Search NASA⌕ Search

SEARCH · Search NASA

Results for “AM Powder Characterization”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,387 records · Page 77
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to fullscale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Moisture Stability of Sulfide Solid-State Electrolytes

In this report we detail a comprehensive study on the moisture stability of sulfide solid-state electrolytes in dry room environments. Although sulfide SSEs have many favorable attributes, this class of materials suffers from poor stability with water. Sulfide SSEs react with water to form gaseous H 2 S and a variety of solid byproducts like Li 3 PO 4 and LiOH, which go on to increase the interfacial impedance of solid-state batteries. Lab-scale research typically utilizes gloveboxes with <1 ppm water, however, the large-scale manufacturing of Li-ion batteries occurs in –40°C dewpoint dry rooms with around 126 ppm water. Consequently, the moisture stability of sulfide SSEs must be addressed if the manufacture of solid-state batteries based on sulfide SSEs is to be scaled up. Here, we are the first to characterize the moisture stability of sulfide SSEs according to both H 2 S and the degradation of ionic conductivity at different moisture setpoints ranging from –76°C to –40°C dewpoint. A variety of different SSE compositions are studied; namely, (Li 2 S) 75 (P 2 S 5 ) 25 , (Li 2 S) 70 (P 2 S 5 ) 30 , (Li 2 O) 7 (Li 2 S) 68 (P 2 S 5 ) 25 , (Li 2 O) 7 (Li 2 S) 63 (P 2 S 5 ) 30 , and (Li 2 S) 75 (P 2 S 5 ) 25 + 20 mol% LiI. We find that moisture stability improves with 75 mol% Li2S modifier content and the introduction of a Li 2 O co-modifier. After a 30 min exposure in a –40°C dewpoint dry room environment we found that (Li 2 S) 75 (P 2 S 5 ) 25 + 20 mol% LiI powder generated 0.1 cc/g H 2 S and its ionic conductivity decreased by over 50%. However, when SSE powder was exposed as a slurry in a dodecane carrier the same SSE composition generated 0 cc/g H 2 S and its ionic conductivity only dropped by 14%. Our results show that sulfide SSEs have acceptable moisture stability when appropriately processed in a dry room environment.

25 ENERGY STORAGE↗
DOE OSTI2020

Predicting Geometric Influences in Metal Additive Manufacturing

Metal additive manufacturing (AM) has evolved from scientific curiosity to a potential paradigm shift in materials manufacturing owing to its ability to control microstructure and fabricate complex geometries. However, geometry, often ignored as a variable, can have a significant impact on microstructure evolution, thereby indirectly limiting the design flexibility offered by AM. Currently, the process of retaining microstructure with changing geometry relies on trial and error-based processing followed by microstructural evaluation that places significant demands on time and costs associated with experimentation and characterization. We demonstrate herein that lightweight thermal models can be effectively used to predict microstructural changes with geometry. These models can in turn be used as precursors to developing geometry independent scan strategies and achieve microstructure control in various alloy systems. Even if the thermal signatures predicted by the model are not accurate, scan strategies can be developed to mimic the thermal conditions during initial process development. We present a case study on one of the most studied AM alloys: Ti-6Al-4V.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Effect of zeolite type, temperature, and pH on Stage III glass alteration behavior for two nuclear waste glasses

We report long-term laboratory scale static alteration tests (up to 1500 d) were conducted on two low-activity waste glasses (LAWA44 and IDF18-A161) at S/V = 2000 m –1 . Tests were seeded with either analcime, clinoptilolite, zeolite P1, or zeolite P2 to induce Stage III glass alteration behavior. The effect of several parameters on glass Stage III behavior was studied with consideration of several variables, including temperature (22 °C – 90 °C) and pH (floating or initially set using KOH at values from 9.5 to 11.5). Temporal solution data and solids characterization at the end of the experiments are reported. Solution data demonstrated the occurrence of a sustained rate acceleration at temperatures down to 40 °C and the activation energy for these Stage III rates was determined for both glasses. Three major secondary phases were identified at the end of the experiments for both glasses: zeolite P1, zeolite P2, and/or analcime (along with minor phases: zeolites, clays, carbonates). The identification of the crystalline phases at the end of the experiment often differed from the zeolite seed phase. In addition, the use of the Avrami equation showed unimpeded zeolite growth (3-dimensional) in certain conditions, suggesting that in certain conditions the glass dissolution rate is controlled by zeolite formation kinetics whereas in other conditions the glass corrosion process impeded zeolite formation kinetics. The morphological evolution of the samples revealed the growth of the zeolites which completely fill the intergranular space in the powder bed. These results are discussed with regards to previous seeded and unseeded Stage III dissolution rate experiments performed on low- and high-activity nuclear waste glasses.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Implications of post-processing induced microstructural changes on the deformation and fracture response of additively manufactured Ti–6Al–4V

