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We report that fabrication of parts with high mechanical properties heavily depend on the quality of powder deployed in the fabrication process. Copper powder in three different powder types were spheroidized using radio-frequency inductively coupled plasma (ICP) spheroidization process (TekSphero-15 system). The characterized powders include virgin powder as purchased from the powder manufacturer, powder used in electron beam powder bed fusion (EB-PBF) process, and reconditioned powder, which was used powder that underwent an oxygen-reduction treatment. The goal of spheroidizing these powder types was to evaluate the change in powder morphology, the possibility of enhancing the powder properties back to their as-received conditions, and assess oxygen reduction of the powder lots given their initial oxygen contents. Also, to investigate the impact of re-spheroidization on powder properties, the second round of spheroidization was performed on the already used-spheroidized powder. The impact of powder type on powder sphericity and particle size distribution was evaluated using the image analysis of scanning electron microscope (SEM) micrographs and laser diffraction, respectively. The spheroidized powder showed higher sphericity and more uniform particle size distribution overall. Depending on the powder collection bin, second round of spheroidization affected the powder sphericity differently. The possibility of deploying the plasma spheroidization process as an alternative oxygen-reduction technique was also investigated through tracking the powders’ oxygen content using inert gas fusion method before and after the spheroidization. The plasma spheroidized powder showed less oxygen content than the hydrogen-treated powder. The second round of spheroidization caused no change in oxygen content. The correlation between oxygen-reduction and created cracks was discussed and compared between plasma spheroidization and hydrogen-treatment. The plasma spheroidization process created a powder with higher sphericity, uniform particle size, and less oxygen content.
Binder jetting (BJ) is an additive manufacturing process that uses a powder feedstock in a layer wise process to print parts by selectively depositing a liquid binder into the powder bed using inkjet technology. This study presents findings from high-speed synchrotron imaging of binder droplet-interaction during the BJ printing process. A custom laboratory-scale BJ test platform was used for testing which enabled control of relevant process parameters including powder material, print geometry, spacing between droplets, powder bed density, and powder moisture content. Powder ejection was observed above the powder bed surface and powder relocation due to droplet impact was observed below the powder bed surface. Powder relocation was observed to be sensitive to powder material, powder bed density, powder bed moisture, droplet spacing, and print geometry. Increasing powder bed density was found to increase particle ejection velocity but reduce the total number of particles ejected. Process parameters that increase binder / moisture content in the powder bed were found to reduce powder ejection. The number of ejected powder particles was reduced for lower droplet spacings. Both powder ejection and powder relocation below the powder bed were reduced by treating the surface of the powder bed with a water/triethylene glycol (TEG) mixture before printing. In conclusion, results from this study help to build understanding of the physical mechanisms in the BJ printing process that may contribute to formation of defects observed in final parts.
Additive Manufacturing (AM) powder flowability is critical to metal 3D printing, because the more fluid the powder is, the better powder spreads. AM Powder Flowability Capabilities at NASA MSFC studies density, flow, particle size distribution, and morphology for programs such as Moon-to-Mars Planetary Autonomous Construction Technology (MMPACT), ASTM Proficiency Testing for AM and Powder Metallurgy, and MSFC’s AM team. Examining and measuring powder characteristics is essential for improving flowability of AM powder and ensuring lot-to-lot consistency, which will help to prevent defects in manufactured parts. The Contamination Control Team (CCT) uses several methods to characterize AM powder. Optical particle size distribution and morphology analyses determine particle parameters including size, circularity, convexity, and dimensions. The Carney and Hall Flowmeter Funnel measures time it takes powder to flow through a funnel to compare relative flowability (free-flowing and non-free-flowing). In addition to this, the device utilizes a density cup which determines apparent density. Lastly, the Revolution Powder Analyzer measures dynamic powder flowability and behavior over time via digital imaging. Using the CCT’s lab, the team has produced ASTM Powder Proficiency Testing results with flow rates, apparent density, particle size distribution, and tap density on titanium-based and nickel-based powder and compared data with other companies/labs. Morphology data was also collected for various regolith simulant powder for the MMPACT program. Lastly, the CCT used morphology data to examine the flowability of Inconel 718 powder for Selective Laser Melting (SLM) and Directed Energy Deposition (DED) printers at MSFC. The CCT’s essential work in studying and enabling AM powder characterization has helped and will continue to help study new and refined powders in the AM industry.
