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DOE OSTI2020

Structural integrity of additively manufactured stainless steel with cold sprayed barrier coating under combined cyclic loading

Integration of metal additive manufacturing (AM) and cold spray (CS) technologies provide an unprecedented opportunity to manufacture coated material systems with complex geometrical features. The application of these material systems in functionally critical components requires adequate structural integrity, particularly in the presence of cyclic loading. This article researches the multiaxial fatigue (axial-torsional cyclic loading) behavior of a coated material system consisting of 15Cr-5Ni precipitation-hardening stainless steel (15-5 PH SS) substrate additively manufactured by direct metal laser sintering with a layer of chromium carbide nickel (CrC-Ni) barrier coating deposited by CS. The influence of AM and CS-induced residual stresses on fatigue performance of test specimens was thoroughly studied. Additionally, the effect of surface roughness and processes induced defects were considered to explain the crack growth mechanism. Stresses assessed by synchrotron X-ray diffraction indicated a substantial accumulation of residual stresses, particularly in the outer surface of the as-fabricated 155 PH SS specimens. The state of residual stress was changed notably following the deposition of CrC-Ni coating in the axial, hoop, and radial directions of the fatigue test specimen. Also, CS deposition of CrC-Ni coating caused significant improvement in the surface quality of the additively manufactured components. Fatigue test results indicated, CS deposition of CrC-Ni substantially enhances the fatigue life of the AM-produced 15-5 PH SS substrate in all loading conditions, particularly in the high cycle fatigue regime. The improvement in the fatigue life of the specimens with coating was associated with a reduction in equivalent residual stress at the substrate surface and improvement in the specimens' surface condition (i.e., reduced surface roughness). The fractographic analysis of the specimen indicated the cracks tend to initiate in the surface of both as-fabricated and cold-sprayed specimens. However, the mechanism of crack growth changed notably following the deposition of CrC-Ni coating. The cracks tended to propagate in the planes parallel or with a small deviation from the build layers of the AM-produced specimens. On the other hand, deposition of CrC-Ni coating increased the deviation of crack growth plane from the build layers of the substrate.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Influence of Spatter on Porosity, Microstructure, and Corrosion of Additively Manufactured Stainless Steel Printed Using Different Island Size

Specimens of 316 L stainless steel were printed using laser powder bed fusion (LPBF), a popular metal additive manufacturing (AM) technique, with varying island sizes. Not many researchers have considered the impact of spatter while optimizing LPBF printing parameters. In this research, the influence of spatter was considered while also investigating the effect of varied island size on the microstructure, surface roughness, microhardness, and corrosion resistance of LPBF-316 L. No correlation was observed between surface roughness or microhardness and minor variations in island size. However, a correlation was drawn between varied island sizes and porosity in LPBF-316 L. The specimens associated with larger island sizes showed significantly enhanced corrosion resistance due to fewer manufacturing defects and reduced porosity, attributed to the minimal influence of the spatter. Based on analysis, the LPBF parameters were revised, which lead to superior corrosion resistance of LPBF-316 L, attributed to high density and reduced porosity.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Foams in Hohlraums

Foam materials are starting to find application in laser-heated hohlraums used to drive inertial confinement fusion (ICF) implosions. The disparate scales of the solid foam elements (nm) compared to the typical problem scale (mm) make it expensive to resolve the individual foam elements in hydrodynamic calculations. In this project we developed two new models for treating foam materials – a 3D hydrodynamic model that treats the foam as bits of pre-expanded solid material separated by voids, and a subgrid model that captures the essential physics of laser-heated foams without requiring resolution of the individual solid elements. We also explored the microphysics of the transition from interpenetrating kinetic behavior to fully-collisional fluid-like behavior during the early time heating and expansion of foam elements through a combination of single-fluid and multi-fluid hydrodynamics calculations and particle-in-cell calculations. The model was benchmarked against these calculations and against experimental data on laser-heated chemical and additive-manufactured (AM) foams. Since there was no existing data on laser-heated AM foams, we performed the first experiments on such foams at the Jupiter Laser Facility. Samples of three different types of printed AM foams were heated using a single 0.5 micron laser. The foam densities ranged from 10 to 100 mg/cc (supercritical for 0.5 micron light). We measured the backscattered light (power and spectrum), the transmitted light, and the time-integrated temperature of the foam samples. This benchmarked subgrid foam model is a new capability that should allow routine calculation of ICF designs using foam elements, potentially opening up a new design space.

