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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

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↗
NASA NTRS2023

Numerical Study of Solidification Crack Susceptibility in Novel Refractory Alloy Systems

Calculation of Phase Diagrams (CALPHAD) -based solidification computa­tions, such as Scheil or equilibrium computations, have been utilized to propose crack solidification susceptibility indices (CSSIs) of cracking. These CSSIs have been proposed in order to predict the cracking susceptibility of an alloy in the solidification range, as a function of its solidification frac­tion and as dependent upon its wt.% elemental composition through the CALPHAD computation & via comparative methods between one composition & the next. Recently Kou at al. have proposed a novel CSSI where the gradient of the e.x. Scheil solidification curve is obtained in the critical solidification cracking region of greater than 0.95 fraction of solid. Therefore, a direct Temperature dependent metric is now available for the prediction, and presumably the control, of solidification cracking. In this TM, the researchers apply this Kou gradient method to refractory alloys for the first time & discuss justification for the approach via Spearman rank correlation with Varestraint cracking test data as well as by comparisons with Thermocalc based vulnerability time CSSI calculations. A Python Pycalphad module example of the approach is provided & can be utilized as an open-source resource that utilizes also open-source available thermodynamical databases, making the CSSI quantitative aspect of ICME more available and freely available to practitioners.

ICME integrated computational materials engineerin↗
NASA NTRS2023

Hot Cracking Behavior and Beam-Induced Grain Refinement in Electron Beam Freeform Fabricated Al 7075

Electron beam freeform fabrication (EBF 3 ) is a high deposition rate, wire-based directed energy deposition (DED) additive manufacturing (AM) process used to print metallic parts in a vacuum environment. While high specific strength 7xxx-series Al alloys are of interest in the aerospace and automotive industries, these alloys suffer from hot cracking issues during fusion welding and AM. In this work, linear deposits of Al 7075 were fabricated with EBF 3 to study the effects of baseplate thickness, preheat temperature, and beam focus on hot cracking behavior. Solidification cracks were observed in the first deposition layer, and by the third layer coalesced into large “macrocracks” running vertically through the build height. Fine, intergranular liquation “microcracks” appeared between macrocracks below the root of the final deposit layer fusion zone. Increasing the substrate preheat temperature from 165°C to 320°C deepened the partially melted zone and resulted in a more than twofold increase in the liquation microcrack density. Analysis of Scheil solidification diagrams revealed that fugitive losses of Zn and Mg during deposition increased the susceptibility to solidification cracking and promoted substrate liquation cracking. Focused electron beam (EB) conditions combined with a high aspect ratio elliptical raster pattern resulted in bands of refined, equiaxed grains. The refined microstructure suppressed solidification macrocracking and caused a nearly fivefold reduction in liquation crack density, demonstrating that beam-induced grain refinement may be a promising low-cost method for reducing hot cracking during AM.

aluminum↗
NASA NTRSDate not supplied

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↗
NASA NTRS1978

Arc termination cracks in Inconel 718 and Incoloy 903

The welding of the nickel base, heat resistant alloys that are used extensively for welded Shuttle engine components revealed solidification cracking characteristics at weld termination points. If not detected and removed, these crater cracks may cause costly component failure. To better understand this characteristic, welding termination techniques were studied and methods developed to eliminate crater cracks. It was determined that weld termination solidification cracking can be eliminated by controlled decrease of welding current, welding voltage, wire feed, and travel speed.

Bayless, E.↗
NASA NTRS2024

Welding of Crack Sensitive Aluminum Alloys for Liquid Rocket Propulsion Applications