Improved small-particle powders and powder-processing conditions have been developed for use in plasma spray deposition of thermal-barrier and environmental barrier coatings. Heretofore, plasma-sprayed coatings have typically ranged in thickness from 125 to 1,800 micrometers. As explained below, the improved powders make it possible to ensure complete coverage of substrates at unprecedently small thicknesses of the order of 25 micrometers. Plasma spraying involves feeding a powder into a hot, high-velocity plasma jet. The individual powder particles melt in the plasma jet as they are propelled towards a substrate, upon which they splat to build up a coating. In some cases, multiple coating layers are required. The size range of the powder particles necessarily dictates the minimum thickness of a coating layer needed to obtain uniform or complete coverage. Heretofore, powder particle sizes have typically ranged from 40 to 70 micrometers; as a result, the minimum thickness of a coating layer for complete coverage has been about 75 micrometers. In some applications, thinner coatings or thinner coating layers are desirable. In principle, one can reduce the minimum complete-coverage thickness of a layer by using smaller powder particles. However, until now, when powder particle sizes have been reduced, the powders have exhibited a tendency to cake, clogging powder feeder mechanisms and feed lines. Hence, the main problem is one of synthesizing smaller-particle powders having desirable flow properties. The problem is solved by use of a process that begins with a spray-drying subprocess to produce spherical powder particles having diameters of less than 30 micrometers. (Spherical-particle powders have the best flow properties.) The powder is then passed several times through a commercial sifter with a mesh to separate particles having diameters less than 15 micrometers. The resulting fine, flowable powder is passed through a commercial fluidized bed powder feeder into a plasma spray jet.
Additive Manufacturing (AM) powder flowability is critical to metal 3D printing, because the more fluid the powder is, the better powder spreads. The NASA MSFC’s Contamination Control Team (CCT) studies density, flow, particle size distribution, and morphology for programs such as Moon-to-Mars Planetary Autonomous Construction Technology (MMPACT), ASTM Proficiency Testing for AM and Powder Metallurgy, and MSFC’s AM team. Examining and measuring powder characteristics is essential for improving flowability of AM powder and ensuring lot-to-lot consistency, which will help to prevent defects in manufactured parts. The CCT uses several methods to characterize AM powder. Optical particle size distribution and morphology analyses determine particle parameters including size, circularity, convexity, and dimensions. The Carney and Hall Flowmeter Funnel measures time it takes powder to flow through a funnel to compare relative flowability (free-flowing and non-free-flowing). In addition to this, the device utilizes a density cup which determines apparent density. Lastly, the Revolution Powder Analyzer measures dynamic powder flowability and behavior over time via digital imaging. Using the CCT’s lab, the team has produced ASTM Powder Proficiency Testing results with flow rates, apparent density, particle size distribution, and tap density on titanium-based and nickel-based powder and compared data with other companies/labs. Morphology data was also collected for various regolith simulant powder for the MMPACT program. Lastly, the CCT used morphology data to examine the flowability of Inconel 718 powder for Selective Laser Melting (SLM) and Directed Energy Deposition (DED) printers at MSFC. The CCT’s essential work in studying and enabling AM powder characterization has helped and will continue to help study new and refined powders in the AM industry.
NASA Langley Research Center (LaRC) in Hampton, VA, and the Center for Welding, Joining, and Coating Research (CWJCR) in the Department of Metallurgical and Materials Engineering at the Colorado School of Mines (CSM) in Golden, CO, have collaborated for nearly fifteen years to develop metallic powder core tubular wire (PCTW) feedstock for additive manufacturing (AM) using electron beam deposition. The motivation for this development was to offset dealloying observed during deposition of titanium and aluminum alloy solid wire feedstock in the LaRC electron beam freeform fabrication (EBF3) system and to explore novel alloy compositions by tailoring the powder fill. EBF3 is a fusion-based AM process that is performed under vacuum and is consequently prone to vaporization loss of low vapor pressure alloying elements. Research spanning four graduate student research projects succeeded in developing the basic methodology to fabricate PCTW, the mass balance equations used to define the powder fill, microstructure control through particulate inoculation, and the feasibility of producing metal matrix composite materials. Metallic PCTW is comprised of a thin foil sheath wrapped around a powder blend. Fabrication of PCTW at CSM was accomplished using a tubular wire mill system to first bend a flat strip into a u-shaped cross