materials with superior mechanical and thermal properties. GRCop-42(Cu-4 wt.% Cr-2 wt.% Nb) is one such candidate material developed by NASA and is now being manufactured using additive manufacturing (AM) techniques. AM offers a unique processing environment different from traditional metal fabrication processes. This study characterized the mechanical and structural properties of as-deposited and heat-treated GRCop-42manufactured with Blown Powder Directed Energy Deposition (BPD)based on preliminary testing. The materials were characterized using several techniques including surface profiling by laser microscopy, mechanical stiffness by instrumented indentation, crystal structure, residual stress measurements using XRD and residual XRD, and chemical composition and microstructural evaluation using SEM with EBSD. The results of the study are compared using the BPD techniques for samples in the as-deposited and heat-treated conditions.

GRCop-42↗

DOE OSTI2024

In-situ and ex-situ characterization of irradiated AM materials

This study investigates the irradiation performance of laser powder bed fusion (LPBF) 316L and 316H stainless steels (SS), and their wrought counterparts. While LPBF 316L has been more studied, LPBF 316H is relatively new, with little prior data on its irradiation behavior. The research involved fabricating, preparing, irradiating, and characterizing six materials: LPBF 316L (two variants), LPBF 316H (two variants), and wrought 316L and 316H. LPBF materials were subjected to various heat treatments, including solution annealing and stress relief, and were irradiated using in-situ and ex-situ ion techniques at temperatures of 300°C and 600°C, with doses ranging from 0.2 dpa to 25 dpa. Under ex-situ irradiation with 4 MeV Ni 2+ ions at 600°C, the dislocation cell structures in LPBF316L-1 and LPBF316H-1 gradually evolved into a uniform dislocation network. At a low irradiation dose (0.2 dpa), the cell structures were still partially visible. At 2 dpa, a uniform dislocation network formed, though remnants of the original cell structure were still discernible as contrast domains. At 5 dpa and 10 dpa, even the contrast domains vanished. For irradiation at 300°C, the cell structure was still clearly visible at 0.2 dpa for LPBF316L-1. For LPBF316H-1, the dislocation cell structure was less apparent at the same dose but was still recognizable. With further increase in dose at 300°C, the dislocation cell walls were completely replaced by irradiation-induced defects and no longer visible. Void formation was observed for irradiation at 600°C. At 2 dpa, no evident voids were observed in either LPBF316L-1 or LPBF316H-1.

36 MATERIALS SCIENCE↗

NASA NTRS2016

Design, Development and Hotfire Testing of Monolithic Copper and Bimetallic Additively Manufactured Combustion Chambers

NASA and industry partners are working towards fabrication process development to reduce costs and schedules associated with manufacturing liquid rocket engine components with the goal of reducing overall mission costs. One such technique being evaluated is powder-bed fusion or selective laser melting (SLM) otherwise commonly referred to as additive manufacturing. The NASA Low Cost Upper Stage Propulsion (LCUSP) program was designed to develop processes and material characterization for the GRCop-84 copper-alloy commensurate with powder bed additive manufacturing, evaluate bimetallic deposition and complete testing of a full scale combustion chamber. As part of this development, the process has been transferred to industry partners to enable a long-term supply chain of monolithic copper combustion chambers. As a direct spin off of this program, NASA is working with industry partners to further develop the printing process for the GRCop-84 material in addition to the C-18150 (CuCrZr) material. To advance the process further and allow for optimization with multiple materials, NASA is also investigating the feasibility of bimetallic additively manufactured chambers. A 1.2k sized thrust-chamber was designed and developed to compare the printing process of the GRCop-84 and C-18150 SLM materials. A series of similar MCC liners also completed development with an Inconel 625 jacket bonded to the GRcop-84 liner evaluating direct metal deposition (DMD) laser and arc-based techniques. This paper describes the design, development, manufacturing and testing of these combustion chambers and associated lessons learned throughout the design and development process.

