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Impact of Powder Supply Variation on Mechanical Properties for Additive Manufacture of Alloy 718

The Additive Manufacturing Structural Integrity Initiative (AMSII) examined how a number of different Alloy 718 powder lots can create variation in microstructure and mechanical properties in parts fabricated using Laser Powder Bed Fusion. Being a common alloy, Alloy 718 powder can be found in a variety of compositions, fabrication techniques, and powder size distribution. Sixteen virgin powders, and three recycled powders were used to build samples for microstructure analysis, fatigue and tensile testing. The major impacts of the different powders manifested in variations in the microstructure, such as minor phases and grain size variation. There were corresponding variations in mechanical properties. A down-selection of powders were chosen for additional analysis, and a powder recyclability study was completed to look at the effect of reused powder.

Alloy 718↗

M2 Selective Laser Melting GRCop-42 Recycling Study

A powder recycling study was conducted to examine the effects of powder reuse on physical and mechanical properties of SLM GRCop-42. Twelve sequential builds were conducted, each reusing powder from the previous build topped off with virgin powder to fill the powder chamber. Powder morphology, particle size distribution, flowability, and chemistry were examined for each subsequent build, along with the mechanical properties of tensile and LCF specimens built with each powder batch. It was found that only powder flowability demonstrated a trend with increasing reuse, with flowability and cohesiveness generally decreasing over the course of the 12 builds. Minor variation in powder chemistry was observed throughout the study, however, the variations did not correlate with increasing powder reuse

Additive Manufacturing↗

Impact of Powder Variability on the Microstructure and Mechanical Behavior of Selective Laser Melted Alloy 718

Powder-bed additive manufacturing processes use fine powders to build parts layer-by-layer. Alloy 718 powder feedstocks for selective laser melting (SLM) additive manufacturing are produced commercially by both gas and rotary atomization and are available typically in the 10-45 or 15-45 microns size ranges. A comprehensive investigation was conducted to understand the impact of powder variability on the microstructure and mechanical behavior of SLM 718 heat treated to Aerospace Material Specification (AMS) 5664. This study included sixteen virgin powders and three once-recycled powders within the 10-45 and 15-45 microns size ranges that were obtained from seven direct source suppliers and one reseller. Although alike as highly regular spheroids, these powders showed distinct differences in composition (especially Al, C and N contents), particle size distributions, and powder features such as degree of agglomeration, fusion and surface roughness. Compositional differences expectedly had the strongest impact on microstructure. High N and C contents formed TiN-nitrides and/or (Nb,Ti,Mo)-C carbides on the grain boundaries, prevented recrystallization during heat treatment, and resulted in retained (001)-scalloped shaped grains that ranged from 19 to 41 microns in average size. In the absence of this particle pinning, the average grain size of the heat treated SLM 718 ranged from 51 microns to 90 microns. Room temperature tensile and high cycle fatigue (HCF) testing compared as-fabricated (AF) and low stress ground (LSG) surface conditions. Tensile testing revealed consistent behavior between the two surface conditions and amongst the powder lots. The finer grained SLM 718 builds displayed the lowest tensile properties. A SLM 718 build fabricated from a powder with eight times lower C content showed statistically better tensile properties presumably due to enhanced coarsening of (delta)-Ni3Nb precipitates. The specimens from once-recycled powders had slightly higher tensile strengths and slightly higher ductility compared to their virgin equivalents; once-recycling also did not substantially degrade the mean HCF life. The LSG fatigue lives agreed with conventionally manufactured 718 data, while AF lives exhibited a knock-down due to surface roughness. The fatigue lives of AF specimens were statistically equivalent across powder lots except for one and failures typically initiated at stress concentrators associated with SLM surface asperities. Fatigue testing of low stress ground specimens result in both transgranular and within facet crack initiations. More than half of the cracks initiated from these facets for the machined condition; however, these facets appeared to be within grains that were larger-than-average in size. A nitrogen-atomized powder with fine prior particles of TiN-nitrides and M(Ti,Nb,Mo)C carbides from atomization on powder surfaces resulted in the best fatigue performance with segregation of these particles to the SLM 718 grain boundaries leading to higher resistance to early-stage crack propagation. Typically the fine-grained builds with minor phases along the grain boundaries did not perform well in fatigue, whereas a larger-grain build with lower carbon content and coarser delta-Ni3Nb precipitates showed the next best HCF response. Further details of the build microstructure and its impact on tensile and fatigue behavior was considered.

laser deposition↗

Open-source Numerical Modeling of Solidification Cracking Susceptibility: Application to Refractory Alloy Systems