section, deposit a powder fill, create a lap joint to seal the wire, and draw to final diameter. Powder management systems were developed to ensure uniform mixing of powder constituents and identify feed rates for optimum fill ratios. Processing parameters were successfully developed for titanium and aluminum alloy sheaths to account for material work hardening during drawing. Mass balance equations were developed to account for compositional contributions of the sheath and powder fill. PCTW composition can be adjusted through selection of the sheath or powder materials. PCTWs were successfully developed to offset Al loss in deposits of Ti-6-4 and Mg loss in Al 6061, resulting in deposits that were within the composition limits for each material. Ti-6-4 deposits were fabricated using PCTW comprised of commercially pure (CP) titanium sheath and a fill of pre-alloyed Ti-6-4 powder with additions of elemental Al and V powders. Additions of both elements were required to account for the CP Ti from the sheath, and Al was further enhanced to offset documented losses in EBF3 deposits. For Al 6061 deposits, composition was modulated through the choice of sheath material. The PCTW was made using an Al 5052 sheath to supplement Mg content and a fill composition of pre-alloyed 6061 powder with additions of Si and Cu.The slower solidification rate of the EBF3 process compared with laser powder bed fusion processes can lead to coarse-grained microstructures and mechanical property anisotropy. EBF3deposits of Ti-6-4 exhibited large epitaxially grown β grains, which result in degraded mechanical properties in the deposition direction. Microstructure refinement was achieved through a combination of electron beam modulation and the use of a PCTW designed for Ti-6-4 deposits and modified by the addition of powder made from Fe and B. Resulting deposits exhibited reductions in β grain size, α phase colony intercept length and lath width, and an increased volume fraction of β phase. The mechanism of microstructure refinement was related to precipitation of boride particles. Hardness testing confirmed that mechanical property anisotropy was reduced and an overall increase in hardness was achieved.Metal matrix composite (MMC) materials offer strength and stiffness benefits over unreinforced materials. Two methods were investigated using PCTW technology for producing Al 6061 basedMMC materials; the direct addition of SiC reinforcing particles and the in-situ generation of reinforcements through reaction synthesis of precursor powders. Al 6061 based MMCs reinforced with SiC exhibited particle clustering and formation of aluminum carbides during deposition. The application of a Ni coating to the SiC particles prior to incorporation into the powder fill eliminated aluminum carbide formation and aided particle distribution during deposition. Modulation of beam focus and power further reduced aluminum carbide formation and aided particle distribution. In reaction synthesis, precursor additions undergo an exothermic reaction during deposition to form new ceramic products, generally of finer scale than the initial precursor components. The product phases provide reinforcement in the MMC and act as nucleation sites during solidification, resulting in grain refinement, improved mechanical properties, and reduced susceptibility to solidification cracking. Higher tensile strength and stiffness were demonstrated in Al 6061 based MMCs with 2 vol% reinforcement. These combined research efforts demonstrate the potential of PCTW technology for customizing of alloy composition and achieving microstructure control. A manufacturing process for titanium- and aluminum-based PCTWs was developed based on iterative design, theoretical calculations, and empirical data. PCTW technology successfully mitigated Al loss from Ti-6-4 and Mg loss in Al 6061, resulted in grain refinement in Ti-6-4, and demonstrated fabrication of Al based MMCs
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.
The powder spreading is a vital step of powder-based additive manufacturing (AM) processes. The quality of spread powder can considerably influence the properties of fabricated parts. Poorly packed powder beds with high surface roughness result in printed part layers with large porosity and low dimensional accuracy, leading to poor mechanical properties. Therefore, the powder spreadability and its dependence on process parameters and powder characteristics should be quantified to improve the efficiency of powder-based AM methods. This study proposes a novel dimensionless powder spreadability metric that can be commonly used in different powder-based AM processes. The quality of spread powder in terms of powder bed density and surface roughness was evaluated by adjusting the process parameters including recoating velocity and layer thickness, and powder characteristics including particle size distribution. In addition, the dynamic repose angle was proposed and examined as another powder spreadability metric. Furthermore, the results showed that these two proposed metrics were strongly correlated and lower recoating velocity and larger layer thickness led to higher spreadability and lower dynamic repose angle.