36 MATERIALS SCIENCE↗

NASA NTRS2019

Laser Sintering of Thermoset Polyimide Composites

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the CAD model. SLS generally uses thermoplastic polymeric powders, such as polyamides (i.e. Nylon), and the resultant 3D objects are often weaker in their strength compared to traditionally processed materials, due to the lack of polymer inter-chain connection in the z-direction. Our previous effort showed the challenges of printing a melt-processable RTM370 imide resin powder terminated with reactive 4-phenylethynylphthalic anhydride by LS, due to its inherently low viscosity of these oligomers. This paper presented the first successful 3D printing of high temperature carbon fiber filled thermoset polyimide composites, followed by post cure cycles to promote additional crosslinking for achieving higher temperature (Tg = 370 °C) capability. The processes to build tensile specimens and a component by LS, and the characterization of RTM370 imide resin by DSC and rheology as well as evaluation of the LS printed polyimide composite specimens by SEM and mechanical tests will be discussed.

Polyimide Composites↗

DOE OSTI2024

Environmental Degradation in Advanced Reactor Environments

The Advanced Materials and Manufacturing Technologies (AMMT) program operating under the Department of Energy Office of Nuclear Energy is accelerating the qualification and deployment of additively manufactured materials in advanced reactor environments. Laser powder bed fusion (LPBF) has emerged as a promising additive manufacturing technique to fabricate complex components with the potential of tailored material properties. In the nuclear industry, metal additive manufacturing can offer numerous advantages, such as reduced lead times, streamlined quality assurance, and cost-effective low-volume production of new and replacement components with conventional or novel materials and geometries. The rapid and effective qualification of the effect of processing variability on the performance and degradation of additively manufactured materials is essential for the deployment of these components into advanced reactor environments. This talk presents an overview of the Environmental Effects area activities within AMMT. AMMT is performing irradiation and corrosion testing of several materials built by LPBF, including 316L and 316H stainless steels. Our irradiation efforts encompass neutron irradiation testing and ion irradiation testing to provide a robust technical basis for understanding the effect of process variability on materials degradation. We develop focused irradiation test plans that align well with risk-informed and technologically inclusive approaches to licensing. We will also discuss our plans and specific concerns for corrosion testing additively manufactured material, with a primary focus on molten salt and liquid sodium environments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRSDate not supplied

Experimental Characterization of Additively Manufactured Nickel-Titanium Shape Memory Alloy Heat Pipes

Shape memory alloys (SMA) have been identified for use in spacecraft components as replacement for conventional deployment mechanisms. They may be used in thermal management components such as radiators to create self-deploying radiators. One SMA, NiTi, has also been developed for additive manufacturing processes. Heat pipes are a common way to create highly effective and lightweight spaceflight radiators, and heat pipes can also be made from NiTi and related alloys. The wick is the critical element of a functioning heat pipe, and recent progress over the past years has led to the development of additively manufactured heat pipe wicks in various materials. The combination of these efforts is the focus of this project: creating an additively manufactured, shape memory alloy self-deploying heat pipe radiator. This paper will focus on the experimental characterization of these additively manufactured NiTi heat pipes. The heat pipe coupons were additively manufactured by direct metal laser sintering (DMLS), with an integral liquid cooled condenser. Heat is input to the heat pipe via a thin film heater. Thermocouples were spot welded to the heat pipes to measure temperature at several axial locations. The heat pipes were tested with two working fluids: water and ethanol. Ethanol is not an ideal working fluid for heat pipes but is useful in characterizing them because it wets well to a wide variety of surfaces. Water is in general a superior working fluid for heat pipes, but its contact angle and therefore wicking performance strongly depends on the surface chemistry of the surface it is in contact with. A particular measurement of interest in this test is the evaporator to condenser thermal conductance, which will be compared in the full paper to recently published correlations for additively manufactured heat pipes. Experimental results for two straight geometry and one bellows geometry heat pipe will be presented. The bellows geometry is of interest for condenser of the self-deploying radiator design.