Gradl, Paul↗

DOE OSTI2019

Improved Oxygen Reduction Reaction Activity of Nanostructured CoS 2 through Electrochemical Tuning

Searching for efficient Pt-free oxygen reduction reaction (ORR) electrocatalysts has been actively pursued among the current electrocatalyst research community. The family of transition-metal chalcogenides, especially cobalt disulfide (CoS 2 ), has been reported as competitive ORR catalysts. In this work, we perform a detailed analysis of the intrinsic activity in terms of onset potentials and selectivity toward hydrogen peroxide of CoS 2 in both acid and alkaline medium. Our detailed characterizations of this system via X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and calculated bulk and surface thermodynamics and ORR mechanism reveal pH-dependent electrochemical evolution of the CoS 2 surfaces. Using XPS results before and after ORR in combination with density functional theory (DFT) calculations for individual surfaces reveals sulfur to oxygen substitution, and partial dissolution occurs in acidic media, while thin cobalt oxide films supported by CoS 2 are formed in alkaline media. The comprehensive DFT calculations of the ORR activities on these systems reveal that sulfur is an unlikely ORR active site, while undercoordinated Co metal site in the CoS 2 is less active than very active undercoordinated Co metal site in the Co oxide film. Using these guiding principles, we then demonstrate that electrochemical lithium (Li) tuning of CoS 2 in organic electrolyte increases its ORR performance in both acid and alkaline medium. Detailed characterizations demonstrate that the grain size of CoS 2 particle is considerably reduced and has a much richer surface oxygen content after electrochemical Li tuning (LiET-CoS 2 ) as the direct consequence of the Li galvanostatic cycling. The general efficacy of this method toward transition-metal chalcogenides (T-M-X) is further demonstrated by enhanced ORR activities of CoS and Ni 3 S 2 in alkaline and neutral medium, respectively. This work opens up an opportunity for probing more advanced T-M-X-based catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Characterization of Roughness, Porosity and Thermal Resistances of Continuous Casting Mold Slag Layers Devitrified and Crystallized in Laboratory

This paper presents an experimental investigation about the variation, with temperature, of surface roughness, porosity, degree of crystallization and microstructure, occurring in solid layers of a commercial mold powder slag used for casting medium carbon steel thin slabs. Characterization is done with samples devitrified and crystallized at 698 K, 823 K, 898 K and 973 K (425 °C, 550 °C, 625 °C and 700 °C) for 10,800 seconds, in the furnace of a high-temperature confocal laser scanning microscope. As well as, with slag disks devitrified non-isothermally in a heat flow apparatus based on the application of Fourier's law in steady state conditions, where the high temperature surface is maintained at selected values, between 927 K and 1241 K (654 °C and 968 °C). Surface roughness and porosity determinations are performed by image analysis of confocal laser scanning and scanning electron micrographs, respectively. For the time considered and temperatures ≥ 823 K (550 °C) the slag crystallizes completely, and variations of roughness and porosity with temperature are associated with changes in size and packing of the primary crystalline-phase grains. Crystallization induced porosity is significant and causes slag layer expansion. Hence crystallization does not lead to gap formation with a neighboring surface (e.g., mold wall) by shrinkage. Instead, surface separation arises from development of roughness, and measurements with the heat flow apparatus confirm that interfacial thermal resistance between a slag layer and a metallic wall can be estimated from the sum of the means of maximum peak to valley height of their surfaces. Furthermore, the results establish that slag layers roughness and porosity increase with temperature and reveal effective thermal conductivities in the range of ~ 0.3 to ~ 0.5 W/m K. Low effective thermal conductivities must be a consequence of porous bands, whose porosity depends on temperature and reaches values as high as ~ 0.20 and ~ 0.50.