Ti–6Al–4V parts fabricated via electron beam melting (EBM) powder bed fusion are often subjected to hot isostatic pressing below the β-transus temperature to mitigate defects. During which the pressure aids in pore closure and the thermal exposure results in coarsening of α phase while retaining the columnar prior-β phase grain morphology present in the as-fabricated condition. The same post-processing treatment can also be carried out above β-transus temperature which is an effective way to modify both the grain morphology and the associated α textures. Here, the objective of this work is to correlate thermally induced microstructural changes to the deformation and fracture response of the EBM processed Ti–6Al–4V. To this end, we have carried out both sub-transus and super-transus heat-treatments of the as-fabricated material. The mechanical response of the as-fabricated and all heat-treated materials are characterized by in-situ tensile tests under a high-resolution digital optical microscope. This enabled us to capture large-scale panoramic images of the deforming microstructure, and overcome the trade-off between the image resolution and the field of view during in-situ experiments. The series of images captured throughout the imposed deformation are subsequently used to perform microstructure-based digital image correlation to measure microstructural-scale strains over a large area. The results of the in-situ tests together with detailed fractographic analyses are then used to elucidate how the heterogeneous deformation spanning over multiple microstructural length-scales, for example, at the scale of lamellae, colonies of lamellae and grain boundaries, affect the overall deformation and fracture response of the post-processed materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

NaCo 2 (SeO 3 ) 2 (OH): competing magnetic ground states of a new sawtooth structure with 3d 7 Co 2+ ions

While certain magnetic sublattices have long been known theoretically to give rise to emergent physics via competing magnetic interactions and quantum effects, finding such configurations in real materials is often deeply challenging. Here we report the synthesis and characterization of a new such material, NaCo 2 (SeO 3 ) 2 (OH) which crystallizes with a highly frustrated sublattice of sawtooth Co 2+ chains. Single crystals of NaCo 2 (SeO 3 ) 2 (OH) were synthesized using a low-temperature hydrothermal method. X-ray single crystal structure analysis reveals that the material crystallizes in orthorhombic space group of Pnma (no. 62). Its crystal structure exhibits one-dimensional chains of corner-sharing isosceles triangles that are made of two crystallographically distinct 3d 7 Co 2+ sites (Co(1) and Co(2)). The chains run along the b-axis and are interconnected via [SeO 3 ] groups to form a three-dimensional structure mediating super-exchange interactions. The temperature dependent magnetization data show a ferromagnetic-like (FM) transition at 11 K (T 1 ) followed by an antiferromagnetic (AFM) transition at about 6 K (T 2 ). Neutron-powder diffraction measurements reveal that at T 1 = 11 K only the Co(2) site orders magnetically, forming ferromagnetic zigzag chains along the b-axis. Below T 2 = 6 K, both Co(1) and Co(2) sites order in a nearly orthogonal configuration, with Co(1) moments lying inside the plane of the sawtooth chain while Co(2) moments cant out of the plane. The canting of the magnetic moments leads to a net ferromagnetic component along b-axis, parallel to the chain direction. The ordered moments are fully compensated in the ac-plane. Inelastic neutron scattering measurements reveal crystal field excitations that are consistent with the presence of a spin–orbital entangled pseudo-spin state J eff = 1/2 for the Co 2+ ions. Low-energy spin-wave excitations are observed below the second magnetic transition. The analysis of powder excitation spectrum suggests complex exchange interactions that go beyond a Heisenberg Hamiltonian model with nearest neighbor couplings. Our results demonstrate the richness of the magnetic properties of sawtooth-type structures and encourage the study of similar structures with different oxyanion groups.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2005

