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 991 records · Page 55

High-throughput additive manufacturing and characterization of refractory high entropy alloys

Refractory High Entropy Alloys (RHEAs) and Refractory Complex Concentrated Alloys (RCCAs) are high-temperature structural alloys ideally suited for use in harsh environments. While these alloys have shown promising structural properties at high temperatures that exceed the practical limits of conventional alloys, such as Ni-based superalloys, exploration of the complex phase-space of these materials remains a significant challenge. We report on a high-throughput alloy processing and characterization methodology, leveraging laser-based metal additive manufacturing (AM) and mechanical testing techniques, to enable rapid exploration of RHEAs/RCCAs. We utilized in situ alloying and compositional grading, unique to AM processing, to rapidly-produce RHEAs/RCCAs using readily available and inexpensive commercial elemental powders. We demonstrate this approach with the MoNbTaW alloy system, as a model material known for having exceptionally high strength at elevated temperature when processed using conventional methods (e.g., casting). Microstructure analysis, chemical composition, and strain rate dependent hardness of AM-processed material are presented and discussed in the context of understanding the structure-properties relationships of RHEAs/RCCAs.

36 MATERIALS SCIENCE↗

Characterization of U-10Zr-2Sn-2Sb and U-10Zr-2Sn-2Sb-4Ln to assess Sn+Sb as a mixed additive system to bind lanthanides

In this paper, tin and antimony are being investigated as potential additives to metallic fuel to control fuel-cladding chemical interaction (FCCI). A primary cause of FCCI is lanthanide fission products moving to the fuel periphery and interacting with the cladding. This interaction can lead to wastage of the cladding and, given enough time or burn-up, eventually to a cladding breach. The current study involves a microstructural characterization of as-cast and annealed U-10Zr-2Sn-2Sb and U-10Zr-2Sn-2Sb-4Ln, where Ln = 53Nd-25Ce-16Pr-6La, all in wt %, as alloys which could prevent FCCI. Scanning electron microscopy (SEM) analysis and X-ray powder diffraction indicates the additive-Zr compound in U-10Zr-2Sn-2Sb is Zr 5 (Sn,Sb) 3 , while the additive-Ln compound being formed in U-10Zr-2Sn-2Sb-4Ln is Ln 5 (Sn,Sb) 4 , with significantly more Sb than Sn (37 at. % versus 6 at. %, respectively). The bulk of the Sn, with a small amount of Sb, remained as Zr 5 (Sn,Sb) 3 precipitates. Finally, the potential benefits of a mixed additive system, along with relative stabilities of the intermetallic compounds, are discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Automated high-throughput tensile testing reveals stochastic process parameter sensitivity

The mechanical properties of additively manufactured metals tend to show high variability, due largely to the stochastic nature of defect formation during the printing process. This study seeks to understand how automated high throughput testing can be utilized to understand the variable nature of additively manufactured metals at different print conditions, and to allow for statistically meaningful analysis. This is demonstrated by analyzing how different processing parameters, including laser power, scan velocity, and scan pattern, influence the tensile behavior of additively manufactured stainless steel 316L utilizing a newly developed automated test methodology. Microstructural characterization through computed tomography and electron backscatter diffraction is used to understand some of the observed trends in mechanical behavior. Specifically, grain size and morphology are shown to depend on processing parameters and influence the observed mechanical behavior. In the current study, laser-powder bed fusion, also known as selective laser melting or direct metal laser sintering, is shown to produce 316L over a wide processing range without substantial detrimental effect on the tensile properties. Ultimate tensile strengths above 600 MPa, which are greater than that for typical wrought annealed 316L with similar grain sizes, and elongations to failure greater than 40% were observed. As a result, it is demonstrated that this process has little sensitivity to minor intentional or unintentional variations in laser velocity and power.