In this welding test campaign, electron beam welding (EBW) and manual gas tungsten arc welding (GTAW) processes were utilized to join an additively manufactured aluminum alloy nozzle to a wrought aluminum flange. Both aluminum alloys were 6061, which in their conventional form are susceptible to solidification cracking issues. The AM nozzle utilized a novel high-performance modified version of 6061 which exhibits crack resistant properties during the AM process and during welding. When manually conducting GTAWs a filler wire with the same modified version of 6061 was utilized to weld different combinations of 6061 coupons (either modified or unmodified). Due to the grain refinement technology in the modified 6061, either as filler material or base material, there was complete elimination of weld solidification cracking. During EBW development a combination of wrought 6061 with a modified and additively manufactured 6061 was investigated. The EBWs developed exhibited no crack like defects. Each weld development program utilized non-destructive evaluation, metallography, and mechanical testing to determine the final weld acceptance. Mechanical testing involved hardness evaluation and tension testing on welded coupons. Both welding techniques were successfully developed and exhibited adequate properties for the final test articles and met all requirements of the development campaign. These welds were ultimately developed to be utilized on a set of all-aluminum liquid rocket nozzles to demonstrate additively manufactured aluminum alloys for propulsion applications. These aluminum nozzles were tested at NASA Marshall Space Flight Center’s hot fire test facility and subsequently underwent a test campaign involving a variety of chamber pressures and liquid propellant combinations. Following the hot fire test campaign each weldment was investigated for post operation performance and any defects that may have evolved during testing.

Welding↗
NASA NTRSDate not supplied

Al-Cu-Zn-Mg Alloy for Additive Manufacturing by Electron Beam Deposition

The application of fusion-based additive manufacturing (AM) to aircraft structural components is limited by the lack of high-strength aluminum alloys optimized for AM processing. High strength aluminum alloys (such as 7050-T7451) are difficult to process by AM because of their solidification cracking susceptibility and loss of volatile alloying elements such as Zn and Mg. The performance of a proprietary Al-Cu-Zn-Mg alloy wire feedstock was evaluated for AM utilizing electron beam deposition. Deposit microstructure, composition, occurrence of porosity and cracking, and post-heat treatment tensile and fracture toughness were correlated with deposition parameters. Post-heat treatment strength, ductility, and fracture toughness were lower than typical values for wrought 7050-T7451, related to significant losses of Zn and Mg and to porosity. Recommendations are offered for modifications to wire feedstock composition and adjustments to deposition conditions and heat treatment to enable AM of electron beam deposited material that has strength comparable to 7050-T7451 wrought products.

Al-Cu-Zn-Mg alloy, electron beam deposition, mecha↗
NASA NTRS2023

CALPHAD Models to Guide Refractory Alloys Additive Manufacturing: In-Situ Compounds Formation, Nanoparticles, and Impurities Considerations

This technical memorandum (TM) seeks to model and discuss aspects of nanoparticle and micrometer-scale particle or ‘microparticle’ inclusions in refractory metal alloy manufacturing, via a currently used additive manufacturing (AM) method that results in equivalent wt.% addition of dissolved elements in the melt pool composition and subsequent formation of nanometer-scale MC and MO inclusions. Additionally, the authors begin to consider the effects of oxygen (O), a ubiquitous impurity, in AM; and seek to understand a combined optimization of alloying, nano- and micro strengthening and refinement, elemental additions, and even in-situ compounds and alloys species formation. To gain insights, this TM focuses on a pair of refractory alloys currently of interest to NASA: tungsten-rhenium-tantalum carbide (with O impurities) (W-Re-TaC(-O)) and tungsten-rhenium-tantalum-carbon (with O impurities) (W-Re-Ta-C(-O)), which are processed via powder bed fusion (PBF)-SLM.

ICME integrated computational materials engineerin↗
NASA NTRSDate not supplied

Metallic Powder Core Tubular Wire (PCTW) Development for Additive Manufacturing

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

Marcia S Domack↗
NASA NTRS2014

Mitigation of Crack Damage in Metallic Materials

A system designed to mitigate or heal crack damage in metallic materials has been developed where the protected material or component is coated with a low-melting temperature film. After a crack is formed, the material is heated, melting the film which then infiltrates the crack opening through capillary action. Upon solidification, the healing material inhibits further crack damage in two ways. While the crack healing material is intact, it acts like an adhesive that bonds or bridges the crack faces together. After fatigue loading damages, the healing material in the crack mouth inhibits further crack growth by creating artificially-high crack closure levels. Mechanical test data show that this method sucessfully arrests or retards crack growth in laboratory specimens.