Introduction. Alloys such as aluminum, nickel-base, and austenitic stainless steels are susceptible to solidification cracking during welding and 3D printing. Compositional optimization is one method used to effectively mitigate solidification cracking of those alloy systems. With the surge in hypersonic and in-space propulsion activities, refractory metals (Nb, Mo, Ta, W, and Re) and their alloy derivatives are increasing in importance due to their extreme high melting point and retention of high-temperature strength; however, their chemistry was most typically optimized to promote ductility during mechanical operations such as drawing and forming. Welding of such alloys has been a challenge due to a number of issues including solidification cracking, atmospheric contamination (O, C, and N), as well as a shift in ductile-to-brittle transition to higher temperature following grain growth induced by welding. Compositional optimization of refractory alloys for solidification cracking resistance in particular is desirable as their usage increases with the advent of advanced manufacturing methods such as 3D printing. This work evaluates the effect of compositional variation in refractory metal systems on the solidification cracking susceptibility with the goals of optimizing existing alloys and joining process techniques, and formulating new alloys with increased solidification cracking resistance. Experimental Procedures. A python code was developed in a Jupyter notebook environment (Michael and Sowards, 2023) to facilitate the calculation of crack susceptibility index proposed by Kou (2015). Composition is entered as a single point, or as a 1-D or 2-D array. The notebook calls pycalphad (Otis and Liu, 2017 and Bocklund et al, 2020) to calculate the evolution of fraction solid as a function of temperature (under either Scheil or equilibrium assumptions) and then evaluates steepness of the fraction solid curve near the terminal stage of solidification to predict solidification cracking resistance. Open source thermodynamic databases available at online repositories are used (van de Walle). The process is setup in an automated fashion to generate plots that show variation in solidification cracking susceptibility according to composition on 1-D line plots or 2-D contour plots. The Jupyter notebook and crack susceptibility algorithm was also integrated with a widely used commercial CALPHAD code for validation and alloy exploration. Results and Discussion. The crack susceptibility model was first validated against a series of refractory alloy compositions evaluated in past work which utilized a specialized Varestraint test built inside a vacuum chamber environment (Lessman and Gold, 1971). The alloys tested in the Varestraint apparatus included T-111 (Ta-8W-2Hf), ASTAR-811C (Ta-8W-1Re-0.7Hf-0.025C), FS-85 (Nb-27Ta-10W-1Zr), T-222 (Ta-9.6W-2.4Hf-0.01C), Ta-10W, B-66 (Nb-5Mo-5V-1Zr), and SCb-291 (Nb-10W-10Ta). The initial test of the model showed a strong correlation with empirical Varestraint data, i.e., a Spearman rank correlation between model predictions and hot cracking measurements was observed to be greater than 0.8. Following the validation, a set of refractory metal binary mixtures was investigated to evaluate sensitivity of Nb, Mo, W, and Ta to C, N, and O content. A series of plots were produced that suggest ppmw ranges of C, N, and O where solidification cracking increases significantly and reaches a maximum. Also comparative ranking of each primary refractory metal to each interstitial was produced. For example C produces greater cracking response in Mo whereas O produces greater cracking response in Ta and Nb. Such compositional values have utility in setting limits on pickup of these interstitial elements during welding and printing rather than using a one-size-fits-all approach. Furthermore, the results have use in determining additive powder recycling requirements, which is especially pertinent for refractory metal powders due to their high cost compared to conventional alloys. Another application created thousands of hypothetical alloys within the nominal specified composition range of two widely used refractory alloys C103 (Nb-10Hf-1Ti) and TZM (Mo-0.5Ti-0.1Zr). The cracking index was calculated for the alloys and results were fed into machine learning regression techniques including Multiple Linear Regression, Ridge Regression, and Lasso Regression to determine relative potency each alloying element had on computed solidification cracking index. A series of linear equations were produced that relate composition of C103 and TZM to solidification cracking index. The crack susceptibility of C103 for example is described by an equation of the form: cracking index ~ O + 0.667*C + 0.635*N + 0.00037*Ta – 0.0008*Hf (in wt.%) From that equation, it is clear that O has strong propensity to induce solidification cracking. Interestingly, Hf is shown to reduce calculated cracking response. Finally, realizing the potential of this method to discover new refractory alloy formulations across the period table that have low solidification cracking sensitivity, the code was applied to new untested alloy systems including W-Zr-C, W-Ta-C, and others. Conclusions. In summary, an open source numerical method has been developed using Python code to calculate Kou’s crack susceptibility index. The method was applied to refractory metals which are inherently difficult to study from a weldability testing standpoint since inert shielding gas is not sufficient and welding is typically done in vacuum, especially in light of findings presented here where oxygen has profound influence on solidification cracking. This work revealed the effect of compositional variations on a series of refractory metals and showed the framework defined here will be useful in 1) the development of new alloys that have improved weldability and 3D printability, 2) placing compositional limits on existing alloys, and 3) ensuring adequate controls of manufacturing processes such as 3D printing where powder reuse is critical. Keywords. pycalphad; Python; refractory metals; solidification cracking. References. B. Bocklund et. al. (2020) http://doi.org/10.5281/zenodo.3630657. S. Kou. (2015) https://doi.org/10.1016/j.actamat.2015.01.034. G.G. Lessmann and R.E. Gold. Welding Journal, issue 1, pp. 1-s – 8-s (1971). F.N. Michael and J.W. Sowards. NASA/TM-20230002218 (2023). R. Otis and Z.-K. Liu. (2017) http://doi.org/10.5334/jors.140. A. Van de Wallle et. al. (2018) https://doi.org/10.1016/j.calphad.2018.04.003.