36 MATERIALS SCIENCE↗

Entropy Engineering and Tunable Magnetic Order in the Spinel High-Entropy Oxide

Spinel oxides are an ideal setting to explore the interplay between configurational entropy, site selectivity, and magnetism in high-entropy oxides (HEOs). In this work, we characterize the magnetic properties of the spinel (Cr, Mn, Fe, Co, Ni) 3 O 4 and study the evolution of its magnetism as a function of nonmagnetic gallium substitution. Across the range of compositions studied here, from 0 to 40% Ga, magnetic susceptibility and powder neutron diffraction measurements show that ferrimagnetic order is robust in the spinel HEO. However, we also find that the ferrimagnetic order is highly tunable, with the ordering temperature, saturated and sublattice moments, and magnetic hardness all varying significantly as a function of Ga concentration. Through X-ray absorption and magnetic circular dichroism, we are able to correlate this magnetic tunability with strong site selectivity between the various cations and the tetrahedral and octahedral sites in the spinel structure. In particular, we find that while Ni and Cr are largely unaffected by the substitution with Ga, the occupancies of Mn, Co, and Fe are each significantly redistributed. Ga substitution also requires an overall reduction in the transition metal valence, and this is entirely accommodated by Mn. Finally, we show that while site selectivity has an overall suppressing effect on the configurational entropy, over a certain range of compositions, Ga substitution yields a striking increase in the configurational entropy and may confer additional stabilization. In conclusion, spinel oxides can be tuned seamlessly from the low-entropy to the high-entropy regime, making this an ideal platform for entropy engineering.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Real time study of grain enlargement in zirconium under room-temperature compression across the α to ω phase transition

We report a synchrotron Laue diffraction study on the microstructure evolution in zirconium (Zr) as it undergoes a pressure-driven structural phase transformation, using a recently developed real time scanning x-ray microscopy technique. Time resolved characterizations of microstructure under high pressure show that Zr exhibits a grain enlargement across the α-Zr to ω-Zr structural phase transition at room-temperature, with nucleation and growth of ω-Zr crystals observed from initially a nano-powdered α-Zr matrix. The observed grain enlargement is unusual since the enlargement processes typically require substantially high temperature to overcome the activation barriers for forming and moving of grain boundaries. Possible mechanisms for the grain enlargement are discussed.

36 MATERIALS SCIENCE↗

Oxygen Effects on Solidification Behavior of Gas Tungsten Arc–Welded Laser Powder Bed Fusion–Fabricated 304L Stainless Steel

ct The laser – powder bed fusion (L-PBF) process inherently accumulates interstitial gas elements during powder fabrication and laser deposition processes. Such elements can lead to localized variations in the weld pool and affect the solidification behavior (when compared with its wrought equivalent), in addition to chemical micro-segregation within the fabricated material. This study was conducted to characterize the solidification behavior of gas tungsten arc welds made on L-PBF 304L stainless steel. The effect of surface active elements on the local solidification rates was studied. An emphasis was placed on the role local solidification rates and temperature gradients throughout the weld play on the resultant weld solidification structure and micro-segregation. It was determined that gas tungsten arc welds on L-PBF 304L stainless steel exhibited a vermicular ferrite solidification structure compared to a mix of vermicular and lathy ferrite structure in wrought 304L. The varying thermal gradients affected the solidification modes and partitioning of elements leading to fluctuations of micro-segregation in the L-PBF 304L. Macroscopically, such partitioning affected the surface tension within the weld pool, producing asymmetric weld pool geometries. The compositional differences between wrought and L-PBF fabricated 304L stainless steels resulted in irregular solidification behaviors during welding affecting the final weld microstructure.

36 MATERIALS SCIENCE↗

Study of Poly(ether ketone ketone) (PEKK): Outgassing Characteristics and Likely Residual Synthesis Impurities

In May-June, 2020, a study was conducted to characterize the outgassing properties of a series PEKK (Poly(ether ketone ketone)) samples using cryo-GC/MS headspace analysis. Three sets of samples were interrogated: sample group 1 consisted of 2 additively manufactured PEKK samples (PEKK "ole and "New") prepared by KCNSC from powder material from Solvay Specialty Polymers USA, LLC. Sample groups 2 and 3 consist of 5 PEKK powder types (used as feedstock for additive manufacturing processes) and 4 additively-manufactured PEKK material lots, respectively. Contrary to expectations, all samples of PEKK material were observed to outgas sulfur-containing compounds. Other analyses (EDS/EMA, GC-TOF/MS of PEKK sample extractions) confirmed the presence of sulfur in the PEKK bulk material. Specifically, Diphenyl sulfone (used as a reagent or high-temperature solvent in the synthesis of Polyaryletherketone or PAEK polymers) was observed in three of the powders and in both the PEKK "Old" and "New" samples, suggesting that the source of the sulfur can be traced to impurities in the material left over from the synthesis process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Experimental Investigation of Magnesium Powder Combustion With C02 for Mars Ascent Applications

