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Microstructure control of in situ metal matrix nanocomposites (MMNCs) poses a barrier to their large-scale production. Here, we interrogate in unprecedented detail the formation mechanisms, morphologies, and microstructures of an in situ Al/TiC MMNC processed via salt flux reaction. Through synchrotron-based X-ray nanotomography (TXM) and scanning and transmission electron microscopy, we visualize in over five orders-of-magnitude of length-scale the TiC nanoparticles, Al_3Ti intermetallics, and their co-locations. 3D reconstructions from TXM revealed a surprising variety of Al_3Ti morphologies, including an orthogonal plate structure. By combining our experimental results with phase-field simulations, we demonstrate that this growth form originates from the intermetallic nucleating epitaxially on a TiC particle which is larger than a critical size at a given undercooling. Yet TiC particles that are too small to nucleate Al_3Ti can also impact the growth of the intermetallic, by splitting the intermetallic plates during solidification. These insights on the divalent roles of the nanoparticles offer general guidelines for the synthesis and processing of MMNCs. 

We investigate the coarsening dynamics of the three-phase eutectic Al-Ag2Al-Al2Cu at 723 K via in situ transmission X-ray nano-tomography. Unlike previous investigations that compared observations between different samples annealed for different times, our three-dimensional measurement shows at nanoscale resolution the microstructural changes occurring in the same field-of-view, enabling new insight on the capillary-driven evolution of a ladder-like pattern. With the aid of a new reconstruction algorithm and machine learning segmentation, we trace the interfaces of the eutectic and observe significant structural changes within 4 hr. of aging. Even though the average length-scales of the eutectic solids follow a temporal power law, the microstructure is not self-similar. Instead, it evolves (in part) through the coalescence of neighboring Ag2Al solids at the expense of the intervening Al2Cu. By combining our X-ray data with electron diffraction to identify the common planes at the interphase boundaries, we show that coalescence leads to a decrease in lattice misfit, and hence, interfacial energy. At longer times, the interphase boundaries with low misfit compete for surface area, resulting in a ‘locking’ of the interfacial shape. 

Abstract We present a phase-field (PF) model to simulate the microstructure evolution occurring in polycrystalline materials with a variation in the intra-granular dislocation density. The model accounts for two mechanisms that lead to the grain boundary migration: the driving force due to capillarity and that due to the stored energy arising from a spatially varying dislocation density. In addition to the order parameters that distinguish regions occupied by different grains, we introduce dislocation density fields that describe spatial variation of the dislocation density. We assume that the dislocation density decays as a function of the distance the grain boundary has migrated. To demonstrate and parameterize the model, we simulate microstructure evolution in two dimensions, for which the initial microstructure is based on real-time experimental data. Additionally, we applied the model to study the effect of a cyclic heat treatment (CHT) on the microstructure evolution. Specifically, we simulated stored-energy-driven grain growth during three thermal cycles, as well as grain growth without stored energy that serves as a baseline for comparison. We showed that the microstructure evolution proceeded much faster when the stored energy was considered. A non-self-similar evolution was observed in this case, while a nearly self-similar evolution was found when the microstructure evolution is driven solely by capillarity. These results suggest a possible mechanism for the initiation of abnormal grain growth during CHT. Finally, we demonstrate an integrated experimental-computational workflow that utilizes the experimental measurements to inform the PF model and its parameterization, which provides a foundation for the development of future simulation tools capable of quantitative prediction of microstructure evolution during non-isothermal heat treatment.