36 MATERIALS SCIENCE↗

DOE OSTI2024

The evolution of model Rh/Fe 3 O 4 (001) catalysts in hydrogen environments

Single metal atoms dispersed on oxides are a new emerging class of catalysts owing to their unique electronic and chemical properties. Here, in this study, we have prepared a series of model single-atom catalysts possessing well-characterized Rh sites that include Rh adatoms (Rh ad ), mixed surface layers with octahedrally-coordinated Rh (Rh oct ), as well as metallic Rh clusters and nanoparticles (Rh met ) on Fe 3 O 4 (001). Using X-ray photoelectron spectroscopy (XPS) and scanning tunneling microscopy (STM), we investigated the activity of such model systems towards H2 and their stability in reducing environments. Our results show that the atomically dispersed Rhad and Rhoct species do not activate H 2 , which would result in the formation of surface hydroxyls on Fe 3 O 4 (001). In contrast, the presence of Rh met in H 2 results in the formation of hydroxyls and subsequent etching of the Fe 3 O 4 (001) at higher temperatures (≥ 500 K) due to water formation via the Mars-van Krevelen mechanism. Additionally, such surface etching leads to the release of the Rh oct from the surface lattice and their sintering to Rh met . To bridge the material gap between the surface science models and high surface area catalysts, we perform parallel studies on powder Rh/Fe 3 O 4 catalysts. The XPS characterization shows remarkable similarities between these systems. Further, our surface science studies provide an atomistic picture of the behavior of high surface area catalysts in the H 2 atmosphere.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Laser powder bed fusion of Inconel 718 on 316 stainless steel

The joining of Inconel 718 and 316 stainless steel has notable industrial importance. However, traditional arc-welding has many issues. In particular, the formation of the detrimental Nb-rich Laves phase in the heat affected zone can promote crack initiation and propagation, which leads to poor mechanical properties. The small heat input and the rapid solidification of laser powder bed fusion (PBF) has the potential to suppress this problem. Despite the infancy of the multi-material PBF, it is of interest to investigate the relationship among the process parameter, the microstructure at the materials joining point, and the mechanical performance. In this study, we used high-speed x-ray imaging to in-situ monitor the printing of Inconel 718 tracks on a 316H SS substrate via laser powder bed fusion, followed by post-build characterization and testing with SEM, XRD and nanoindentation. We observed that a higher linear energy density resulted in a more diffused interface and a smaller compositional gradient, but as a trade-off, generated more keyhole pores and thermal cracks. Furthermore, we also showed that the built layer exhibited chemical inhomogeneity at two length scales: a tens-of-mu m-scale compositional vortex due to the melt flow, and a sub-mu m-scale Nb-rich dendritic structure due to the non-equilibrium solidification that led to the formation of the Laves phase. It was inferred that the chemical inhomogeneity may benefit the mechanical properties at the interface by providing more interlocking between the two materials and also by limiting the effect of the brittle Laves phase to potentially short range.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Is Cs 2 TiBr 6 a promising Pb-free perovskite for solar energy applications?

In a quest for Pb-free perovskites suitable for solar energy applications, Cs 2 TiBr 6 has recently been reported as a promising compound, with appropriate optical and electrical properties as well as high stability under environmental stresses. In this study, we pursue investigation on this compound, demonstrating phase pure Cs 2 TiBr 6 powder formation using solution synthesis and providing complementary experimental characterization and theoretical calculations. An experimental absorption onset of around 2.0 eV is extracted and a weak broad photoluminescence is measured. Density functional theory calculations predict an indirect bandgap, parity-forbidden for both the direct and indirect transitions, which explains the weak and Stokes shifted luminescence. Additionally, we highlight the strong instability of Cs 2 TiBr 6 powder in ambient atmosphere. Therefore, our experimental results supported by theoretical calculations differ from previous results and raise doubts on the suitability of Cs 2 TiBr 6 in its pristine form for solar energy applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Synthesis, crystal growth and characterization of the pyrochlore Er 2 Ti 2 O 7

