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The relationship between acoustic emission (AE) and damage source areas in SiC/SiC minicomposites was modeled using insights from tensile testing in-scanning electron microscope (SEM). Damage up to matrix crack saturation was bounded by: (1) AE generated by matrix cracking (lower bound) and (2) AE generated by matrix cracking, and fiber debonding and sliding in crack wakes (upper bound). While fiber debonding and sliding exhibit lower strain energy release rates than matrix cracking and fiber breakage, they contribute significant damage area and likely produce AE. Fiber breaks beyond matrix crack saturation were modeled by two conditions: (i) only fiber breaks generated AE; and (ii) fiber breaks occurred simultaneously with fiber sliding to generate AE. While fiber breaks are considered the dominant late-stage mechanism, our modeling indicates that other mechanisms are active, a finding that is supported by experimental in-SEM observations of matrix cracking in conjunction with fiber failure at rupture.

The Alnico 8 alloy has been printed using the selective laser melting additive manufacturing approach, resulting in material with magnetic properties in the as-printed state comparable to properties produced by conventional casting or powder metallurgy routes. Microstructural characterization in 3D, via electron backscattered diffraction (EBSD) in a TriBeam microscope, simultaneously reveals a fine-scale grain structure, grain orientations and sub-grain misorientation gradients as a function of proximity to spherical pores that form during the print process. The nanostructure of the 3D printed part has the same highly coherent spinodal α 1 / / α 2 structure observed in conventionally fabricated Alnico 8, which gives rise to a coercivity ( H c ) of 51.2 kA m - 1 . Further investigation of the phase constituents by TEM analysis provides an understanding of the microstructure evolution during the additive manufacturing process. Modified processing pathways for improved microstructure and properties are discussed.

A multi-modal data-merging framework that enables the reconstruction of slip bands in three dimensions over millimeter-scale fields of view is presented. The technique combines 3D electron back-scattered diffraction (EBSD) measurements with high-resolution digital image correlation (HR-DIC) information collected in the scanning electron microscope (SEM). A typical merging workflow involves the segmentation of features within the strain field (slip bands, deformation twins) and the microstructure (grains), alignment of datasets and the projection of slip bands into the 3D microstructure, using the knowledge of the local crystallographic orientation. This method is demonstrated in two materials: a face-centered cubic (FCC) nickel-base superalloy and hexagonal close-packed (HCP) titanium alloy.

In this work, we demonstrate that damage mechanism identification from acoustic emission (AE) signals generated in minicomposites with elastically similar constituents is possible. AE waveforms were generated by SiC/SiC ceramic matrix minicomposites (CMCs) loaded under uniaxial tension and recorded by four sensors (two models with each model placed at two ends). Signals were encoded with a modified partial power scheme and subsequently partitioned through spectral clustering. Matrix cracking and fiber failure were identified based on the frequency information contained in the AE event they produced, despite the similar constituent elastic properties of the matrix and fiber. Importantly, the resultant identification of AE events closely followed CMC damage chronology, wherein early matrix cracking is later followed by fiber breaks, even though the approach is fully domain-knowledge agnostic. Additionally, the partitions were highly precise across both the model and location of the sensors, and the partitioning was repeatable. The presented approach is promising for CMCs and other composite systems with elastically similar constituents.

The mechanical properties of superalloys are strongly governed by the resistance to shearing of ordered precipitates by dislocations. In the operating environments of superalloys, the stresses and temperatures present during thermomechanical loading influence the dislocation shearing dynamics, which involve diffusion and segregation processes that result in a diverse array of planar defects in the ordered L12γ′ precipitate phase. This review discusses the current understanding of high-temperature deformation mechanisms of γ′ precipitates in two-phase Ni-, Co-, and CoNi-base superalloys. The sensitivity of planar fault energies to chemical composition results in a variety of unique deformation mechanisms, and methods to determine fault energies are therefore reviewed. The degree of chemical segregation in the vicinity of planar defects reveals an apparent phase transformation within the parent γ′ phase. The kinetics of segregation to linear and planar defects play a significant role in high-temperature properties. Understanding and controlling fault energies and the associated dislocation dynamics provide a new pathway for the design of superalloys with exceptional properties.