Additive manufacturing↗

DOE OSTI2025

Corrosion of Wrought and LPBF 316H in Molten Eutectic Na-Mg Chloride Salt

This presentation shows experimental work at INL evaluating the corrosion behavior of wrought and laser powder bed fusion (LPBF) 316H stainless steel (SS) in chloride molten salt systems. This evaluation focuses on understanding the relationship between the material’s as-built characteristics and its corrosion performance, the effects of acid cleaning and descaling before corrosion.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2013

Comparison of Raindrop Size Distribution Measurements by Collocated Disdrometers

An impact-type Joss-Waldvogel disdrometer (JWD), a two-dimensional video disdrometer (2DVD), and a laser optical OTT Particle Size and Velocity (PARSIVEL) disdrometer (PD) were used to measure the raindrop size distribution (DSD) over a 6-month period in Huntsville, Alabama. Comparisons indicate event rain totals for all three disdrometers that were in reasonable agreement with a reference rain gauge. In a relative sense, hourly composite DSDs revealed that the JWD was more sensitive to small drops (,1 mm), while the PD appeared to severely underestimate small drops less than 0.76mm in diameter. The JWD and 2DVD measured comparable number concentrations of midsize drops (1-3mm) and large drops (3-5 mm), while the PD tended to measure relatively higher drop concentrations at sizes larger than 2.44mm in diameter. This concentration disparity tended to occur when hourly rain rates and drop counts exceeded 2.5mm/h and 400/min, respectively. Based on interactions with the PD manufacturer, the partially inhomogeneous laser beam is considered the cause of the PD drop count overestimation. PD drop fall speeds followed the expected terminal fall speed relationship quite well, while the 2DVD occasionally measured slower drops for diameters larger than 2.4mm, coinciding with events where wind speeds were greater than 4m/s. The underestimation of small drops by the PD had a pronounced effect on the intercept and shape of parameters of gamma-fitted DSDs, while the overestimation of midsize and larger drops resulted in higher mean values for PD integral rain parameters

disdrometers↗

NASA NTRSDate not supplied

Ignition of Metals in Heated Supersonic Particle Impact with Inert Particulate

The conventional understanding of particle impact ignition characteristic elements relies on the following principles: 1) flammable particulate (except in the case of titanium and aluminum target materials); 2) gas velocity greater than 100 ft/s; 3) Impact point ranging from 45° to perpendicular to the path of the particle [1]; 4) flammable target material. To test assumptions about particulate flammability being necessary for particle impact ignition of less reactive target materials, such as Inconel 718, testing was performed with inert particulate. Supersonic particle impact testing was conducted with heated gas and 1500-µm sapphire particulate on various target materials: 304 stainless steel, wrought and selective laser melted Inconel 718, and Monel 400. Posttest characterization of impact craters was performed on each type of metallic target sample, including surface characterization performed by light optical microscopy and scanning electron microscopy with energy dispersive spectroscopy. Full consumption of the stainless steel and wrought Inconel 718 targets were noted to occur with sequential impacts. The results of testing will be discussed in detail, as well as recommendations for updating the understanding of the particle impact ignition mechanism.