Reactive Additives for Phenylethynyl-Containing Resins

Phenylethynyl-containing reactive additive (PERA) compounds and mixtures have been found to be useful for improving the processability of oligomers, polymers, co-oligomers, and copolymers that contain phenylethynyl groups. The additives can be incorporated in different forms: A solution of an amide acid or an imide of a PERA can be added to a solution of phenylethynyl-containing oligomer, polymer, co-oligomer, or copolymer; or An imide powder of a PERA can be mixed with a dry powder of a phenylethynyl-containing oligomer, polymer, co-oligomer, or copolymer. The effect of a given PERA on the processability and other properties of the resin system depends on whether the PERA is used in the amide acid or an imide form. With proper formulation, the PERA reduces the melt viscosity of the resin and thereby reduces the processing pressures needed to form the adhesive bonds, consolidate filled or unfilled moldings, or fabricate fiber-reinforced composite laminates. During thermal cure, a PERA reacts with itself as well as with the phenylethynyl-containing host resin and thereby becomes chemically incorporated into the resin system. The effects of the PERA on mechanical properties, relative to those of the host resin, depend on the amount of PERA used. Typically, the incorporation of the PERA results in (1) increases in the glass-transition temperature (Tg), modulus of elasticity, and parameters that characterize behavior under compression, and (2) greater retention of the aforementioned mechanical properties at elevated temperatures without (3) significant reduction of toughness or damage tolerance. Of the formulations tested thus far, the ones found to yield the best overall results were those for which the host resin was the amide acid form of a phenylethynyl-terminated imide (PETI) co-oligomer having a molecular weight of 5,000 g/mole [hence, designated PETI-5] and a PERA denoted as PERA-1. PETI-5 was made from 3,3',4'4'-biphenyltetracarboxylic dianhydride, 3,4'-oxydianiline (3,4'-ODA), 1,3-bis(3-aminophenoxy) benzene (1,3-APB), and 4-phenylethynylphthalic anhydride (PEPA). PERA-1 was made from 3,5-diamino- 4.-phenylethynylbenzophenon and equimolar amounts of phthalic anhydride and PEPA. To make PERA-1 in the imide form, the aforementioned ingredients were processed by refluxing in glacial acetic acid. To make the amide form of PERA-1, the ingredients were reacted in N-methyl-2-pyrrolidinone (NMP) under nitrogen at a temperature of 23 C (see figure). On the basis of the processability and other properties, a blend comprising 20 weight percent of PERA-1 and 80 weight percent PETI-5 was selected for further evaluation. Relative to neat PETI-5, the blend exhibited an increase in Tg; improved processability; and comparable values of shear strength in adhesion to titanium panels, open-hole compressive properties, compression properties after impact, and resistance to microcracking.

Connell, John W.↗
DOE OSTI2019

Synthesis and characterization of the novel antiferromagnet LaNiB 3 O 7

Here, we present the synthesis, structure, and magnetic properties of the novel borate LaNiB 3 O 7 - the first magnetically ordered compound reported in the CaAlB 3 O 7 structure type. This material is made of alternating sheets of corner-sharing borate tetrahedra and planes of La and Ni ions, with distorted nickel oxide [NiO 6 ] octahedra and lanthanum oxide [LaO 10 ] polyhedra. Temperature-dependent magnetic susceptibility data reveal dominantly antiferromagnetic interactions and an antiferromagnetic transition with a Neel temperature of 19 K, confirmed by specific heat data. The magnetic moment per nickel ion is 3.06 μ B . This compound uncovers a new family of rare-earth transition-metal borates to probe for magnetic interactions.