The developing roles of damage mechanisms in the failure response of SiC/SiC minicomposites was investigated by the characterization of microscale damage accumulation with respect to microstructure. A multi-modal approach combining spatially resolved acoustic emission (AE) with tensile testing in-SEM (scanning electron microscope) was used to simultaneously examine surface (observed in-SEM) and bulk damage (monitored via AE). Strong agreement was shown between the evolving crack density estimated by AE and in-SEM measurements. The following were observed: (i) in-plane matrix content and distribution impacted crack growth; (ii) spatially-distributed matrix cracks generated varying stress-dependent AE; and (iii) certain individual cracks became more probable failure locations due to unique combinations of damage mechanisms that drove their growth. This approach enabled characterizing potential failure determinants and suggests that early damage behavior is related to certain microstructural features (e.g. surface flaws), while subsequent damage behavior is coupled to interactions of local mechanisms evolving with stress.

The details of polycrystalline microstructure often influence the early stages of yielding and strain localization under monotonic and cyclic loading, particularly in elastically anisotropic materials. A new software package, MechMet (mechanical metrics) provides a convenient finite element tool for solving field equations for elasticity in polycrystals in conjunction with investigations of microstructure-induced heterogeneity. The simulated displacement field is used to compute several mechanical metrics, such as the strain and stress tensors, directional stiffness, relative Schmid factor, and the directional strength-to-stiffness ratio. The virtual polycrystal finite element meshes needed by MechMet can be created with the Neper package or any other method that produces a 10-node, tetrahedral, serendipity element. Formatted output files are automatically generated for visualization with Paraview or VisIt. This paper presents an overview of the MechMet package and its application to polycrystalline materials of both cubic and hexagonal structures.

Titanium alloys are processed to develop a wide range of microstructure configurations and therefore material properties. While these properties are typically measured experimentally, a framework for property prediction could greatly enhance alloy design and manufacturing. Here a microstructure-sensitive framework is presented for the prediction of strength and ductility as well as estimates of the bounds in variability for these properties. The framework explicitly considers distributions of microstructure via new approaches for instantiation of structure in synthetic samples. The parametric evaluation strategy, including the finite element simulation package FEpX, is used to create and test virtual polycrystalline samples to evaluate the variability bounds of mechanical properties in Ti-6Al-4V. Critical parameters for the property evaluation framework are provided by measurements of single crystal properties and advanced characterization of microstructure and slip system strengths in 2D and 3D. Property distributions for yield strength and ductility are presented, along with the validation and verification steps undertaken. Comparisons between strain localization and slip activity in virtual samples and in experimental grain-scale strain measurements are also discussed.

During service, superalloy turbine components degrade over time by creep and fatigue deformation mechanisms due to a complex combination of stresses at high temperatures. The high cost of fabricating Ni-base superalloy components and, consequently, replacement components has encouraged the development of rejuvenation (restoration) procedures to extend useful service life. The processes that limit repeated rejuvenation of directionally solidified GTD444 and single-crystal Rene N5(SX) alloys have been studied in detail. A rejuvenation cycle includes a rejuvenation heat treatment and/or small-scale material removal, followed by creep or fatigue testing. With the application of multiple rejuvenation cycles, the total creep rupture life of Rene N5(SX) tested at 982 °C and 206 MPa was extended by a factor of 2.8 over the baseline rupture life. To produce this increase in rupture life, creep strains were limited to 2 or 3 pct prior to application of a rejuvenation cycle, involving solutioning at 28 °C below the $$\gamma ^{\prime }$$ solvus temperature for 2 hours and aging at 1079 °C for 4 hours. Rejuvenation of compressive hold-time fatigue damage was also successful with the use of small-scale material removal. Due to the tortuosity of the grain boundaries in GTD444(DS), some boundaries are initially oriented transverse to the growth direction. The enhanced plasticity near these grain boundaries may be the primary reason why the initially single-crystal Rene N5(SX) specimens were more amenable to rejuvenation than GTD444(DS). For both alloys, recrystallization after multiple rejuvenation cycles was responsible for early failure during the subsequent creep test. Resonant ultrasound spectroscopy was successfully implemented to detect the presence of recrystallized grains.

The microstructural origins of highly localized elastic strain concentrations in polycrystalline microstructures under monotonic loading are studied using grain-scale, in situ digital image correlation and crystal plasticity finite element method. It is shown that the locations of exceptionally high elastic strain concentrations in the microstructure depend on particular crystallographic and morphological orientations of grains and less so on crystalline details of their local neighborhood. Based on these results, we discuss how topological and crystallographic features of annealing twin boundaries can increase the likelihood of slip band initiation throughout the microstructure of polycrystalline Ni-base superalloys.