pycalphad↗

Microstructural and Mechanical Characterization of a Dispersion Strengthened Medium Entropy Alloy Produced Using Selective Laser Melting

High entropy alloys (HEAs) are an interesting new class of alloys which have been shown to exhibit both notable strength and ductility for a wide range of temperature and stresses. In addition, the remarkably small difference between the solvus and liquidus temperatures for many face centered cubic HEAs makes them an excellent candidate for selective laser melting fabrication. In this study, the microstructure and mechanical properties of a dispersion strengthened equiatomic NiCoCr alloy successfully produced using selective laser melting are explored. The effect laser speed, laser power, and powder recyclability have on final part density and microstructural segregation are analyzed through both x-ray diffraction and high resolution scanning electron microscopy. These results are further validated and compared to stable phase predictions produced using a commercially available high entropy alloy mobility database. Lastly, the tensile strengths resulting from different heat treatment pathways are detailed.

Smith, T. M.↗

In Situ Manufacturing is a Necessary Part of Any Planetary Architecture

The key to any sustainable presence in space is the ability to manufacture necessary tools, parts, structures, spares, etc. in situ and on demand. Cost, volume, and up-mass constraints prohibit launching everything needed for long-duration or long-distance missions from Earth, including spare parts and replacement systems. There are many benefits to building items as-needed in situ using computer aided drafting (CAD) models and additive manufacturing technology: (1) Cost, up-mass, and volume savings for launch due to the ability to manufacture specific parts when needed. (2) CAD models can be generated on Earth and transmitted to the station or spacecraft, or they can be designed in situ for any task. Thus, multiple people in many locations can work on a single problem. (3) Items can be produced that will enhance the safety of crew and vehicles (e.g., latches or guards). (4) Items can be produced on-demand in a small amount of time (i.e., hours or days) compared to traditional manufacturing methods and, therefore, would not require the lengthy amount of time needed to machine the part from a solid block of material nor the wait time required if the part had to be launched from Earth. (5) Used and obsolete parts can be recycled into powder or wire feedstock for use in later manufacturing. (6) Ultimately, the ability to produce items as-needed will reduce mission risk, as one will have everything they need to fix a broken system or fashion a new part making it available on a more timely basis.

Edmunson, Jennifer E.↗

An Open-Source Numerical Model for Mitigating Refractory Alloy Hot Cracking Susceptibility

Refractory alloys are susceptible to solidification cracking during welding and 3D printing. Composition control is an effective method of controlling solidification cracking. This work evaluates the effect of compositional variation in refractory metal systems on a computed solidification cracking susceptibility. A numerical model has been developed using Python code and open-source CALPHAD software to calculate Kou’s crack susceptibility index. The model is validated against past weldability studies performed on several refractory alloy systems. The approach is extended towards the development of new alloys with improved 3D printability and weldability and is shown to have utility in defining compositional limits for existing alloys and feedstocks. Furthermore, the model will aid in determining process controls for powder reuse and recycling.

pycalphad↗

Developments of Bosch Process Architectures for ISRU Terrestrial Applications

To effectively realize NASA’s goals of a sustainable presence on the Moon and be-yond, In-Situ Resource Utilization (ISRU) must be leveraged. To reduce launch mass for space missions, commodities such as oxygen and carbon can be produced in-situ. Oxygen can be used for life support and as a propellant, and carbon can be used for battery production, filtration, additive manufacturing, and steel casting. Carbon is a required reactant in the carbothermal reduction process, a leading candidate for oxygen production on the lunar surface. To pro-duce these consumables, the Carbon Utilization Technology for Lunar and Atmospheric Systems (CUTLAS) project is developing architectures that leverage the Bosch process. The Bosch process re-acts CO 2 and H 2 to produce carbon powder and water, which can then be electrolyzed, leaving O 2 and recycled H 2 . This process is also applicable to carbon dioxide emissions on Earth.