36 MATERIALS SCIENCE↗
NASA NTRS2010

Rapid Active Sampling Package

A field-deployable, battery-powered Rapid Active Sampling Package (RASP), originally designed for sampling strong materials during lunar and planetary missions, shows strong utility for terrestrial geological use. The technology is proving to be simple and effective for sampling and processing materials of strength. Although this originally was intended for planetary and lunar applications, the RASP is very useful as a powered hand tool for geologists and the mining industry to quickly sample and process rocks in the field on Earth. The RASP allows geologists to surgically acquire samples of rock for later laboratory analysis. This tool, roughly the size of a wrench, allows the user to cut away swaths of weathering rinds, revealing pristine rock surfaces for observation and subsequent sampling with the same tool. RASPing deeper (.3.5 cm) exposes single rock strata in-situ. Where a geologist fs hammer can only expose unweathered layers of rock, the RASP can do the same, and then has the added ability to capture and process samples into powder with particle sizes less than 150 microns, making it easier for XRD/XRF (x-ray diffraction/x-ray fluorescence). The tool uses a rotating rasp bit (or two counter-rotating bits) that resides inside or above the catch container. The container has an open slot to allow the bit to extend outside the container and to allow cuttings to enter and be caught. When the slot and rasp bit are in contact with a substrate, the bit is plunged into it in a matter of seconds to reach pristine rock. A user in the field may sample a rock multiple times at multiple depths in minutes, instead of having to cut out huge, heavy rock samples for transport back to a lab for analysis. Because of the speed and accuracy of the RASP, hundreds of samples can be taken in one day. RASP-acquired samples are small and easily carried. A user can characterize more area in less time than by using conventional methods. The field-deployable RASP used a Ni/Cad rechargeable battery. Power usage was less than 1 Wh/ cm3 even when sampling strong basalts, so many samples could be taken on a single battery charge.

Peters, Gregory↗
NASA NTRS2020

Mineralogy and Geochemistry of Sedimentary Rocks and Eolian Sediments in Gale Crater, Mars: A Review After Six Earth Years of Exploration with Curiosity

The Mars Science Laboratory Curiosity rover arrived at Mars in August 2012 with a primary goal of characterizing the habitability of ancient and modern environments. Curiosity was sent to Gale crater to study a sequence of ∼3.5 Ga old sedimentary rocks that, based on orbital visible and near- to short-wave infrared reflectance spectra, contain secondary minerals that suggest deposition and/or alteration in liquid water. The sedimentary sequence in the lower slopes of Mount Sharp in Gale crater preserves a dramatic shift on early Mars from a relatively warm and wet climate to a cold and dry climate, based on a transition from smectite-bearing strata to sulfate-bearing strata. The rover is equipped with instruments to examine the sedimentology and identify compositional changes in the stratigraphy. The Chemistry and Mineralogy (CheMin) instrument is one of two internal laboratories on Curiosity and includes a transmission X-ray diffractometer (XRD) and X-ray fluorescence (XRF) spectrometer. CheMin measures loose sediment samples scooped from the surface and drilled rock powders, and the XRD provides quantitative mineralogy to a detection limit of ∼1 wt.% for crystalline phases. Curiosity has traversed>20 km since landing and has primarily been exploring an ancient lake environment fed by streams and groundwater. Of the 19 drilled rock samples analyzed by CheMin as of sol 2300 (January 2019), 15 are from fluvio-lacustrine deposits that comprise the Bradbury and Murray formations. Most of these samples were drilled from units that did not have a clear mineralogical signature from orbit. Results from CheMin demonstrate an astounding diversity in the mineralogy of these rocks that signifies geochemical variations in source rocks, transportation mechanisms, and depositional and diagenetic fluids. Most detrital igneous minerals are basaltic, but the discovery in a few samples of abundant silicate minerals that usually crystallize from evolved magmas on Earth remains enigmatic. Trioctahedral smectite and magnetite at the base of the section may have formed from low-salinity pore waters with a circumneutral pH in lake sediments. A transition to dioctahedral smectite, hematite, and Ca-sulfate going up section suggests a change to more saline and oxidative aqueous conditions in the lake waters themselves and/or in diagenetic fluids. Perhaps one of the biggest mysteries revealed by CheMin is the high abundance of X-ray amorphous materials (15–73 wt.%) in all samples drilled or scooped to date. CheMin has analyzed three modern eolian sands, which have helped constrain sediment transport and mineral segregation across the active Bagnold Dune Field. Ancient eolian sandstones drilled from the Stimson formation differ from modern eolian sands in that they contain abundant magnetite but no olivine, suggesting that diagenetic processes led to the alteration of olivine to release Fe(II) and precipitate magnetite. Fracture-associated halos in the Stimson and the Murray formations are evidence for complex aqueous processes long after the streams and lakes vanished from Gale crater. The sedimentology and composition of the rocks analyzed by Curiosity demonstrate that habitable environments persisted intermittently on the surface or in the subsurface of Gale crater for perhaps more than a billion years.

