Solidification processing offers the first opportunity to control microstructure, properties, and performance in metallic alloy components. Until recently, microstructural evaluations were limited to post-solidification characterization by destructive methods. We review the development of time-resolved, in situ imaging techniques capable of capturing solid–liquid interfacial evolution in metallic alloys with high spatial and temporal resolution under diverse solidification conditions relevant for applications ranging from conventional directional solidification, crystal growth, and casting, to welding and additive manufacturing. These experiments enable direct visualization of transient behaviors that would otherwise remain unknown, uniquely providing insights into the physics that impact microstructure and defect development, and strategies for microstructural control and defect mitigation. Understanding microstructural evolution and the characteristics that form under various solidification conditions is essential for the development of multiscale, experimentally informed predictive modeling. This is highlighted by solidification simulations that utilize in situ measurements of solidification dynamics from state-of-the-art experimental techniques.

In this work, the correlation between magnetic-domain structure and microstructure in combined reaction-processed equiatomic L10 FePd has been investigated using magnetic force microscopy. The microstructure consisted of approximately equiaxed grains with an average grain size of ∼1 μm and a grain size distribution ranging from below the theoretical critical domain size (Dcrit∼0.2–0.3 μm) up to approximately 5 μm in diameter. The domain structure was characterized as “mixed” in nature, consisting of smaller single-domain grains, larger multidomain grains, and a larger scale interaction domain structure encompassing many grains. The domain boundaries separating interaction domains tended to lie along grain boundaries, and it is proposed that the observed interaction domains should be considered in descriptions of the magnetization and magnetization reversal behavior of this material. In particular, pinning of interaction domain walls by intragranular features of the microstructure such as grain boundaries and single-domain grains could play a role in the measured coercivities.

Excimer-laser-induced rapid lateral solidification was used to produce large grain microstructures in copper and silver thin films. These were multilayer thin film structures consisting of sputter deposited copper and silver thin films encapsulated by silica (SiO2/metal/SiO2/Si substrate). In this process, a single excimer laser pulse and projection imaging optics were used to melt a 60 micron wide line in the metal film. The resolidification of the melted lines is found to occur laterally in the plane of the film, resulting in grains greater than 20 um in length and 1 um wide. Electron diffraction analysis allowed identification of a strong <001> texture in the growth direction along the major axis of the elongated grains as well as similar texture parallel to the film surface. Various dislocation and faulted defect structures are identified and examined in the context of the rapid solidification and potential application to interconnects.

The role of slip transfer processes across the heterophase interfaces in two-phase TiAl intermetallics has been studied. Polysynthetically twinned crystals of TiAl (PST-TiAl) have been used as model systems for individual grains in technologically relevant polycrystalline lamellar TiAl alloys. Compressive plastic loads have been applied for orientations of the lamellar interfaces parallel and perpendicular to the loading directions to produce hard mode slip activity. Transmission electron microscopy has been used to determine the active deformation modes in the constituent phases and to study the slip transfer across heterophase interfaces. The results are discussed with respect to the mechanical behavior of PST-TiAl and lamellar TiAl alloys, which is of relevance to in-service performance and metallurgical processing operations.

Planar defects produced in L10-ordered FePd during annealing after cold-deformation in the disordered cubic state have been characterized by transmission electron microscopy (TEM). The defects evolving during annealing include arrays of overlapping stacking faults (SF's), {111}-conjugated microtwins (μT's) and thermal antiphase boundaries (APB's). The defect formation mechanisms proposed here are similar to twinning mechanism reported for FCC-metals during annealing. Thus, SF arrays and faulted μT's in the L10-ordered FePd appear to form during the early stages of annealing by atomic attachment faulting on {111}-facets of the transformation interfaces. During later stages of annealing the reduced amount and the change in nature of the driving forces for the microstructural rearrangement result in changes in the predominant defect formation mechanism. The features of the defect genesis in L10-FePd are discussed with respect to solid-state transformations during processing of these ferromagnetic intermetallics.

Thermo mechanical processing of equiatomic FePd has been used to establish a nearly equiaxed microstructure that consists of mono-variant L10 ordered grains. The technically important hard magnetic properties, e.g. coercivity, of the uniaxial ferromagnetic L10-FePd with equiaxed microstructure depend on the grain size. Thus, here, the evolution of grain size during the later stages of annealing has been studied using SEM and computer assisted image analysis with the goal to determine the activation parameters for the relevant coarsening processes. Using a classical grain growth analysis the activation parameter for coarsening of the 5% largest grains in the populations of L10-ordered grains in FePd has been determined as approximately 30kcal/mol.

The role of slip transfer processes across the heterophase interfaces in two-phase TiAl intermetallics has been studied. Polysynthetically twinned crystals of TiAl (PST-TiAl) have been used as model systems for individual grains in technologically relevant polycrystalline lamellar TiAl alloys. Compressive plastic loads have been applied for orientations of the lamellar interfaces parallel and perpendicular to the loading directions to produce hard mode slip activity. Transmission electron microscopy has been used to determine the active deformation modes in the constituent phases and to study the slip transfer across heterophase interfaces. The results are discussed with respect to the mechanical behavior of PST-TiAl and lamellar TiAl alloys, which is of relevance to in-service performance and metallurgical processing operations.

The fine structure and the character of a dislocations on prism planes have been determined for room-temperature deformed polycrystalline Ti3Al using a combination of experimental and computational techniques of transmission electron microscopy (TEM). Within the resolution limits of the weak-beam technique the fine structure of prism plane a dislocations in Ti3Al is found to be planar and to comprise only a single ribbon of antiphase boundary and no experimentally observable stacking faults.