Leser, Patrick E.↗
NASA NTRS1986

Producing Refractory Microballoons

Metals, ceramics, and glasses just some of possible raw materials. Key components of equipment for new microballoon fabrication process nozzle, crucible assembly, and drop tube. Recessed, conical inner orifice aids in producing uniform, symmetrical microballoons. All-graphite crucible assembly resistant to misalinement and cracks. Drop tube ensures timely solidification of microballoons used in fluidized-bed heat exchangers; as containers for hazardous materials; catalysts in chemical and pharmaceutical processes; solid fuel for rockets; fuel containers for fusion power experiments; shock-wave dampers; and starting materials for high-strength, low-density sintered alloys and ceramics.

Lee, M. C.↗
NASA NTRS1986

Processing-structure characterization of rheocast IN-100 superalloy

The rheocasting solidification process was applied in the production of IN-100 nickel base superalloy, and the effects of processing variables, such as stirring speed, isothermal stirring time, and volume fraction solid during isothermal stirring, on the resultant rheocast structure were investigated. Ingots that were furnace cooled at the same rate but without stirring were compared with the rheocast ingots. Rheocasting yielded fine-grained structures, where the extent of microsegregation, the variation in macrostructure, and the solidification-induced porosity and ingot cracking were found to be reduced in comparison to the unstirred ingots. The grain size and nonuniformity were reduced by increasing the stirring speed, isothermal stirring time, or the volume fraction solid during stirring; decreased microsegregation was achieved by an increase in the volume fraction solid. The structures of grain boundaries lent support to the grain boundary mechanism proposed by Vogel et al. (1977) for rheocasting.

Cheng, Jung-Jen Allen↗
NASA NTRS1990

Effect of boron on intergranular hot cracking in Ni-Cr-Fe superalloys containing niobium

Solidification mechanisms had a dominant influence on microfissuring behavior of the test group. Carbon modified the Laves formation significantly and showed that one approach to alloy design would be balancing carbide formers against Laves formers. Boron's strong effect on microfissuring can be traced to its potency as a Laves former. Boron's segregation to grain boundaries plays at best a secondary role in microfissuring.

Thompson, R. G.↗
NASA NTRS1973

Additional thermal fatigue data on nickel- and cobalt-base superalloys, part 1

The fluidized bed technique was used to measure the relative thermal fatigue resistance of twenty-one superalloys. Among the thirty-six variations of composition, solidification method, and surface protection the cycles to cracking differed by two to three orders of magnitude. Some alloys suffered serious weight losses and oxidation. Thermal fatigue data, oxidation, and dimensional changes are reported. The types of superalloys are identified.

Howes, M. A. H.↗
NASA NTRS1973

Additional thermal fatigue data on nickel and cobalt-base superalloys

The fluidized bed technique was used to measure the relative thermal fatigue resistance of 21 superalloys: B1900, B1900 DID, IN-100, MAR-M 200, Udimet 700 wrought and cast, NX-188, WAZ-20, TAZ-8A, M22, IN 713C, IN 738, IN 162, MAR-M 509, Rene 80, RBH, NASA VI A, TD-NiCr, MAR-M 302, WI-52, and X-40. IN-100, MAR-M 200, NX-188, WAZ-20 and TAZ-8A were also tested in the directionally solidified form. B1900, B1900 DID, IN-100, MAR-M200, Udimet 700, NX-188, WAZ-20 and TAZ-8A were tested with surface protection. Among the 36 variations of composition, solidification method, and surface protection the cycles to cracking differed by 2 to 3 orders of magnitude. Some alloys suffered serious weight losses and oxidation. Previous fluidized bed thermal fatigue data on some of these alloys were reported in N71-10027. Thermal fatigue data, oxidation, and dimensional changes are reported in N73-30507. Metallographic and hardness data are given in this report.

Howes, M. A. H.↗
NASA NTRS1992

Effects Of B On Intergranular Hot Cracking In Ni Alloys

Report describes experiments on role of boron on solidification of 718-type nickel/chromium/iron superalloys containing niobium and relative intergranular segregations of boron, sulfur, and phosphorus in alloys. Ten alloys studied by use of light and scanning electron microscopy (SEM), energy-dispersive x-ray analysis, transmission electron microscopy (TEM) with energy-dispersive analysis of thin-film specimens, mechanical tests for susceptibility to microfissuring, differential thermal analysis (DTA), scanning Auger microscopy, and Gleeble thermal analysis.

Thompson, Raymond G.↗