E.B. Rampe↗
DOE OSTI2019

Propagation of Degradation-Induced Defects in Zeolitic Imidazolate Frameworks

Isolated defects induced by water and acid gases have been extensively characterized in ZIF-8, a prototypical metal–organic framework material, yet there is little understanding regarding how these single bond-breaking events lead to the structural amorphization observed after prolonged experimental exposure in acidic environments. We use density functional theory calculations to provide the first analysis of defect propagation in a zeolitic imidazolate framework (ZIF) material. Given a single bond-breaking event (the first step in the formation of any defect state), we exhaustively explore the energetics of subsequent defect states and find strong preference for additional bond-breaking located adjacent to the previous defect in both two-defect and three-defect systems. This series of favorable reaction energies is more exothermic when we replace water with sulfuric acid as a protonating agent, in agreement with experimental observations that ZIF-8 degradation is accelerated in humid acid gas environments. To offer initial insights into experimental signatures of defect propagation, we compare the simulated powder pattern in structures at varying levels of defect concentrations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1971

Improved plaque materials for aerospace nickel-cadmium cells

Improved cadmium electrode substrates with precisely controlled microstructures for possible use in aerospace nickel-cadmium cells were prepared. The preparative technique was a powder metallurgical process in which a fugitive pore-former and a nickel powder were blended, then isostatically compacted, and subsequently sintered. Cadmium electrodes prepared from such substrates were cycle tested using an accelerated tortuous test regime. It was discovered that plaques of 60% or 80% porosity prepared with a 25 micron pore-former were better than state-of-the-art electrodes in terms of efficienty and/or mechanical strength. The 60% structures were particularly outstanding in this respect in that they had efficiencies only 5-10 percentage points lower than state-of-the-art electrodes and vastly superior mechanical properties. This added strength was observed to eliminate cracking and physical degradation of the electrodes during processing and cycling. The cadmium electrodes prepared from the 80% porous substrates proved to be the best electrodes made during the course of the work from the point of view of highest efficiency. Three-point bend tests were used to measure mechanical properties of the plaques produced and also as a general characterization tool. In addition, the BET surface areas of selected specimens was determined. The SEM was used for judging microscopic uniformity and quantitatively determining the induced pore size and various other fine structures in the substrates. The technique of X-ray radiography was used to follow the bulk uniformity of the substrates at various stages of their processing.

Luksha, E.↗
DOE OSTI2021

Characterization of hot-pressed von Alpen type NASICON ceramic electrolytes

The Na-ion conducting solid electrolyte NASICON is a promising solid state electrolyte (SSE) for use in Na based electrochemical systems. The effects of particle morphology and synthesis of von Alpen type NASICON via hot-pressing were investigated. Spray dried particles were shown to improve mechanical and electrochemical properties. X-ray diffraction, scanning electron microscopy, impulse excitation measurements, Vickers hardness, and impedance spectroscopy were used to correlate relationships between phase purity, microstructure, mechanical properties, and electrochemical properties. Scanning electron microscopy showed the presence of a glass phase as between 19.08% and 28.23% area percentage and a ZrO 2 phase between 0.46% and 3.51% area percentage in the hot-pressed samples. Impulse excitation showed elastic modulus varying from 83.65 to 97.65 GPa. The first values of Poisson's ratio and shear modulus of NASICON are reported as between 0.23 and 0.26 and 33.87 to 38.79 GPa, respectively. Vickers hardness and fracture toughness measurements showed Vickers hardness ranging from 4.30 to 4.68 GPa and fracture toughness ranging from 1.05 to 1.09 MPa m ½ . Impedance spectroscopy showed grain conductivities ranging from 1.023 to 1.287 mS/cm, with grain boundary resistance percentages between 73.22 and 47.5%. Total conductivities ranged from 0.292 to 0.596 mS/cm, with 0.596 mS/cm being achieved at room temperature for the spray dried powders with lower grain boundary resistance percentages.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Evaluating the bond strength and fracture mechanisms of cold-sprayed zinc coating on AZ91 magnesium substrate via a combined experimental and computational approach