Particle Impact↗

DOE OSTI2025

Laser powder bed fusion of ODS Fe–Cr–Al (0.3Zr, 0.3Y 2 O 3 ): Unveiling processing-microstructure- mechanical property relationships

Here, this study investigates the fabrication of oxide dispersion strengthened (ODS) Fe-Cr-Al alloys via laser powder bed fusion (LPBF) with strategic additions of 0.3 wt% Zr and 0.3 wt% Y 2 O 3 for enhanced mechanical performance in nuclear applications. Systematic processing parameter optimization yielded three distinct conditions: one low-density product with significant defects and two near-full-density materials with improved consolidation. Comprehensive characterization confirmed single-phase α-ferrite matrix formation with successful incorporation of Y-, Zr-, O-, and C-rich precipitates characteristic of ODS alloys. However, precipitate density remained low (∼10 7 cm −3 ), resulting in sink strength values substantially below optimal levels for radiation resistance. Microhardness values (mid-200s HV) correlated inversely with grain size following the Hall-Petch relationship, indicating grain boundary strengthening as the dominant mechanism rather than precipitation strengthening. The optimized processing conditions achieved excellent mechanical properties with room temperature yield strength of approximately 500 MPa and 30 % elongation, demonstrating superior strength-ductility synergy compared to other additively manufactured ODS materials and performance consistent with literature values for LPBF-processed ODS-FeCrAl alloys. This investigation reveals both the potential and limitations of LPBF processing for ODS Fe-Cr-Al alloys. While successful defect-free fabrication was achieved, results highlight the critical need for systematic optimization of processing parameters and post-processing heat treatments to enhance precipitate density for effective dispersion strengthening and radiation resistance while maintaining additive manufacturing advantages.

Additive manufacturing↗

DOE OSTI2020

Deposit geometry and oxygen concentration spatial variations due to composition change in printed functionally graded components

Functionally graded materials (FGMs) with site specific chemical composition are commonly manufactured by directed energy deposition (DED). Although previous work fabricated an FGM with a compositional variation between a ferritic and austenitic alloy, difficulties arose due to variations in deposit shape with composition change. This problem also occurs for FGMs in literature; however, unlike other cases, the thermophysical properties of these two alloys were similar throughout the build. Here, we investigate the role of chemical composition and surface-active elements on deposit geometry during the manufacture of FGMs by laser DED. Single-track experiments for the relevant FGM compositions are analyzed with results from a well-tested, three-dimensional, transient numerical heat transfer and fluid flow model and thermodynamic calculations. Experiments showed deposit shape varied as a function of composition for constant laser power and scan speed. Thermodynamic analysis indicated that the oxygen solubility in the fusion zone varied significantly for each composition used for the FGM. Numerical modeling revealed that the change in fluid flow caused by Marangoni convection due to dissolved oxygen in the fusion zone were mainly responsible for the changes in deposit shape observed in experiments. Finally, because oxygen can be introduced into the fusion zone through the feedstock as well as the surrounding atmosphere, these findings elucidate a previously unconsidered aspect of process control during DED fabrication of FGMs.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Development of Large-Scale Thrust Chambers using Laser Powder Directed Energy Deposition

Historical manufacturing methods for liquid propulsion combustion chambers have relied on series of tube-walls or slotted channel walls (subsequently brazed or plated) for regenerative cooling paths. Large-scale additive manufacturing techniques offer strong potential to minimize manufacturing lead times and cost for developing liquid propulsion chambers, while maintaining performance metrics of traditionally manufactured hardware. The benefits expand beyond traditional combustion chambers to lesser considered nuclear thermal propulsion chambers where radiation energizes the singular incoming propellant stream instead of an exothermic chemical reaction. While each subset of liquid propulsion chambers reaps similar benefit, the geometric challenges in each design can vary substantially. This manuscript discusses the challenges of large contraction ratio propulsion chambers, bimetallic liners and closeout jackets, and material selection when considering laser powder directed energy deposition. LP-DED presently offers build volumes unattainable by L-PBF systems, required for large diameter thrust chambers. LP-DED typically has faster deposition time and is capable of overhang angles without support material (due to the ability to tilt the build plate and minimize the actual build angle). These benefits come at the cost of feature resolution. Designers and manufacturers should consider the effects of thick-wall features printed parallel to the primary surface versus perpendicular due to distortion. Thick-wall and thin-wall features printed in the same plane can substantially increase build time. Where large-scale L-PBF overlaps in size, there may be limited benefit in the quantity of powder required for the build due to the low capture rate of LP-DED and a case-by-case examination is required.

