Phase Fraction and Evolution of Additively Manufactured (AM) 15-5 Stainless Steel and Inconel 625 AM-Bench Artifacts.

A proper understanding of the structure and microstructure of additively manufactured (AM) alloys is essential not only to the prediction and assessment of their material properties, but also to the validation and verification of computer models needed to advance AM technologies. To accelerate AM development, as part of the AM-Bench effort, we conducted rigorous synchrotron-based X-ray scattering and diffraction experiments on two types of AM alloys (AM 15-5 stainless steel and AM Inconel 625). Taking advantage of the high penetration of synchrotron hard X-rays, we determined the phases present in these alloys under different build conditions and their statistically meaningful phase fractions using high-resolution X-ray diffraction. Using in situ multi-scale X-ray scattering and diffraction, we quantitatively analyzed the phase evolution and development of major precipitates in these alloys as a function of time during stress relief heat treatments. These results serve to validate AM microstructure models and provide input to higher-level AM processing and property models to predict the material properties and performances.

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.