One parameter that has both economic and performance effects in the manufacturing of steel parts is the powder feedstock used. 316 L steel powder can be produced through water atomization or gas atomization, where both the powder size and the atomization process determine the cost of powder feedstock. Gas atomized powder is spherical and has a lower oxygen content than water atomized powder, making it the preferred choice for performance, but comes at a higher financial cost. Here, in this study, various 316 L powder batches are characterized to understand physical properties and microstructural variations. Density and flowability were determined using gas pycnometry and Hall flow tests. Powder morphology and porosity were qualitatively analyzed via optical microscopy and scanning electron microscopy, Finally, transmission electron microscopy was used to determine changes in phases present. Spherical gas atomized powder of 30–100 μm contained Mn$-$Si rich oxides both on the surface and within the matrix. Meanwhile, irregular water atomized powder 30 μm in diameter contained silicon oxides without manganese. All powder particles contained a nickel rich cellular structure which was shown to support the formation of additional phases. While literature has observed general microstructural features across 316 L powder particles, transmission electron microscopy (TEM) in this study has identified variations in precipitation and cell structures. Information regarding morphology, flowability, density, and phase distributions can be applied to understand variations in part consolidation, which will in turn show which powder aspects are significant for production.
The effects of BaF2-CaF 2 particle morphology on PS304 feedstock powder flow ability have been investigated. BaF2-CaF2 eutectic powders were fabricated by comminution (angular) and by gas atomization (spherical). The fluoride powders were added incrementally to the other powder constituents of the PS304 feedstock: nichrome, chromia, and silver powders. A linear relationship between flow time and concentration of BaF2-CaF2 powder was found. Flow of the powder blend with spherical BaF2-CaF2 was better than the angular BaF2-CaF2. Flow ability of the powder blend with angular fluorides decreased linearly with increasing fluoride concentration. Flow of the powder blend with spherical fluorides was independent of fluoride concentration. Results suggest that for this material blend, particle morphology plays a significant role in powder blend flow behavior, offering potential methods to improve powder flow ability and enhance the commercial potential. These findings may have applicability to other difficult-to-flow powders such as cohesive ceramics.
The breakdown of solid metal into powder during the hydride-dehydride process is commercially important for the formation of titanium and other metal powders. Typically, the milling of the brittle hydride powder occurs in a ball mill, where milling media impacts powder particles to break them down. The milling media can impact particles that are larger than desired, as desired, or smaller than desired, indiscriminately making all particles smaller. In this work, we investigate how to minimize waste powder production during milling using two different milling methods, planetary ball milling and milling in a sieve shaker (sieve-milling). Both processes yielded similar amounts of 20–75 μm diameter powder (the target size range); however, sieve-milling generated a significantly smaller amount of undersized waste powder. The powders were characterized by X-ray diffraction, SEM/STEM, and magnetic susceptibility. Several differences between ball milling and sieve-milling processes are discussed. We then conclude that the decreased yield of undersized powder in sieve-milling was due to a combination of lower impact energy in sieve-milling, unreacted metallic cores in the hydride flakes, and the ability to mill target particle sizes during sieve-milling. While these results are from the milling of brittle hydride powder, similar methods may be applicable to other brittle powders, including ceramics or salts.
Abstract Poly(phenylene sulfide) (PPS) is a high‐performance polymer suiting the needs of powder bed fusion (PBF) early‐adopter industries. Although there are many benefits to PBF's powder bed‐based, one drawback is thermal ageing of the powder not incorporated into printed parts. Ideally, unfused powder can be reused in future builds; however, it is unlikely that critical printability properties of the thermally aged powder will remain unchanged. Changes in properties lead to either limited reuse through a practice of mixing used and new powder, or elimination of all powder after each build. In this paper, the authors report effects of thermal ageing in simulated printing conditions on properties of PPS critical to PBF processing. PBF‐grade PPS powder is exposed to process‐mimicking conditions. Properties relevant to the three PBF manufacturing process sub‐functions are assessed for the aged powders. Single‐layer prints are made using aged powder to observe polymer‐PBF interactions ad machina. Significant and systematic deviations from the as‐received state of the powder are observed for thermal and coalescence related properties with increasing exposure time and temperature. These changes are interpreted both in terms of physical and chemical changes in PPS and in terms of how these changes may impact the PBF printing process.
Achieving high powder packing density is critical in binder jet additive manufacturing (BJAM), as it directly influences the final part density, mechanical properties, and sintering behavior. Multi-modal powder blends, which combine particles of different sizes, have been explored as a strategy to optimize packing efficiency and minimize defects. In this study, bimodal and trimodal powder blends were obtained by mixing silicon carbide powder in three different sizes. These results show that increased powder density is achievable with bimodal powder blends but is reduced in trimodal blends, and it was found that a 13 % increase in the powder tap density was achieved using a bimodal blend of powder. The powder size distribution of the bimodal blend was measured at various stages during binder jet additive manufacturing and, no measurable powder separation occurred even after eight prints. Altogether, this study shows limited advantage to trimodal powder blends but good promise for bimodal blends for increasing printed density while maintaining reusability in the binder jet process.