Combustion of metals with CO2 has been identified as a possible propellant for Mars ascent applications. CO2 could be condensed from the Martian atmosphere, reducing the amount of propellant that must be transported from Earth. An attractive feature of this approach compared to other in situ propellant concepts is that no chemical processing on Mars is required. Magnesium has been identified as the most promising metal for this application because it ignites and burns easily in CO2. Preliminary systems studies indicate a 2 to 1 delivered mass advantage for Mg ascent propulsion using in situ C02, as compared to a conventional storable propellant system. The Propulsion Research Center at MSFC is undertaking an experimental investigation of magnesium powder combustion with CO2 in order to provide fundamental data on the combustion performance of Mg powder + CO2 mixtures needed to assess the feasibility of developing a practical Mg powder + CO2 rocket engine. Initial combustion experiments will be carried out in a small scale atmospheric pressure dump combustor. Effects of varying the Mg particle size, firing rate and O/F ratio on combustion stability and efficiency will be investigated. The combustion process will be characterized by optical flame measurements and extraction of combustion product samples. The experimental facility is currently being prepared and combustion experiments will begin during the first quarter of 2005. The final paper will describe the test facility and initial experimental results.

Foote, John P.↗

Marshall Space Flight Center's Impact Testing Facility Capabilities

Marshall Space Flight Center s (MSFC) Impact Testing Facility (ITF) serves as an important installation for space and missile related materials science research. The ITF was established and began its research in spacecraft debris shielding in the early 1960s, then played a major role in the International Space Station debris shield development. As NASA became more interested in launch debris and in-flight impact concerns, the ITF grew to include research in a variety of impact genres. Collaborative partnerships with the DoD led to a wider range of impact capabilities being relocated to MSFC as a result of the closure of Particle Impact Facilities in Santa Barbara, California. The Particle Impact Facility had a 30 year history in providing evaluations of aerospace materials and components during flights through rain, ice, and solid particle environments at subsonic through hypersonic velocities. The facility s unique capabilities were deemed a "National Asset" by the DoD. The ITF now has capabilities including environmental, ballistic, and hypervelocity impact testing utilizing an array of air, powder, and two-stage light gas guns to accommodate a variety of projectile and target types and sizes. Numerous upgrades including new instrumentation, triggering circuitry, high speed photography, and optimized sabot designs have been implemented. Other recent research has included rain drop demise characterization tests to obtain data for inclusion in on-going model development. The current and proposed ITF capabilities range from rain to micrometeoroids allowing the widest test parameter range possible for materials investigations in support of space, atmospheric, and ground environments. These test capabilities including hydrometeor, single/multi-particle, ballistic gas guns, exploding wire gun, and light gas guns combined with Smooth Particle Hydrodynamics Code (SPHC) simulations represent the widest range of impact test capabilities in the country.

Finchum, Andy↗

Additive Manufacturing of SiC Based Ceramics and Ceramic Matrix Composites

Silicon carbide (SiC) ceramics and SiC fiber reinforcedSiC ceramic matrix composites (SiCSiC CMCs) offer high payoff as replacements for metals in turbine engine applications due to their lighter weight, higher temperature capability, and lower cooling requirements. Additive manufacturing approaches can offer game changing technologies for the quick and low cost fabrication of parts with much greater design freedom and geometric complexity. Four approaches for developing these materials are presented. The first two utilize low cost 3D printers. The first uses pre-ceramic pastes developed as feed materials which are converted to SiC after firing. The second uses wood containing filament to print a carbonaceous preform which is infiltrated with a pre-ceramic polymer and converted to SiC. The other two approaches pursue the AM of CMCs. The first is binder jet SiC powder processing in collaboration with rp+m (Rapid Prototyping+Manufacturing). Processing optimization was pursued through SiC powder blending, infiltration with and without SiC nano powder loading, and integration of nanofibers into the powder bed. The second approach was laminated object manufacturing (LOM) in which fiber prepregs and laminates are cut to shape by a laser and stacked to form the desired part. Scanning electron microscopy was conducted on materials from all approaches with select approaches also characterized with XRD, TGA, and bend testing.

3-D printing↗

Process Optimization of Carbon Electrode Materials Manufacturing by Experimental Study and Machine Learning Techniques

Electrospun carbon fibers from coal have been investigated as electrodes for batteries and supercapacitors. Despite the excellent properties of coal-derived carbon fibers (CCNF) for energy storage devices, there still lacks systematic understanding on how various process parameters affect final electrode performances, which poses challenges to scale from pilot to high volume manufacturing. The goals of this project are twofold. First, we focuse on process optimization for converting a new precursor from powder river basin (PRB) coal, referred to as coal-based polyurethane (CPU) to CCNF using electrospinning. Second, different machine learning techniques will be examined using experimental data from this work and open literature. Specifically, for CPU the following process parameters need to be characterized and optimized in order to produce CCNFs with desirable mechanical integrity and physiochemical properties: precursor composition and viscosity, operating voltage and distance, oxidation and carbonization temperature and duration. Consequently, physiochemical properties of the fibers were characterized to correlate these process parameters with desirable electrochemical performance. Given the complex nature of the fiber production process, ML models are assessed for their ability to capture the nonlinear relationship between process parameters and the electrochemical properties in applications including supercapacitors. As such, we applied various machine learning techniques, to determine which technique produces a model that best predicts device function.