Magnesium (Mg) alloys are ideal candidates for automotive applications due to their high strength to weight ratio, castability, recyclability etc., however, they lack corrosion and oxidation resistance. Solid-state deposition techniques, such as cold spray, have been demonstrated to enhance their corrosion resistance as it relies on the severe plastic deformation of powder particles upon impact with the substrate to form a metallurgical bond with the substrate and within the coating. At cold sprayed interfaces, a heterogeneous microstructure is formed that includes some porosity, oxides and intermetallics which can significantly affect coating performance. Thus, establishing a direct correlation between the interface microstructure and its properties can aid in designing optimal cold spray parameters. In this study, we investigated the microstructure and mechanical properties of a zinc (Zn) coating deposited on a high pressure die cast (HPDC) AZ91 Mg substrate via high resolution scanning transmission electron microscopy, in situ micro-tensile testing, and finite element method (FEM) modeling. Micro-tensile pillars fabricated using the plasma focused ion beam (PFIB) successfully isolates the coating-substrate interface within the gauge length. The average bond strength of Zn-Mg interface was determined to be ∼140 MPa with failure occurring partially at the interface and mostly into the coatings. A detailed microstructural characterization revealed evidence of a strong metallurgical bonding at the Zn-Mg interface and formation of the C14 MgZn 2 laves phase interlayer resulting in a mixed mode of fracture during the micro-tensile experiments. FEM modeling reveals the stress distribution along the interfaces and suggests that a MgZn 2 layer thickness between 200–400 nm is optimum to increase the bond strength and minimize the triaxiality. Such a site-specific interfacial analysis with correlative computational modeling provides crucial insight into the overall performance of cold spray interfaces.

Bond strength↗
DOE OSTI2026

Linking microstructure to creep behavior in vertically and horizontally built LPBF Haynes 282 compared with wrought material via θ -projection

Laser Powder Bed Fusion (LPBF) has emerged as a promising route for fabricating intricate geometries in high-performance alloys. Haynes 282 (H282) is a strong candidate for applications such as heat exchangers or engines due to its excellent creep strength and thermal stability; however, the long-term creep behavior of LPBF-processed H282 remains poorly understood. In this study, the θ -projection method is used to analyze and extrapolate the creep behavior of vertically built LPBF, horizontally built LPBF, compared to wrought H282 tested at 816 °C. Vertically built LPBF H282 exhibits the lowest minimum creep rate (MCR), while the horizontally built condition shows a higher MCR comparable to that of wrought H282. Despite these differences, both LPBF conditions exhibit significantly shorter rupture life and reduced rupture strain than the wrought material, with the most severe degradation observed in the horizontal builds, consistent with an earlier onset of tertiary creep and accelerated strain-rate evolution. Microstructural characterization reveals that both LPBF and wrought H282 exhibit abundant twin-related boundary character; however, their grain boundary topologies differ markedly. The wrought alloy contains a higher fraction of low-angle grain boundaries and continuous twin lamellae, whereas the LPBF microstructure is characterized by a suppressed low-angle boundary population and fragmented twin-related boundaries embedded within irregular high-angle grain boundary networks. Fractographic analysis further reveals predominantly intergranular cracking in LPBF H282, accompanied by grain-boundary-decorated carbides, Al 2 O 3 inclusions, and high-aspect-ratio pores. These results demonstrate that grain boundary topology, rather than minimum creep rate alone, plays a critical role in governing creep damage accumulation and rupture behavior in LPBF and wrought H282.

