Effect of heat treatment on the microstructural evolution of a nickel-based superalloy additive-manufactured by laser powder bed fusion.

Elemental segregation is a ubiquitous phenomenon in additive-manufactured (AM) parts due to solute rejection and redistribution during the solidification process. Using electron microscopy, in situ synchrotron X-ray scattering and diffraction, and thermodynamic modeling, we reveal that in an AM nickel-based superalloy, Inconel 625, stress-relief heat treatment leads to the growth of unwanted δ-phase precipitates on a time scale much faster than that in wrought alloys (minutes versus tens to hundreds of hours). The root cause for this behavior is the elemental segregation that results in local compositions of AM alloys outside the bounds of the allowable range set for wrought alloys. In situ small angle scattering experiments reveal that platelet-shaped δ phase precipitates grow continuously and preferentially along their lateral dimensions during stress-relief heat treatment, while the thickness dimension reaches a plateau very quickly. In situ XRD experiments reveal that nucleation and growth of δ-phase precipitates occur within 5 min during stress-relief heat treatment, indicating a low nucleation barrier and a short incubation time. An activation energy for the growth of δ phase was found to be (131.04 ± 0.69) kJ mol-1. We further demonstrate that a subsequent homogenization heat treatment can effectively homogenize the AM alloy and remove the deleterious δ phase. The combined experimental and modeling methodology in this work can be extended to elucidate the phase evolution during heat treatments in a broad range of AM materials.

Application of Finite Element, Phase-field, and CALPHAD-based Methods to Additive Manufacturing of Ni-based Superalloys.

Numerical simulations are used in this work to investigate aspects of microstructure and microseg-regation during rapid solidification of a Ni-based superalloy in a laser powder bed fusion additive manufacturing process. Thermal modeling by finite element analysis simulates the laser melt pool, with surface temperatures in agreement with in situ thermographic measurements on Inconel 625. Geometric and thermal features of the simulated melt pools are extracted and used in subsequent mesoscale simulations. Solidification in the melt pool is simulated on two length scales. For the multicomponent alloy Inconel 625, microsegregation between dendrite arms is calculated using the Scheil-Gulliver solidification model and DICTRA software. Phase-field simulations, using Ni-Nb as a binary analogue to Inconel 625, produced microstructures with primary cellular/dendritic arm spacings in agreement with measured spacings in experimentally observed microstructures and a lesser extent of microsegregation than predicted by DICTRA simulations. The composition profiles are used to compare thermodynamic driving forces for nucleation against experimentally observed precipitates identified by electron and X-ray diffraction analyses. Our analysis lists the precipitates that may form from FCC phase of enriched interdendritic compositions and compares these against experimentally observed phases from 1 h heat treatments at two temperatures: stress relief at 1143 K (870 °C) or homogenization at 1423 K (1150 °C).

Homogenization Kinetics of a Nickel-based Superalloy Produced by Powder Bed Fusion Laser Sintering.

Additively manufactured (AM) metal components often exhibit fine dendritic microstructures and elemental segregation due to the initial rapid solidification and subsequent melting and cooling during the build process, which without homogenization would adversely affect materials performance. In this letter, we report in situ observation of the homogenization kinetics of an AM nickel-based superalloy using synchrotron small angle X-ray scattering. The identified kinetic time scale is in good agreement with thermodynamic diffusion simulation predictions using microstructural dimensions acquired by ex situ scanning electron microscopy. These findings could serve as a recipe for predicting, observing, and validating homogenization treatments in AM materials.

Antimicrobial properties of a multi-component alloy.

High traffic touch surfaces such as doorknobs, countertops, and handrails can be transmission points for the spread of pathogens, emphasizing the need to develop materials that actively self-sanitize. Metals are frequently used for these surfaces due to their durability, but many metals also possess antimicrobial properties which function through a variety of mechanisms. This work investigates metallic alloys comprised of several metals which individually possess antimicrobial properties, with the target of achieving broad-spectrum, rapid sanitation through synergistic activity. An entropy-motivated stabilization paradigm is proposed to prepare scalable alloys of copper, silver, nickel and cobalt. Using combinatorial sputtering, thin-film alloys were prepared on 100 mm wafers with ≈50% compositional grading of each element across the wafer. The films were then annealed and investigated for alloy stability. Antimicrobial activity testing was performed on both the as-grown alloys and the annealed films using four microorganisms-Phi6, MS2, Bacillus subtilis and Escherichia coli-as surrogates for human viral and bacterial pathogens. Testing showed that after 30 s of contact with some of the test alloys, Phi6, an enveloped, single-stranded RNA bacteriophage that serves as a SARS-CoV-2 surrogate, was reduced up to 6.9 orders of magnitude (> 99.9999%). Additionally, the non-enveloped, double-stranded DNA bacteriophage MS2, and the Gram-negative E. coli and Gram-positive B. subtilis bacterial strains showed a 5.0, 6.4, and 5.7 log reduction in activity after 30, 20 and 10 min, respectively. Antimicrobial activity in the alloy samples showed a strong dependence on the composition, with the log reduction scaling directly with the Cu content. Concentration of Cu by phase separation after annealing improved activity in some of the samples. The results motivate a variety of themes which can be leveraged to design ideal antimicrobial surfaces.

Nitrogen Effects in Additively Manufactured Martensitic Stainless Steels: Conventional Thermal Processing and Comparison with Wrought.

The microstructures of additively manufactured (AM) precipitation-hardenable stainless steels 17-4 and 15-5 were investigated and compared to those of conventionally produced materials. The residual N found in N2-atomized 17-4 powder feedstock is inherited by the additively produced material, and has dramatic effects on phase stability, microstructure, and microstructural evolution. Nitrogen is a known austenite stabilizing element, and the as-built microstructure of AM 17-4 can contain up to 90 pct or more retained austenite, compared to the nearly 100 pct martensite structure of wrought 17-4. Even after homogenization and solutionization heat treatments, AM 17-4 contains 5 to 20 pct retained austenite. In contrast, AM 15-5 and Ar-atomized AM 17-4 contain<5 pct retained austenite in the as-built condition, and this level is further decreased following post-build thermal processing. Computational thermodynamics-based calculations qualitatively describe the observed depression in the martensite start temperature and martensite stability as a function of N-content, but require further refinements to become quantitative. A significant increase in the volume fraction of fine-scale carbide precipitates attributed to the high N-content of AM 17-4 is also hypothesized to give rise to additional activation barriers for the dislocation motion required for martensite nucleation and subsequent growth. An increase in the volume fraction of carbide/nitride precipitates is observed in AM 15-5, although they do not inhibit martensite formation to the extent observed in AM 17-4.

Systems Design Approach to Low-Cost Coinage Materials.

A systems approach within an Integrated Computational Materials Engineering framework was used to design three new low-cost seamless replacement coinage alloys to reduce the raw material of the current US coinage alloys. Maintaining compatibility with current coinage materials required matching the currently used alloy properties of yield strength, work-hardening behavior, electrical conductivity, color, corrosion resistance and wear resistance. In addition, the design alloys were required to use current production processes. CALPHAD-based models for electrical conductivity and color were developed to integrate into the system design. Three prototype alloys were designed, produced and characterized. The design process highlighted the trade-off between minimizing the raw material costs and achieving the desired color properties. Characterization of the three prototype alloys showed good agreement with the design goals.