Carbon capture↗

Electromagnetic Melt Processing: A Pathway to New Additive Manufacturing Technologies for Functional High-Performance Thermoplastics

In this study, we apply the electromagnetic (EM) melt processing of thermoplastics on an innovative EM field-driven powder bed fusion additive manufacturing (AM) concept for high-performance functional parts: Selective Microwave Melting/Sintering (SMM/SMS). This technique leverages the EM susceptibility of carbon nanotube-coated polymer micro-pellets to achieve rapid, localized heating and powder fusion. Thus, selective microwave melting (SMM) was used to fabricate multilayer specimens made of recycled polyphenylene sulfide (rPPS) and carbon nanotubes (CNTs). The resulting SMM specimens exhibited very good interlayer integrity, localized fusion at pellet boundaries, and tolerable residual porosity, indicating effective fusion and acceptable consolidation. CNT-rich interphases were retained after irradiation, generating anisotropic electrically active network pathways and enabling conductivity enhancement at low filler content. At only 1.0 wt% CNT, the specimens exhibited electrical conductivity approximately three orders of magnitude higher than neat rPPS. Dynamic mechanical analysis showed improved viscoelastic response relative to neat rPPS, while tensile testing confirmed that the SMM-processed specimens retained practical mechanical integrity despite localized voids. These results demonstrate that SMM can effectively consolidate EM susceptible thermoplastic powder beds while preserving their segregated conductive networks. This may become a scalable route for producing multifunctional thermoplastic parts with low filler loadings, tunable anisotropy, and structured materials and parts. Overall, the findings suggest that EM field-based AM can help overcome key limitations of conventional thermoplastic processing by enabling scalable, energy-efficient fabrication of nanostructured composites and expanding AM to a broader range of resins, including high-performance thermoplastics with customized functional properties.

Powder bed fusion↗

Water Purification Systems

A water purification/recycling system developed by Photo-Catalytics, Inc. (PCI) for NASA is commercially available. The system cleanses and recycles water, using a "photo-catalysis" process in which light or radiant energy sparks a chemical reaction. Chemically stable semiconductor powders are added to organically polluted water. The powder absorbs ultraviolet light, and pollutants are oxidized and converted to carbon dioxide. Potential markets for the system include research and pharmaceutical manufacturing applications, as well as microchip manufacture and wastewater cleansing.

Source record↗

Improved coal-slurry pipeline

High strength steel pipeline carries hot mixture of powdered coal and coal derived oil to electric-power-generating station. Slurry is processed along way to remove sulfur, ash, and nitrogen and to recycle part of oil. System eliminates hazards and limitations associated with anticipated coal/water-slurry pipelines.

Dowler, W. L.↗

Development of Aluminum Feedstock for Additive Manufacturing

The rapid evolution of materials science and manufacturing technologies in recent years has offered new pathways to manipulate materials for bespoke manufacturing. Here we aim to develop feedstocks for applications such as radiator panels, fuel tanks, and structural components for outfitting. As a strong, light weight and thermally conductive material aluminum is ideal for these applications. An often-overlooked source of aluminum waste is food packaging used on the International Space Station. Reusing this waste stream will reduce the cost and logistics of regular sparing. In Space Manufacturing (ISM) will utilize this technology is such areas as sparing and outfitting. However, processing aluminum can present challenges, especially in the context of additive manufacturing and sintering, due to its high reactivity and tendency to form a tenacious oxide layer. Identifying appropriate binders and sintering profiles can overcome these challenges. Herein we present our work on obtaining aluminum powder derived from food packaging, binder selection for aluminum feedstock, and a demonstration of bound metal deposition printing.

aluminum↗

Outfitting the In-Space Manufacturing Advancement Center (ISMAC)

Marshall Space Flight Center has begun investment into a new collaborative workspace where ISM technologies can be advanced utilizing multidisciplinary teams. Equipment has been commissioned to explore ISM technologies related to electronics, welding, additive manufacturing, recycling, and metal extraction from Lunar or Martian regolith. This is an overview of the latest capabilities outfit to the new In-Space Manufacturing Advancement Center.

