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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 613 records · Page 34
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Defects and anomalies in powder bed fusion metal additive manufacturing

Metal additive manufacturing is a disruptive technology that is revolutionizing the manufacturing industry. Despite its unrivaled capability for directly fabricating metal parts with complex geometries, the wide realization of the technology is currently limited by microstructural defects and anomalies, which could significantly degrade the structural integrity and service performance of the product. Accurate detection, characterization, and prediction of these defects and anomalies have an important and immediate impact in manufacturing fully-dense and defect-free builds. As such, this review seeks to elucidate common defects/anomalies and their formation mechanisms in powder bed fusion additive manufacturing processes. They could arise from raw materials, processing conditions, and post-processing. While defects/anomalies in laser welding have been studied extensively, their formation and evolution remain unclear. Additionally, the existence of powder in powder bed fusion techniques may generate new types of defects, e.g., porosity transferring from powder to builds. Practical strategies to mitigate defects are also addressed through fundamental understanding of their formation. Such explorations enable the validation and calibration of models and ease the process qualification without costly trial-and-error experimentation.

42 ENGINEERING↗
DOE OSTI2020

Mirostructure Characterization of Friction Consolidated Copper-Nickel using a Machine Learning Approach: Developing Process to Microstructure Associations

Friction consolidation (FC) is a solid phase processing approach where discrete material forms such as powders, chips, nuggets, etc. are densified via shear deformation. The precursors are placed in a billet container and brought in contact with a rotating tool that applying the desirable amount of normal force. Under the combined action of the rotation and normal pressure, the discrete precursor is consolidated through porosity reduction and shear deformation. FC is increasingly being studied as an attractive approach to manufacturing fully dense parts from powder forms owing to its ability to mix, alloy and consolidate difficult-to-process precursors in minimal number of process steps. Material consolidation and deformation in shear consolidation processes have been studied extensively previously for different material combinations previously. However, despite the extensive research in this area, understanding of the mechanistic processes in pore consolidation, deformation-induced mixing and material solubility during FC is still evolving. Material development using solid phase processing approaches such as FC is often performed based on research experience/education, which can be biased. Conventional analysis and simulation tools in this area tend to be successful only when material thermodynamic pathways and microstructural evolution sequences resulting from processing are clearly defined or known. They are not as effective for emerging advanced manufacturing technologies where material evolution pathways are not well established. The ability to predict optimal process parameters based on material chemistry and bulk properties is essential to accelerate materials design and processing, as are an understanding of the relevant structure-processing-property relationships. These structure-processing-property-performance relationships are at the core of materials science research. Microstructure characterization provides the link to these four core areas, often through visualizing material microstructure using imaging techniques. However, linking microstructure image data (i.e., micrographs) to variables of interest (e.g., processing parameters, material chemistry) in a reproducible, generalizable, and quantitative manner is a significant challenge. Typically, quantitatively linking image data to processing history relies on significant domain knowledge and manual or subject matter expert (SME)-heuristic based image analysis. Such an approach to image analysis has the potential to be biased, inefficient, and difficult to replicate.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterization of alkali silica reaction gels using Raman spectroscopy

The ability of Raman spectroscopy to characterize amorphous materials makes this technique ideal to study alkali silica reaction (ASR) gels. The structure of several synthetic ASR gels was thoroughly characterized using Raman Spectroscopy. The results were validated with additional techniques such as Fourier transmission infrared spectroscopy, X-ray powder diffraction and thermogravimetric analysis. The Raman spectra were found to have two broad bands in the 800 to 1200 cm{sup −1} range and the 400 to 700 cm{sup −1} range indicating the amorphous nature of the gel. Important information regarding the silicate polymerization was deduced from both of these spectral regions. An increase in alkali content of the gels caused a depolymerization in the silicate framework which manifested in the Raman spectra as a gradual shift of predominant peaks in both regions. The trends in silicate depolymerization were in agreement with results from a NMR spectroscopy study on similar synthetic ASR gels.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Pure and cerium-doped zinc orthosilicate as a pigment for thermoregulating coatings