LP-DED↗

NASA NTRSDate not supplied

A Comparison of Microstructure and Mechanical Performance of Inconel 718 Manufactured via L-PBF, LP-DED, and WAAM Technologies

The microstructure and mechanical properties of additively manufactured (AM) alloys can be significantly affected by variations in cooling rates, resulting from different process conditions across different additive manufacturing (AM) platforms. Therefore, it is crucial to understand the effect of manufacturing process on the microstructure and mechanical properties of AM Inconel 718. This study examines three AM processes: laser powder bed fusion, laser powder directed energy deposition, and wire arc additive manufacturing. Results show that fully heat treated laser powder bed fused (L-PBF) and wire arc additively manufactured (WAAM) Inconel 718 specimens exhibit higher strength compared to laser powder directed energy deposited (LP-DED) ones due to finer grain structure in L-PBF and retained dendritic microstructure in WAAM. The ductility in LP-DED Inconel 718 was slightly higher compared to WAAM and L-PBF due to relatively small carbide size, which causes stress concentration in a small material volume, leading to delayed fracture.

Additive manufacturing (AM)↗

NASA NTRS2017

Relationship of Powder Feedstock Variability to Microstructure and Defects in Selective Laser Melted Alloy 718

Powder-bed additive manufacturing processes use fine powders to build parts layer by layer. For selective laser melted (SLM) Alloy 718, the powders that are available off-the-shelf are in the 10-45 or 15-45 micron size range. A comprehensive investigation of sixteen powders from these typical ranges and two off-nominal-sized powders is underway to gain insight into the impact of feedstock on processing, durability and performance of 718 SLM space-flight hardware. This talk emphasizes an aspect of this work: the impact of powder variability on the microstructure and defects observed in the as-fabricated and full heated material, where lab-scale components were built using vendor recommended parameters. These typical powders exhibit variation in composition, percentage of fines, roughness, morphology and particle size distribution. How these differences relate to the melt-pool size, porosity, grain structure, precipitate distributions, and inclusion content will be presented and discussed in context of build quality and powder acceptance.

Characterization↗

DOE OSTI2025

PowderJet: Spherical metal powder production via multi-orifice droplet-on-demand metal jetting

Leading metal additive manufacturing techniques, such as laser powder bed fusion and directed energy deposition, rely on high-quality spherical metal powders. However, traditional powder production methods like gas atomization face limitations, including low in-spec yield, asphericity, and internal porosity. We introduce PowderJet, a powder production platform that uses electromagnetic pulses to eject liquid metal droplets from a multi-orifice nozzle. Unlike stochastic methods, PowderJet tightly controls powder size, distribution, and purity through a droplet-on-demand approach. We detail the system’s design, operation, and performance using a combined experimental and computational fluid dynamics (CFD) framework. Initial results with Al4008 and Cu110 alloys demonstrate successful production, yielding unsieved aluminum powder batches with a mean diameter of 200 µm and a narrow size distribution (15 µm standard deviation). The produced powders are highly spherical, achieving a roundness > 0.95. PowderJet operates with a small melt volume (3 mL) and supports continuous refilling, enabling production rates between 30 and 140 cm³/hr depending on jetting frequency, number of orifices and particle size. CFD simulations show that future systems could achieve rates exceeding 1000 cm³/hr for particle sizes as small as 40 µm. PowderJet’s high yield of in-spec powder makes it ideal for producing precious or hazardous materials that are inefficient to manufacture using conventional methods. This platform offers a scalable, precise, and efficient solution for producing high-quality powders tailored for advanced manufacturing applications.