By Increasing the powder layer thickness we could increase material deposition rates and reduce build times during laser powder bed fusion (LPBF). However, increasing the powder layer thickness could also negatively affect the local melting and subsequent microstructure of the printed material. This study systematically investigated, for the first time, the defect evolution and microstructural changes of LPBF stainless steel 316 (SS316) processed by using various powder layer thicknesses of 40, 80, and 120 μm while also varying the laser dwell time for the pulsed laser. Through image analysis, the pore density was found to increase with increasing powder layer thickness, particularly when the dwell time was too high or too low. The maximum achievable density (>99%) was found over a wide processing window when using the smallest powder layer thickness of 40 μm between dwell times of 60 and 100 μs. Increasing the powder layer thicknesses to 80 and 120 μm resulted in maximum densities of 98.7 and 96.8%, respectively, but the window for acceptable laser dwell times that could achieve these densities narrowed considerably. A microstructural analysis of the melt pools was performed to measure the melt pool depths and widths, both of which increased with increasing dwell time. However, increasing the powder layer thickness did not affect the melt pool depth and only minorly affected the width. A sub-grain cellular structure distinguished the melt pool boundaries. The cell size increased with increasing dwell time and decreasing powder layer thickness. Moreover, the cell size was used to calculate a cooling rate that had a magnitude of 10 7 K/s and increased with increasing powder layer thickness.
Triply periodic minimal surface (TPMS)-based structures show marked potential in novel nuclear reactor fuel designs, as their high surface area-to-volume ratio increases the efficiency of heat transfer out of the fuel, enabling safer, more innovative reactor designs. This milestone report addresses the role of dUO 2 powder processing route on the fill behavior of TPMS-based cladding shells to understand and advance the feasibility of manufacturing TPMS-based nuclear fuel forms. dUO 2 powder was processed through either a dry granulation route, varying consolidation pressure, or through milling, varying milling time, milling method and milled size distribution. The lowest tapped bulk densities (TBD), but best powder flowabilities, were obtained when testing unprocessed dUO 2 powder which was prone to self-agglomeration and formed low-density spheroids. The highest TBD and lowest flowabilities were obtained when using powder produced by hammer-milling dUO 2 powder to pass through a 200-mesh sieve, which led to particles with angular morphologies. Powder produced by dry granulation exhibited TBD that varied according to the consolidation pressure used to form the initial pellets and exhibited improved flowabilities when compared to hammer-milled material. Because of the large span of granule sizes formed as well as the irregular shape associated with the granules, a packing fraction of 0.69 was achieved, exceeding the analytical solution for random close packing of mono-sized spheres. TPMS polymer shells were loaded with unprocessed, granulated, and hammer-milled dUO 2 powders, and their qualitative packing behaviors were analyzed using x-ray computed tomography (xCT). TBDs calculated after loading TPMS polymer shells were 10-20% lower when compared to tapped bulk density measurements taken in a glass graduated cylinder, indicating a non-trivial impact on the tapped bulk density of either the TPMS channel size, TPMS channel surface material, powder cohesiveness, or a combination of the two parameters. A metallic zircaloy-4 TPMS shell will be loaded with hammer-milled dUO 2 powder upon receipt of the shell from Oak Ridge National Laboratory (ORNL) and shipped to Idaho National Labs (INL) for subsequent hot isostatic pressing (HIP) densification experiments.
The powder bed-based additive manufacturing (AM) process contains uncertainties in the powder spreading process and powder bed quality, leading to problems in repeatability and quality of the additively manufactured parts. This work focuses on identifying the uncertainty induced by particle size distribution (PSD) on powder flowability and the laser melting process, using Ti6Al4V as a model material. The flowability test results show that the effect of PSDs on flowability is not linear, rather the PSDs near dense packing ratios cause significant reductions in flowability (indicated by the increase in the avalanche angle and break energy of the powders measured by a revolution powder analyzer). The effects of PSDs on the selective laser melting (SLM) process are identified by using in-situ high-speed X-ray imaging to observe the melt pool dynamics during the melting process. The results show that the powder beds made of powders with dense packing ratios exhibit larger build height during laser melting. The effects of PSD with efficient packing on powder flowability and selective laser melting process revealed in this work are important for understanding process uncertainties induced by feedstock powders and for designing mitigation approaches.