No abstract

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).

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.

The microstructural evolution of laser powder-bed additively manufactured Inconel 625 during a post-build stress-relief anneal of 1 hour at 1143 K (870°C) is investigated. It is found that this industry-recommended heat treatment promotes the formation of a significant fraction of the orthorhombic D0 a Ni 3 Nb d-phase. This phase is known to have a deleterious influence on fracture toughness, ductility, and other mechanical properties in conventional, wrought Inconel 625; and is generally considered detrimental to materials' performance in service. The d-phase platelets are found to precipitate within the inter-dendritic regions of the as-built solidification microstructure. These regions are enriched in solute elements, particularly Nb and Mo, due to the micro-segregation that occurs during solidification. The precipitation of d-phase at 1073 K (800°C) is found to require up to 4 hours. This indicates a potential alternative stress-relief processing window that mitigates d-phase formation in this alloy. Ultimately, a homogenization heat treatment is recommended for additively manufactured Inconel 625 because the increased susceptibility to d-phase precipitation increases the possibility for significant degradation of materials' properties in service.

No abstract

Gold deposition on rotating disk electrodes, Bi 3+ adsorption on planar Au films and superconformal Au filling of trenches up to 45 μm deep are examined in Bi 3+ -containing Na 3 Au(SO 3 ) 2 electrolytes with pH between 9.5 and 11.5. Higher pH is found to increase the potential-dependent rate of Bi 3+ adsorption on planar Au surfaces, shortening the incubation period that precedes active Au deposition on planar surfaces and bottom-up filling in patterned features. Decreased contact angles between the Au seeded sidewalls and bottom-up growth front also suggest improved wetting. The bottom-up filling dynamic in trenches is, however, lost at pH 11.5. The impact of Au concentration, 80 mmol/L versus 160 mmol/L Na 3 Au(SO 3 ) 2 , on bottom-up filling is examined in trenches up to ≈ 210 μm deep with aspect ratio of depth/width ≈ 30. The microstructures of void-free, bottom-up filled trench arrays used as X-ray diffraction gratings are characterized by scanning electron microscopy (SEM) and Electron Backscatter Diffraction (EBSD), revealing marked spatial variation of the grain size and orientation within the filled features.

This work extends previously detailed void-free, bottom-up feature filling in a near-neutral Na 3 Au(SO 3 ) 2 + Na 2 SO 3 electrolyte containing micromolar concentrations of Bi 3+ . Bottom-up electrodeposition in 17 μm and 45 μm tall trenches with an aspect ratio greater than 10 is demonstrated using potentiostatic, stepped potential and/or stepped current control. Strategies to shorten the incubation period associated with slow deposition on uniformly passivated surfaces, which precedes bottom-up filling at fixed potential, are explored. The first electron backscatter diffraction studies of bottom-up filled Au deposits reveal large grains that span the trench width and often exceed tens of micrometers in length. In contrast, smaller grains are observed near the tops of filled trenches and, under conditions of marginal filling, mid-height within them.

The lack of an engaging pedagogy and the highly competitive atmosphere in introductory science courses tend to discourage students from pursuing science, technology, engineering, and mathematics (STEM) majors. Once in a STEM field, academic and social integration has been long thought to be important for students’ persistence. Yet, it is rarely investigated. In particular, the relative impact of in-class and out-of-class interactions remains an open issue. Here, we demonstrate that, surprisingly, for students whose grades fall in the “middle of the pack,” the out-of-class network is the most significant predictor of persistence. To do so, we use logistic regression combined with Akaike’s information criterion to assess in- and out-of-class networks, grades, and other factors. For students with grades at the very top (and bottom), final grade, unsurprisingly, is the best predictor of persistence—these students are likely already committed (or simply restricted from continuing) so they persist (or drop out). For intermediate grades, though, only out-of-class closeness—a measure of one’s immersion in the network—helps predict persistence. This does not negate the need for in-class ties. However, it suggests that, in this cohort, only students that get past the convenient in-class interactions and start forming strong bonds outside of class are or become committed to their studies. Since many students are lost through attrition, our results suggest practical routes for increasing students’ persistence in STEM majors.