Cincotta, Robert E.F.↗

Fabrication and physicochemical characterization of graphene oxide derived from thermally expanded graphite

Graphene oxide was obtained from expanded graphite according to the modified Hummers method. The reaction time was significantly reduced (from 24 to 8 h) by applying the expanded graphite in the oxidation process. The interlayer distance in obtained samples was equal to 0.70–0.74 nm. Structural features of the material were studied by the powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, XPS spectroscopy, and NMR spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Creep Property Characterization of Potential Brayton Cycle Impeller and Duct Materials

Cast superalloys have potential applications in space as impellers within closed-loop Brayton cycle nuclear power generation systems. Likewise wrought superalloys are good candidates for ducts and heat exchangers transporting the inert working gas in a Brayton-based power plant. Two cast superalloys, Mar-M247LC and IN792, and a NASA GRC powder metallurgy superalloy, LSHR, have been screened to compare their respective capabilities for impeller applications. Mar-M247LC has been selected for additional long term evaluations. Initial tests in helium indicate this inert environment may debit long term creep resistance of this alloy. Several wrought superalloys including Hastelloy(Registered TradeMark) X, Inconel(Registered TradeMark) 617, Inconel(Registered TradeMark) 740, Nimonic(Registered TradeMark) 263, Incoloy(Registered TradeMark) MA956, and Haynes 230 are also being screened to compare their capabilities for duct applications. Haynes 230 has been selected for additional long term evaluations. Initial tests in helium are just underway for this alloy. These proposed applications would require sufficient strength and creep resistance for long term service at temperatures up to 1200 K, with service times to 100,000 h or more. Therefore, long term microstructural stability is also being screened.

Gabb, Timothy P.↗

Evolution of microstructure and microtexture during hot deformation in an advanced P/M nickel base superalloy

Highlights: • Microstructural evolution of PM superalloy sensitive to temperature and strain rate. • Highest DRX with finer grained structure at higher temperatures and strain rates. • Dominance of DDRX showed by serrated grain boundaries and misorientation gradient. • Weak microtextural evolution inclined towards [110] fiber compression texture seen. In the present study, the effect of hot deformation parameters on the microstructural evolution is investigated for an experimental powder metallurgy nickel superalloy. The hot isostatically pressed (HIPed) alloy is isothermally hot compressed at constant true strain rate over wide temperatures (1000 °C, 1050 °C, 1100 °C, 1150 °C) and strain rates (0.001 s{sup −1}, 0.01 s{sup −1}, 0.1 s{sup −1}, 1 s{sup −1}) regimes. Electron Back-Scattered Diffraction (EBSD) characterization of the hot deformed samples is carried out to evaluate the microstructural evolution, grain boundary characteristics, and microtextural behaviour. The strong dependence of dynamic recrystallization characteristics on the hot deformation conditions is divulged through EBSD derived colour inverse pole figure maps endorsed by grain/twin boundary characteristics and misorientation gradient. Dynamic recrystallization (DRX) is maximized at higher deformation temperatures, whereas limited DRX is observed at lower deformation temperatures, especially at higher strain rates. The dominance of discontinuous dynamic recrystallization (DDRX) is manifested through bulged/serrated grain boundaries resulting in the formation of necklace microstructure corroborated by grain boundary cumulative misorientation gradient. Although random microtexture is revealed in both deformed and recrystallized microstructures, the tendency towards the formation of 110 fiber compression texture is apparently evident.

36 MATERIALS SCIENCE↗

Microstructure–Property Correlation in a Laser Powder Bed Fusion Processed High-Strength AF-9628 Steel

Laser powder bed fusion additive manufacturing (LPBF-AM) of a low-alloy, high-performance AF-9628 steel results in exceptionally high strength and good ductility. The reasons for such mechanical properties are investigated through detailed microscopy performed at several length scales. Thus, the characterization of melt pool, porosity, grain morphology, phases, and dislocations is performed in the as-printed material. The as-printed material consists of only 0.004 vol% of uniformly distributed porosity, single-phase martensitic laths with an average lath size of ≈2.5 μm, the absence of carbides indicating interstitial trapping of C atom, and high dislocation density in the martensitic laths. Experimental data through microscopy are then fed in analytical models for calculating strengthening contributions from various strengthening mechanisms. Calculated yield strength agrees well with experimentally determined value, and therefore, activation of various strengthening mechanisms is established in as-printed AF-9628.