Pyrochlore erbium titanate samples in the form of powders (with nominal compositions of Er 2 Ti 2+ x O 7 , -0.08 ≤ x ≤ 0.08) and bulk single crystals were prepared to elucidate the effect of synthesis and growth conditions on their composition, structure, and transition temperature. All the samples were characterized using X-ray diffraction and specific heat measurements. Larger lattice parameters were measured for Ti-deficient stuffed powders, Er 2 (Ti 2- x Er x )O 7- δ , while Ti-rich anti-stuffed powders, (Er 2- x Ti x )Ti 2 O 7+ δ , showed a decrease in the lattice parameter. The lattice parameter for the stoichiometrically synthesized powder, Er 2 Ti 2 O 7 , was measured to be a = 10.07522(9) Å. Single crystals grown by the conventional floating zone (FZ) technique were Ti deficient (stuffed) and darker in color due to oxygen vacancies. Using the traveling solvent floating zone (TSFZ) method, a high structural quality, transparent and stoichiometric Er 2 Ti 2 O 7 single crystal was grown at a lower temperature using the TiO 2 solvent. The heat capacity measurements of the TSFZ grown Er 2 Ti 2 O 7 crystal and stoichiometric powder exhibited a very close magnetic transition temperature T c of ~1.23 K that was suppressed in off-stoichiometric samples, demonstrating correlations between the stoichiometry and ground state magnetism in Er 2 Ti 2 O 7 .

optics, thermal conductivity, defects, charge tran↗

DOE OSTI2025

Chemical speciation correlated with microstructural heterogeneity of interdicted uranium materials

Two uranium powders seized by law enforcement in Victoria, Australia, have been characterized by established nuclear forensic methods in a previously published study. Here, in this work, the results of further characterization by a scanning transmission x-ray microscope (STXM) operating in the soft x-ray regime are reported. STXM images are used to estimate the elemental distribution in micrometer-scale particles of each powder, and oxygen K-edge absorption spectra are used to determine the chemical state of uranium. The results of the current study are consistent with the previous analysis; the first powder is found to be a potassium-uranium hydrate, while the second powder is determined to be a mixture of uranium oxides primarily consisting of UO 3 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2021

Powder diffraction

Powder diffraction is a non-destructive technique, which is experimentally simple in principle. Because the physics behind diffraction is well understood, an exceptionally large amount of information can be obtained from a single measurement. The positions and relative intensities of the peaks yield a fingerprint that can be used for qualitative phase analysis. Quantitative phase analysis can be obtained by detailed analysis of the intensities. Unit cells can be derived from the peak positions. Crystal structures can be solved using powder diffraction data and refined by the Rietveld method. The peak profiles contain information about crystallite size, strain and nanostructure. Non-idealities in the intensities give information on texture. Abandoning the crystallographic model provides information about local structure, by pair distribution function analysis. For powder diffraction, everything is a sample; the technique is commonly applied to characterize minerals, ceramics, metals and alloys, catalysts, polymers, pharmaceuticals, organic compounds, environmental and forensic samples, among others. The major features of contemporary laboratory powder diffractometers are described. Methods for obtaining suitable powder specimens are summarized. Major applications of qualitative and quantitative phase analysis, structure solution, size/strain/nanostructure analysis using peak profiles, texture analysis and pair distribution function analysis are introduced.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Preliminary Characterization and Evaluation on FFF Manufactured 316H and ODS Steels

The Advanced Materials and Manufacturing Technology (AMMT) program develops cross-cutting technologies in support of a broad range of nuclear reactor technologies and maintains U.S. leadership in materials and manufacturing technologies for nuclear energy applications. The overarching vision of AMMT is to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy. Solid-state advanced manufacturing techniques can overcome some of the challenges in liquid-based additive manufacturing (AM) processes and should therefore be considered in material design and manufacturing as well. The work presented in this report forms part of a study on solid-state AM techniques of 316 stainless steels (SS) and oxide dispersion strengthened (ODS) steel components and supports the vision and goals of the AMMT program relevant to accelerate the development and deployment of advanced manufacturing processes. Achieving this can provide a safety improvement through larger safety margins, economic benefit for higher efficiency during operation, and a cost reduction through more effective manufacturing processes and less waste. This study provides preliminary information on development of the fused-filament fabrication (FFF) process using different powder types to demonstrate the sensitivity, and therefore the characterization of these sample components. The full solid-state manufacturing feasibility study will be completed and reported in a final feasibility evaluation during 2025. The study investigation used two 14YWT ODS powder batches, which provided information and the effect of different powder morphologies on manufacturability. The two 316SS powders demonstrated the effect of powder size on the manufacturability using FFF. Two product forms, namely a honeycomb structure and flat samples, were manufactured to demonstrate the flexibility of product form.