Microwave-assisted hydrothermal synthesis followed by high-temperature (1050 °C) calcination was used to prepare pure and cerium-doped zinc orthosilicate (Zn 2 SiO 4 ) pigments. Nanoscale Zn 2 SiO 4 and Ce–Zn 2 SiO 4 powders were blended with potassium silicate (K 2 SiO 3 ) and then applied to the aluminum substrate to obtain thermoregulating coatings. Electron beams with different energies were used to irradiate nanoscale pigment powders and coatings. X-ray diffraction (XRD), scanning electron microscopy (SEM), and transition electron microscopy (TEM) were used to characterize the phase composition, morphology, and atomic-level structure of materials. Here, the diffuse reflectance and absorption measurements of materials before and after irradiation indicated that Ce–Zn 2 SiO 4 -based coatings exhibit better radiation resistance compared to pure Zn 2 SiO 4 . Simple and straightforward preparation, as well as high radiation resistance, make Ce–Zn 2 SiO 4 -based thermoregulating coatings excellent candidates for space vehicles.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Reduced alkali-silica reaction damage in recycled glass mortar samples with supplementary cementitious materials

Recycling waste glass aggregate into concrete can reduce environmental impacts but also may lead to serious alkali silica reaction (ASR) damage. This study aims to characterize ASR damage development in the mortar samples containing reactive glass aggregates and investigate the damage reduction effect of the waste supplementary cementitious materials (SCMs), including recycled glass powders and fly ash. The recycled glass aggregate mortar samples with/without SCMs were prepared in this study. The length change tests were first conducted with the prepared mortar samples based on the ASTM C1260 standard. The results demonstrated the added SCMs can largely decrease early-age ASR expansion rate. The optical microscope and Scanning Electron Microscope (SEM) with Energy Dispersive X-ray Spectroscopy (EDS) were further conducted to characterize the ASR damage in mortar samples and investigate the damage mitigation mechanism with added SCMs. The combined SEM imaging and chemical analysis indicated added SCMs can decrease both the alkali and calcium content of the generated ASR gel. In addition, the ASR damage development inside mortar samples were monitored with dynamic micron X-ray CT (μCT) over a reaction period of 63 hour at the temperature of 80°C. The scanning patterns demonstrated the ASR damage can be easily developed from the area with initial cracks and sharp corners. In conclusion, the images of glass power and fly ash samples showed significantly reduced ASR damage. This study showed that adding of SCMs can largely reduce ASR deterioration and thus facilitate the recycling glass particles into concrete.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2026

Monitoring the Stability of Porous Coordination Cages during the Photoreduction of Porous Salt Thin Films

This study investigates the photochemical properties and stability of zirconium-based porous salts composed of coordination cages and redox-active polyoxometalates (POMs). While bulk porous salts demonstrated photoreduction confined to surface regions due to lim-ited light penetration and scattering effects, thin films of cage-POM assemblies were fabricated to address these challenges. These optically transparent films allowed access to the catalyst core, enabling enhanced photochemical characterization. Comparative studies revealed that the thin films exhibited superior photochemical activity and maintained porosity under optimized conditions, whereas bulk powders suffered from surface-limited photoreduction and cage decomposition. Furthermore, this work highlights the utility of thin films as a platform for studying and advancing the photochemical applications of porous salts.

Hoq, Jahidul [Indiana University, Bloomington, IN ↗
DOE OSTI2026

Post-Mortem Characterization of Cerium Speciation in Molten Calcium Chloride

Abstract Advancing radiochemistry and nuclear materials science requires understanding actinide interactions with molten salts, which are used in next-generation nuclear reactors and for processing of actinides to recover useful fissile material. Understanding chemical interactions of actinides with molten salts has been limited by challenges in developing spectroscopic and X-ray techniques that are compatible with the high temperatures necessary to study molten salts. In this work, interactions of CeO2 (serving as a nonradioactive surrogate for uranium and plutonium) with CaCl2 are characterized following heating. Scanning electron microscopy indicates CeO2 morphological changes from small (<1 μm) particles to 3–5 μm sheets. Powder X-ray diffraction and infrared and Raman spectroscopies show the formation of CeOCl at higher (850–1050 °C) temperatures. In the absence of a chemical reducing agent, it was found that a high-temperature, low-oxygen environment is the key to the formation of oxychloride and that oxychloride formation is inhibited by annealing the CeO2 starting material. Lastly, thermal analysis revealed lowering of the melting point of CaCl2 after heating with CeO2. In all, this work identifies applicable spectroscopic techniques to target studies of heavy elements in molten salt environments and highlights the relationship between chemical speciation and melting behavior, a key thermophysical property.