36 MATERIALS SCIENCE↗

Nanoparticle-enabled increase of energy efficiency during laser metal additive manufacturing

The low energy efficiency of the laser metal additive manufacturing (AM) process is a potential sustainability concern for large-scale industrial production. Explicit investigation of the energy efficiency for laser melting requires the direct characterization of melt pool dimension and vapor depression, which is very difficult due to the opaque nature of the molten metal. Here we report the direct observation and quantification of effects of the TiC nanoparticles on the vapor depression and melt pool formation during laser powder bed fusion (LPBF) of Al6061 by in-situ high-speed high-energy x-ray imaging. Based on the quantification results, we calculated the laser melting energy efficiency (defined here as the ratio of the energy needed to melt the material to the energy delivered by the laser beam) with and without TiC nanoparticles during LPBF of Al6061. Here the results show that adding TiC nanoparticles into Al6061 leads to a significant increase of laser melting energy efficiency (114% increase on average, 521% increase under 312 W laser power, 0.4 m/s scan speed). Systematic property measurement, simulation, and x-ray imaging studies enable us, for the first time, to identify that three mechanisms work together to enhance the laser melting energy efficiency: (1) adding TiC nanoparticles increases the absorptivity; (2) adding TiC nanoparticles decreases the thermal conductivity, and (3) adding TiC nanoparticles enables the initiation of vapor depression and multiple reflection at lower laser power (i.e., lowers the laser power threshold for keyholing). The method and mechanisms of using TiC nanoparticles to increase the laser melting energy efficiency during LPBF of Al6061 we reported here may guide the development of feedstock materials for more energy efficient laser metal AM.

36 MATERIALS SCIENCE↗

Modeling low cycle fatigue (LCF) of additively manufactured Hastelloy X using An accelerated crystal plasticity fatigue damage model

This paper presents a microstructure-based model for low cycle fatigue (LCF) behavior and life of Nickel-based alloy Hastelloy X manufactured using laser-powder bed fusion (L-PBF) additive manufacturing (AM). AM Hastelloy X, a solution-strengthened alloy, is tested at elevated temperature under fully reversed LCF conditions at different strain levels. A generalized plane strain finite element model is generated from electron backscatter diffraction (EBSD) characterization. The constitutive behavior of the material under fatigue is modeled using crystal plasticity and calibrated with both monotonic tensile and cyclic stress–strain data. The fatigue micro-crack initiation and propagation in the microstructure is modeled using a modified Chaboche fatigue damage model. An embedded boundary condition with a homogenous medium is used to apply the cyclic deformation and prevent numerically introduced over-constraints during fatigue simulation. A ‘cycle-jump’ method is used to accelerate the fatigue simulation and reduce the computational cost. The simulation results are compared to LCF experiments, showing satisfactory matches in cyclic stress behavior and number of cycles to macro-crack initiation for all applied strain ranges. In addition, the model illustrates the potential for quantifying microscale fatigue life impacting factors such as microstructure and surface roughness, which is needed to accurately quantify the reliability of AM components in service.

36 MATERIALS SCIENCE↗

Manufacturing porous U10Zr fuels with controlled porosities by SPS and thermal properties

To accommodate the swelling of metallic fuels induced by the fission gas release during burnup in sodium fast reactor for a sodium-free fuel option, advanced U-10Zr fuels with controlled porosity were designed and demonstrated by spark plasma sintering. U-10Zr fuel pellets with manufactured porosities varying from 35% up to fully dense fuel pellets have been fabricated by controlling ball milling times of the starting uranium powders, sintering temperature, pressure, and duration, and the correlation among the microstructure control – porosity – sintering conditions has been established. To further mimick the pore structure in irradiated fuels, different pore formers (NaCl and NH4HCO3) have been used to control the pore size and distribution. Microstructure characterization indicates a lamellar reaction zone of U and Zr, differing from the arc-melted U-10Zr as a result of rapid consolidation of SPS at lower temperature and short durations. The thermal conductivity of U10Zr with different porosities are also measured. Here this work demonstrates the success in manufacturing new metallic fuel forms with controlled porosities and pore distribution, which can be used as model systems to investigate the thermal transfer behavior of metallic fuels in the reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