36 MATERIALS SCIENCE↗

NASA NTRS2013

Design of a Uranium Dioxide Spheroidization System

The plasma spheroidization system (PSS) is the first process in the development of tungsten-uranium dioxide (W-UO2) fuel cermets. The PSS process improves particle spherocity and surface morphology for coating by chemical vapor deposition (CVD) process. Angular fully dense particles melt in an argon-hydrogen plasma jet at between 32-36 kW, and become spherical due to surface tension. Surrogate CeO2 powder was used in place of UO2 for system and process parameter development. Particles range in size from 100 - 50 microns in diameter. Student s t-test and hypothesis testing of two proportions statistical methods were applied to characterize and compare the spherocity of pre and post process powders. Particle spherocity was determined by irregularity parameter. Processed powders show great than 800% increase in the number of spherical particles over the stock powder with the mean spherocity only mildly improved. It is recommended that powders be processed two-three times in order to reach the desired spherocity, and that process parameters be optimized for a more narrow particles size range. Keywords: spherocity, spheroidization, plasma, uranium-dioxide, cermet, nuclear, propulsion

Cavender, Daniel P.↗

DOE OSTI2019

Vickers Microhardness Studies for SmBa{sub 2}Cu{sub 3}O{sub 7-δ} Added with NiO Nanosized Particles

The effect of nanosized particles NiO addition on the Vickers microhardness of polycrystalline SmBa{sub 2}Cu{sub 3}O{sub 7-δ} was investigated. Various amounts of nanosized particles NiO (x = 0.00, 0.02, 0.04, 0.08, and 0.12 wt%) were added to SmBa{sub 2}Cu{sub 3}O{sub 7-δ} prepared by the solid-state reaction method. Sample characterizations were carried out using X-ray powder diffraction (XRD), particle induced X-ray emission (PIXE), Rutherford backscattering (RBS), and scanning electron microscopy (SEM). The nanosized particle addition does not influence the orthorhombic structure of SmBa{sub 2}Cu{sub 3}O{sub 7-δ}, whereas it affects the oxygen content δ. The electrical and mechanical properties of (NiO){sub x}SmBa{sub 2}Cu{sub 3}O{sub 7-δ} samples were measured using four-standard probe technique and Vickers microhardness in order to investigate the effect of NiO nanosized particles on superconducting transition temperature and Vickers microhardness number H{sub v}. The Vickers microhardness data were analyzed using Hays and Kendall (HK), elastic plastic deformation (EPD), and modified proportional specimen resistance (MPSR) models. The analysis showed that the MPSR model was found to be the best to describe the behavior of H{sub v}.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Microstructural evolution and intermetallic formation in Zn-3Mg (wt%) powder mixture processed by high-pressure torsion

Severe plastic deformation (SPD) techniques have been used extensively over the past 40 years for producing strong metals and alloys. High-pressure torsion (HPT) is one of the most promising SPD techniques for achieving high strength through nanoscale grain refinement and phase transformation. In this research, a mixture of pure zinc (Zn) and magnesium (Mg) powders, Zn-3Mg (wt%), was HPT-processed under a pressure of 6 GPa for 1, 5, 10, 20, and 30 turns at room temperature to achieve a high strength biodegradable material. In order to understand the effects of pre-consolidation on the resulting microstructure and hardness, HPT processing was performed on loose powders placed in the die and also on a pre-compacted powder mixture and the resulting HPT disks were characterized by X-ray diffraction, scanning electron microscopy, atom probe tomography, and Vickers microhardness. In both cases, the HPT disk microstructures contained nanoscale grains, and stable and metastable strain-induced intermetallics, but an unusual softening appeared at large shear strains. Grain size, grain morphology, and the formation of different intermetallics were analyzed to explain the unusual hardness distribution, and it was found that an inverse Hall-Petch relationship between hardness and grain size exists. It is suggested that thermally-activated phenomena such as grain boundary sliding contributed to the strain-induced softening of this nano-structured biomaterial due to its low melting point. Finally, the current results are compared with those for HPT-processed cast alloys and hybrids of the same composition.

36 MATERIALS SCIENCE↗