Kelly, Sheridon N. [Lawrence Livermore National La↗
DOE OSTI2022

The structure of sc16 GaP obtained at 17.5 GPa and 1400 K

We report using a laser-heated diamond anvil cell, a powdered sample of gallium phosphide was compressed to 17.5 GPa and heated up to 1400 K. The material obtained was characterized at room temperature using synchrotron x-ray diffraction. Experimental results were compared with first-principles calculations. The polymorph observed assumes the simple cubic structure (sc16) initially reported for GaAs at high pressures. Microdiffraction mapping showed variable grain sizes of the synthesized phase, with the largest grains located in the middle of the heated spot. Structural refinements were performed on selected grains. The structure predicted based on first-principles calculations is in close agreement with the experiments. The two Ga–P bonds show similar lengths in sc16-GaP; however, the bond angles differ, resulting in a distorted tetrahedral coordination geometry.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Tuning the magnetic ground state of Ce 1 - x Yb x RhIn 5 by Yb valence fluctuations

We characterize the properties of Ce 1–x Yb x RhIn 5 single crystals with 0 ≤ x ≤ 1 using measurements of powder x-ray diffraction, energy dispersive x-ray spectroscopy, electrical resistivity, magnetic susceptibility, specific heat, x-ray absorption near edge structure (XANES), and neutron diffraction. Here, the Yb valence v Yb , calculated from the magnetic susceptibility and measured using XANES, decreases from 3+ at x = 0 to ~2.1+ at x act = 0.2 , where x act is the measured Yb concentration. A transition from incommensurate to commensurate antiferromagnetism is observed in neutron diffraction measurements along Q = (0.5, 0.5, l) between 0.2 ≤ x act ≤ 0.27; this narrative is supported by specific-heat measurements in which a second robust feature appears at a temperature T I (T I < T N ) for the same concentration range. Magnetic susceptibility measurements also reveal features which provide additional evidence of magneticordering. The results of this study suggest that the evolution of the Yb valence plays a critical role in tuning the magnetic ground state of Ce 1–x Yb x RhIn 5 .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

28ID1 - PDF Beamline Radiation Shielding Analysis

The high flux hard x-ray damping wiggler (DW100) located in cell 28-ID provides a synchrotron source for the X-ray Powder Diffraction (XPD) beamline and the Pair Distribution Function (PDF) beamline. The primary purpose of these beamlines is the quantitative characterization of the atomic structure of complex materials; not just carefully prepared ideal systems, but materials as they are actually used.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Squeezing clathrate cages to host trivalent rare-earth guests

Strike difference of the trivalent rare-earth cations from their alkali and alkaline-earth peers is in the presence of localized 4f-electrons and strong spin-orbit coupling. Placing trivalent rare-earth cations inside the fullerene molecules or in between the blocks of itinerant magnetic intermetallics gave rise to plethora of fascinating properties and materials. A long-time missing but hardly desired piece is the semiconducting or metallic compound where rare-earth cations are situated inside the oversized polyhedral cages of three-dimensional framework. In this work we present a synthesis of such compounds, rare-earth containing clathrates Ba 8-x R x Cu 16 P 30 . The unambiguous proofs of their composition and crystal structure were achieved by a combination of synchrotron powder diffraction, time-of-flight neutron powder diffraction, scanning-transmission electron microscopy, and electron energy-loss spectroscopy. Our quantum-mechanical calculations and experimental characterizations show that the incorporation of the rare-earth cations significantly enhances the hole mobility and concentration which results in the drastic increase in the thermoelectric performance.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Investigation of the Effect of Chrome and Nickel Concentrations During Two-Piston Splat Quenching of Austenitic Stainless Steels