In-Space Manufacturing↗

Extracting Oxygen from Lunar Simulant Using a Transparent Furnace Pulsed Fluidized Bed

In the event that humans return to the moon, utilizing the local materials will be beneficial for extended stays. Rather than transporting resources, such as oxygen, from Earth, NASA is investigating methods of extracting it from lunar regolith. One promising process is hydrogen reduction. In the hydrogen reduction process, lunar regolith is heated to 1000 C in the presence of hydrogen. The iron oxide (Fe-O) bonds, found in lunar material, are broken and the hydrogen attracts the oxygen to produce water vapor [Allen et al., 1996]. FeO + H2 (right arrow) Fe +H2O. The water vapor is then captured, cleaned, and electrolyzed. The hydrogen is recycled back to the reduction process and the oxygen is stored until consumed by an end user (propulsion, life support, etc.). To obtain a good oxygen yield, the majority of lunar regolith must be exposed to the hydrogen gas and have a high rate of heat transfer from heat source to particle. This is achieved with good solids mixing via fluidization or mechanical agitation. In Generation II of the ROxygen program, the ROxygen Team at Johnson Space Center (JSC) investigated the feasibility of gas only pulsed fluidization as the only means to mix synthetic lunar regolith (simulant) at high temperatures. Fluidized beds have been used in industry to effectively process powders for decades. They consist of gas flowing upward through a bed of particles. The stirring action continuously moves the grains around to achieve uniform mixing of gas, solids, and heat [Geldart, 1986]. A transparent furnace unit was developed by Thoughventions Unlimited LLC (TvU) to aid in the qualitative observation of the fluidization behavior at high temperatures. Multipoint thermocouples and pressure sensors provided quantitative information regarding the quality of mixing. The water produced was measured using humidity sensors and captured using a NASA designed and built condenser. Once the simulant was processed, pneumatically transporting the 'hot' simulant out of the furnace was investigated.

Oryshchyn, L.↗

Cold Metal Transfer (CMT) Wire-Arc Additive Manufacturing (WAAM)

Aluminum has been identified as a compound within regolith and is likely to become a core component of our infrastructure on the lunar surface as in-situ resource utilization (ISRU) capabilities are advanced Large-scale components, outfitting, and repairs of aluminum materials can be fabricated with robotic wire arc additive manufacturing (WAAM) in order to inhabit the moon’s surface long term WAAM is a high value process for lunar advanced manufacturing as it does not require special containment to reduce explosion hazards such as powder-based additive processes and feedstock The welding process of cold metal transfer (CMT) is a relatively new variation of gas metal arc welding (GMAW, also known as MIG) that relies on the detection of a short circuit in the welding process to control the deposition droplet action, resulting in lower heat input and splatter compared to conventional MIG welding The past year was spent developing the CMT-WAAM process for aluminum materials, tested specialty feedstock, tested within the high vacuum environment, and advanced the MSFC capability to perform complex toolpathing from solid models Upcoming and future work includes large depositions working towards material certification for multiple feedstocks, in-situ monitoring, work to use recycled materials for the AM feedstock, and the design and fabrication of a parabolic flight experiment payload.

cold metal transfer↗

A Decision-Support Model for Selecting Additive Manufacturing Versus Subtractive Manufacturing Based on Energy Consumption

This paper presents a simple computational model for determining whether additive manufacturing or subtractive manufacturing is more energy efficient for production of a given metallic part. The key discriminating variable is the fraction of the bounding envelope that contains material – i.e. the volume fraction of solid material. For both the additive process and the subtractive process, the total energy associated with the production of a part is defined in terms of the volume fraction of that part. The critical volume fraction is that for which the energy consumed by subtractive manufacturing equals the energy consumed by additive manufacturing. For volume fractions less than the critical value, additive manufacturing is more energy efficient. For volume fractions greater than the critical value, subtractive manufacturing is more efficient. The model considers the entire manufacturing lifecycle – from production and transport of feedstock material through processing to return of post-production scrap for recycling. Energy consumed by processing equipment while idle is also accounted for in the model. Although the individual energy components in the model are identified and accounted for in the expressions for additive and subtractive manufacturing, values for many of these components may not be currently available. Energy values for some materials’ production and subtractive and additive manufacturing processes can be found in the literature. However, since many of these data are reported for a very specific application, it may be difficult, if not impossible, to reliably apply these data to new process-material manufacturing scenarios since, very often, insufficient information is provided to enable extrapolation to broader use. Consequently, this paper also highlights the need to develop improved knowledge of the energy embodied in each phase of the manufacturing process. To be most valuable, users of the model should determine the energy consumed by their manufacturing process equipment on the basis of energy-per-unit-volume of production for each material of interest – considering both alloy composition and form. Energy consumed during machine idle per unit time should also be determined by the user then scaled to specific processing scenarios. Energy required to generate feedstock material (billet, plate, bar, wire, powder) must be obtained from suppliers.

J K Watson↗