Atomization↗

DOE OSTI2023

On the strength and fracture toughness of an additive manufactured CrCoNi medium-entropy alloy

An additively manufactured (nominally equiatomic) CrCoNi alloy was processed by laser powder bed fusion (LPBF). At ambient temperatures (298 K), this medium-entropy alloy displayed a yield strength, σ y of ~691 ± 9 MPa, and an ultimate tensile strength, σ u of ~926 ± 15.2 MPa; at cryogenic temperatures (77 K), yield and tensile strengths increased respectively to σ y ~ 944 ± 6 MPa and σ u ~ 1382 ± 11 MPa. These strength levels are 57 and 44% higher than that of the wrought alloy, due to strengthening from the solidification cellular structures intertwined with dislocations in the LPBF CrCoNi. The crack-initiation fracture toughness, K JIc was measured to be ~183.7 ± 28 MPa√m at 298 K; this value marginally decreased by ~4% to ~176 ± 11 MPa√m at 77 K. These K JIc values of the LPBF CrCoNi were 11% and 35% lower than the wrought CrCoNi alloy at 298 K and 77 K, respectively. Here, the resistance to crack growth of the LPBF CrCoNi from its hierarchical micro- and meso-structures was evaluated using nonlinear-elastic fracture mechanics by measuring R-curve behavior in the form of the J-integral as a function of crack extension. The specific features of the hierarchical microstructures at different length-scales provide a basis for the strengthening and toughening properties of this additively manufactured medium-entropy alloy. This correlation between the deformation and the hierarchical microstructures at different length-scales may provide future guidance for improving the fracture toughness properties of medium-entropy alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Microstructure effects on fatigue crack growth in additively manufactured Ti–6Al–4V

In this article we investigate the relationship between the different microstructural features in additively-manufactured (AM) Direct Metal Laser Deposited Ti–6Al–4V alloys and the observed fatigue and fracture behaviors, using high resolution Digital Image Correlation experiments and microstructural imaging. Fatigue cracks in the AM specimens were observed to periodically propagate parallel to the α' laths and deflect at prior β grain boundaries. Corresponding plastic strain distributions show needle-like regions of high strain that correlated to the α' laths, suggesting significant influence of the microstructure on the plastic zone. In many cases, the fatigue cracks also propagated towards voids from unsintered powder or gas entrapment in the vicinity. In several experiments, premature failure of the AM specimens occurred under monotonic fracture or cyclic fatigue loading, which we attribute to the presence of void clusters located near the crack-tip. These fatigue and fracture characteristics were similar for AM specimens of different build-orientations.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Development of Laser Powder Bed Fusion NASA HR-2 for Hydrogen Sensitive Liquid Rocket Engine Applications

The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. AM has provided new design and manufacturing opportunities to reduce cost and schedule, consolidate parts, and optimize performance. Laser Powder Bed Fusion (L-PBF) is one of the most commonly used AM processes to fabricate components that have complex shape and need fine feature resolution. Due to exposure to high pressure gaseous hydrogen, mechanical property degradation caused by hydrogen environment embrittlement (HEE) is a critical concern for many materials in liquid hydrogen propulsion systems. NASA has identified the need to develop and advance new materials in unique engine applications using liquid hydrogen as a propellant. One such material being developed at NASA Marshall Space Flight Center is L-PBF NASA HR-2 (Hydrogen Resistant-2), a high-strength Fe-Ni-based superalloy resistant to HEE. The chemistry of NASA HR-2 was formulated to meet requirements for key liquid rocket engine (LRE) components that operate in high-pressure hydrogen environments. Initial development and material characterization found NASA HR-2 has excellent L-PBF printability and its microstructure evolves well after heat treatment. This new alloy has undergone fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing across a range of temperatures. Tensile testing was performed in pressurized gaseous hydrogen (GH2) environment to assess its resistance to HEE. L-PBF NASA HR-2 has an average yield stress of 95 ksi, ultimate tensile stress of 165 ksi, and very high fracture elongation at 34 - 36% when tested in a 5 ksi high pressure hydrogen environment. The tensile property data confirms hydrogen has little influence on its ductility, strength, and fracture behavior. L-PBF NASA HR-2 is a promising option for many hydrogen sensitive LRE components that require exceptional resistance to HEE. The development of L-PBF NASA HR-2 is funded under the grants provided by Jacobs TIPI program and the Liquid Engine Office at NASA Marshall Space Flight Center. This paper will provide an overview of the L-PBF process development, material characterization, mechanical and thermophysical properties, and LRE hardware development for NASA HR-2.

NASA HR-2↗