For solidification rates at or near equilibrium solidification conditions the effects of chrome (Cr) and nickel (Ni) on stainless steel solidification modes and microstructures are well detailed. However, fusion-based additive manufacturing (FBAM) processes that rely on faster, more rapid solidification rates call for a more in-depth understanding of the effects of rapid solidification on the solidification behavior and how these change with variations in alloy composition. Eleven custom stainless steel (SS) alloys with unique compositions based on 316L were made using targeted alloying element additions to generate feedstock with Cr/Ni eq ratios ranging from 0.9 to 2.1. Two-piston splat quenching (SQ) was used to produce rapid solidification conditions similar to those achieved in powder bed fusion processes in a fraction of the time and cost of traditional methods. Employing heat transfer simulations, SEM, TEM, and STEM characterization techniques, the SQ process was found to consistently produce solidification rates estimated to be between ~ 0.4 and 1.6 m/s. Five unique solidification microstructures were identified within the rapidly solidified SQ samples (primary austenite, massively transformed ferrite to austenite, primary austenite and massively transformed ferrite to austenite, primary ferrite, and primary ferrite and massively transformed ferrite to austenite). Both the primary ferrite solidification mode and primary ferrite phase were found to form at lower Cr/Ni eq values than previously predicted. SQ samples with compositions that were within the compositional specifications for 316L SS, an alloy which is commonly used in FBAM processes, demonstrated a wider range of potential solidification modes and microstructures that could form at rapid solidification rates than expected. Finally, by using SQ as a means to simulate rapid solidification conditions similar to those observed in FBAM processes, potential new alloy compositions can be screened faster and more cost effectively than purchasing and running test batches of the metallic powder.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Comparison of powder bed fusion and directed energy deposition for tailoring mechanical properties of traditionally brittle alloys

The mechanical performance of an Fe-Co intermetallic alloy processed by laser powder bed fusion (L-PBF) and laser directed energy deposition (L-DED) additive manufacturing is compared. L-PBF material was characterized by high strength (500–550 MPa) and high ductility (35%) in tension, corresponding to a ~250% increase in strength and an order-of-magnitude improvement in ductility relative to conventional material. Conversely, L-DED material exhibited similarly poor tensile properties to the conventional wrought alloy, with low strength (200–300 MPa) and low ductility (0–2.7%). Finally, the disparity in properties between L-PBF and L-DED material is discussed in the context of the fundamental differences between manufacturing methods.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Keyhole-mode Microscopy Dataset for Laser Powder-bed Fusion Modeling

Laser powder-bed fusion (LPBF) is an additive manufacturing (AM) technology that uses high-power sintering lasers to precisely construct metal designs. Material is accumulated by selectively sintering regions of a metal powder layer to a growing structure underneath forming a 3D geometry. Certain conditions make fusion in this process to operate in "keyhole-mode," characterized by targeted materials evaporating as plasma. While keyhole-mode operations can produce deeper molten pools than that observed in "conduction-mode", this mode of operation is often undesirable, as its molten regions can collapse on themselves, encapsulating metal vapors and forming cavities. The formation of such cavities negatively affects strength and consistency of the fused materials. To identify and avoid these detrimental effects of keyhole-mode operation, considerable data collection and analysis regarding this mode of operation is needed. Therefore, under the support of the "Open Data Initiative," Lawrence Livermore National Lab is releasing a dataset for analysis of this keyhole effect, and the conditions which transition operation from conduction-mode to keyhole-mode melting. This dataset consists of 600+ micrographs from laser powder-bed single track runs, with differing cross-section angles and input parameters, operating under both normal and keyhole mode operations. This journal documents the collection, organization, and usage of this dataset.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Performance Evaluation of LPBF Manufactured 316H Components

This work represents the continuation of a benchmark study that includes modeling, fabrication and characterization as demonstration to support industry’s adoption of advanced manufacturing processes in a variety of structures. This comprehensive study investigated the feasibility of using additive manufacturing (AM) technologies, specifically Laser Powder Direct Energy Deposition (LP-DED) and Laser Powder Bed Fusion (LPBF), to produce complex nuclear microreactor components using 316H stainless steel. The research focused on manufacturing an expanded elbow pipe component with transitioning sections, which are traditionally difficult and costly to produce through conventional manufacturing methods. The overall study’s primary objectives are therefore demonstrating AM viability for nuclear applications, optimizing process parameters, developing comprehensive material characterization protocols, validating computational modeling approaches, and establishing manufacturing guidelines for complex geometries. Although the initial work included the phased approach of cubical, upscaled cylindrical components, it is to enable to obtain more knowledge for the printing of the expanded elbow structure. The project achieved significant progress in process development by successfully optimizing LP-DED parameters to achieve 99.16-99.97% relative density in 316H stainless steel components. Through systematic evaluation of sixteen cube samples with varied laser powers (400-700W) and scan speeds (600-900 mm/min), optimal processing windows were identified at 500-550W with 600-700 mm/min or 650-700W with 650-900 mm/min scan speeds. The DED manufactured 316H demonstrated mechanical properties comparable or superior to wrought materials, with Young's modulus ranging from 153-208 GPa and controlled microstructural characteristics including greater than 95% face-centered cubic (FCC) phases and engineered cellular structures with sizes between 3.23-6.17 µm.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The crystal structure of a new calcium aluminate phase containing formate