Creep↗
DOE OSTI2023

Reactive flash sintering of TiZrN and TiAlN ternary metal nitrides

Here, this study demonstrated the reactive flash sintering (RFS) for two powder mixtures: TiN-ZrN (both conducting) and AlN-TiN (TiN conducting but AlN insulating), targeting ternary metal nitrides (TMN) of Ti 0.5 Zr 0.5 N and Ti 0.5 Al 0.5 N, respectively. A constant volage and pressure (e.g., 8 V DC, ∼15 MPa) at room temperature triggered the flash (current density up to 27 A/mm 2 ) without pre-heating, and the entire RFS process finished in a few minutes. For TiZrN, the flash was instantaneous whereas for TiAlN, there was a long incubation before the flash followed by a quick and dramatic flash. Both conventional ex situ XRD and in situ synchrotron study had been carried out. They showed a uniform Ti 0.57 Zr 0.43 N solution formed in RFS and persisted upon cooling, while (Ti, Al) N solid solution formed at high temperature was not stable and likely went through a very quick phase separation in the cooling process. The final products from RFS had been characterized using SEM/EDS for microstructure. Both TiZrN and TiAlN were dense. Distribution of Ti, Zr, and N was uniform for TiZrN; for TiAlN, Ti and N distribution was uniform, while association of Al with oxygen was observed. TGA-DSC revealed the onset oxidation temperature for TiZrN was comparable to TiN and ZrN, while it was higher by ∼200 °C for TiAlN, likely due to the formation of Al 2 O 3 . In terms of mechanical properties such as hardness or fracture toughness, forming a single-phase solid solution (like TiZrN) does not offer obvious benefits. while large grain size from RFS seemed to be unfavorable. Future optimization of RFS condition and in-depth study by both experiments and simulation are needed to fully understand the composition-processing-structure-property relationships for such TMN from the reactive flash sintering process.

Flash Sintering↗
DOE OSTI2024

Computer vision models and advanced TEM imaging for microstructures of irradiated AM316 stainless steels

Advancements were made in automating microscopy-based material characterization, particularly in studying irradiation effects on additively manufactured (AM) materials using machine learning (ML) and computer vision (CV). These automation efforts address the challenges of analyzing complex microstructures, accelerating the detection of irradiation-induced defects. Two CV models were developed at Argonne National Laboratory (ANL) to enhance transmission electron microscopy (TEM) analysis of irradiated AM 316 stainless steel. The first model focused on the detection of irradiation-induced dislocation loops, which contribute to material hardening and embrittlement. These loops, categorized as faulted or perfect, were automatically detected and classified using a Mask R-CNN model trained on TEM images from both in-situ and ex-situ ion irradiation experiments. The model achieved high accuracy, with precision, recall, and F1 scores of 0.839, 0.734, and 0.776, respectively, demonstrating its effectiveness in analyzing dislocation loops in irradiated AM materials. The second CV model was developed to analyze the size and wall thickness of dislocation cells in laser powder bed fusion (LPBF) 316 stainless steel. Using a U-Net++ architecture with EfficientNet as the encoder, the model was trained on TEM images to segment and measure cell size and wall thickness.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Nanocrystalline ZrN thin film development via atomic layer deposition for U-Mo powder

Zirconium nitride (ZrN) thin film deposited via thermal atomic layer deposition (ALD) has been recently chosen as a candidate technology for application of a diffusion barrier coating on the low enriched uranium alloy powder considered in the NNSA research reactor conversion program. Reported here is the first instance of using ALD for coating actinide materials. For this study, a modified ALD system was constructed to produce one micron thick zirconium nitride (ZrN) coating over spherical particulate of natural uranium-molybdenum (U-Mo) based fuel. The ALD system was designed to have a rotating drum system, with provisions for facilitating sequential exposures of chemicals such as tetrakis dimethyl amido zirconium (TDMAZr) and ammonia (NH 3 ) in order to deposit ZrN. The ALD system was successful in developing a highly conformal ZrN coating covering every individual U-7Mo particle. This article describes the ZrN film synthesis details and reports the produced microstructure and composition of the ALD ZrN as deposited on fuel particulates. The as-fabricated coating was determined to have a nanocrystalline structure in the cubic-ZrN (cF8) phase. It exhibited a dense microstructure with adequate interfacial bonding. TEM-EELS characterization demonstrated that the coating contains a very low amount of oxygen impurity. To understand the potential microstructural evolution for ALD ZrN during reactor operation, an in-situ heavy ion (Kr) irradiation experiment was performed at the IVEM-Tandem facility. A total fluence of 7.5 x 10 15 ions/cm 2 (similar to 10 dpa) was achieved, and apart from minor grain coarsening in the ALD ZrN coating, no significant radiation effects were observed.

36 MATERIALS SCIENCE↗