A new calcium aluminate phase containing formate ions was synthesized and its crystal structure determined. This new phase is indicated as M-phase and was firstly observed in Portland cement pastes hydrated in presence of Ca-formate and in excess of water. The crystal structure of the M-phase was successfully solved in the R-3 space group of the trigonal system on the basis of synchrotron X-ray single crystal diffraction data. The structural model was confirmed by Rietveld refinement of the powder diffraction data acquired on the synthesized pure sample. The crystal structure of the M-phase is similar to that of ettringite, being characterized by columns of AlO{sub 6} octahedra alternating with groups of three edge-sharing CaO{sub 7} polyhedra. The formate ions (HCOO){sup −} share two oxygens with Ca polyhedra and are located in the interspace between the columns. The crystal structure of the M-phase testifies the strong interaction occurring between small organic molecules as formate and the calcium aluminate components of Portland cement.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Characterizing surrogates to develop an additive manufacturing process for U 3 Si 2 nuclear fuel

U 3 Si 2 is considered as an accident-tolerant nuclear fuel candidate due to its promising high uranium density along with its improved thermal properties. The current U 3 Si 2 powder metallurgical fabrication process encompasses numerous process steps with extensive fabrication times. Thus, an additive manufacturing process to fabricate U 3 Si 2 is currently under development to ultimately produce U 3 Si 2 fuel at a lower cost, in a timely and commercially-reliable manner. The current research work seeks to characterize U 3 Si 2 surrogate materials fabricated by a laser synthesis. The characterization results provided novel microstructural data that aided in the early development stages of an additive manufacturing process. For this study, cerium, zirconium, and hafnium, were selected as surrogates based on their thermodynamic properties and crystal structure. As a result, the laser-synthesized samples were characterized by means of scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) along with X-ray diffraction (XRD), where the different phases of formation, morphology, and microstructural features have been analyzed. Laser synthesis showed suitability for alloying Zr-Si and Hf-Si to ultimately form silicide compounds (Zr 3 Si 2 and Hf 3 Si 2 ).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Synthesis and characterization of the novel breathing pyrochlore compound Ba 3 ⁢Tm 2⁢ Zn 5⁢ O 11

In this study, a novel material from the rare-earth based breathing pyrochlore family, Ba 3 ⁢Tm 2 ⁢Zn 5 ⁢O 11 , was successfully synthesized. Powder x-ray diffraction and high-resolution powder neutron diffraction confirmed phase purity and the $F\bar4$3⁢𝑚 breathing pyrochlore crystal structure, while thermogravimetric analysis revealed incongruent melting behavior compared to its counterpart, Ba 3 ⁢Yb 2⁢ Zn 5⁢ O 11 . High-quality single crystals of Ba 3 ⁢Tm 2 ⁢Zn 5 ⁢O 11 were grown using the traveling solvent floating zone technique and assessed using Laue x-ray diffraction and single crystal x-ray diffraction. Further, thermodynamic characterization indicated paramagnetic behavior down to 0.05 K, and inelastic neutron scattering measurements identified distinct dispersionless crystal electric field energy bands, with the fitted crystal electric field model predicting a single-ion singlet ground state and an energy gap of ∼9 meV separating it from the first excited (singlet) state. Additional low-energy excitation studies on single crystals revealed dispersionless bands at 0.8 and 1 meV. Computed phonon dispersions from first-principles calculations ruled out phonons as the origin of these modes, further illustrating the puzzling and unique properties of Ba 3 ⁢Tm⁢ 2 Zn 5 ⁢O 11 .

36 MATERIALS SCIENCE↗