Additive manufacturing (AM) is a new and promising production methodology adept at producing complex geometries, which can be optimized for lower weight and enhanced capabilities. The material properties of these additive components are dictated by the microstructures developed during processing, with a high sensitivity to grain structure and associated anisotropy. With this new processing modality comes the added difficulty of understanding the thermodynamics and kinetic mechanisms that dictate the evolution of microstructure. This research addresses the unique thermal conditions present in AM and the pathways for grain refinement in nanofunctionalized aluminum alloys. The Al-Ta system, in which Al3Ta intermetallic compounds are demonstrated to have substantial grain refining capacity, are the focus of this study. The grain size is shown to be reduced relative to pure aluminum by 1000X when tantalum is added at 1 vol%. The effectiveness of the Al3Ta intermetallic is dictated by the crystallography and availability of the inoculant phase under AM conditions.

Additive manufacturing (AM) promises a major transformation for manufacturing of metallic components for aerospace, medical, nuclear, and energy applications. This perspective paper addresses some of the opportunities for alloy and feedstock design to achieve site-specific and enhanced properties not attainable by conventional manufacturing processes. This paper provides a brief overview of the role of powders, as well as solidification and solid-state phase transformation phenomena typically encountered during fusion-based AM. Three case studies are discussed that leverage the above to arrive at microstructure control. The first case study focuses on approaches to modify the solidification characteristics by in-situ alloying. The second case study focuses on the need for concurrent design of alloys and processing conditions to arrive at the columnar to equiaxed transition during solidification. The third case study focuses on the design of a cobalt alloy for AM, with emphasis on tailoring liquid and solid state phase transformations. The need for comprehensive knowledge of processing conditions during AM, in-situ and ex-situ probing of microstructure development under AM conditions, and post-print processing, characterization, and qualification are articulated for the design of future alloys and component geometries built by AM.

Pathways for ductility Alloys containing multiple elements can be very strong but often suffer from poor ductility. F. Wang et al. found that different mechanisms accommodated plasticity in a molybdenum-niobium-titanium multiprincipal element alloy (see the Perspective by Cairney). Instead of so-called “screw” dislocations, deformation is accommodated by multiple pathways that include “edge” dislocations and activation of crystallographic slip planes. These results offer a design paradigm for developing new high-strength alloys. Science , this issue p. 95 ; see also p. 37

The development of overgrown grains during sub-solvus annealing of a polycrystalline γ − γ ′ nickel-base alloy is investigated, with special emphasis on the primary γ′ precipitates. Quantitative analysis conducted on a large three-dimensional electron back-scattered diffraction dataset reveals a high fraction of γ′ precipitates on the annealing twin boundaries in the large grains. When observed in-situ in a scanning electron microscope, the formation of annealing twins is correlated to the crossing of γ′ precipitates by moving grain boundaries. The role of precipitates in the occurrence of growth accidents is discussed.

Background: Advancements in the Digitial Image Correlation (DIC) technique over the past decade have greatly improved spatial resolution. However, many processes, such as plastic deformation, have a temporal component spanning from fractions of a second to minutes that has not yet been addressed in detail, particularly for DIC conducted in-situ in the scanning electron microscope (SEM). Objective: To develop a methodology for conducting time-resolved digital image correlation in the SEM for analysis of time-dependent mechanical deformation phenomena. Methods: Microscope and electron beam scanning parameters that influence the rate at which time-resolved DIC information is mapped are experimentally investigated, providing a guide for use over a range of timescales and resolutions. Results: Time-resolved DIC imaging is demonstrated on a Ti-7Al alloy, where slip band propagation is resolved with imaging dwell times of seconds. The limits of strain resolution and strain collection speeds are analyzed. Conclusions: The new developed methodology can be applied to a wide range of materials loaded in-situ to quantify time-dependent plastic deformation phenomena.

The possibility of designing multi-principal element alloys in the Ni-Co-Ru system is investigated by first-principles and experimental means. A high-throughput first-principles approach is employed to probe the effect of composition on planar fault energies. Of most interest, a FCC alloy, Ni40Co40Ru20, exhibits a high room temperature strength compared to existing nickel-containing solid solution FCC high entropy alloys. The presence of Ru imparts the alloy with unique properties. First, the low stacking fault energy provides a low critical resolved shear stress for twinning, allowing a TWIP effect. Second, the high lattice friction and the associated high yield strength enables the critical resolved shear stress for twinning to be reached at low strains at room temperature, resulting in the formation of a dense network of planar defects for increased work hardening. A TRIP effect is also observed at higher strains at room temperature.

A new approach which involves a diffuse multi-layer fault model coupled with a cluster approach to statistical mechanics (CASM) infrastructure has been developed to identify the proximate structure for the antiphase boundary (APB) on {111} planes in L12. We report a new structure, ‘ γ a ′ ’ which approximates the bonding environment of an APB better than a previously reported structure, ‘ω’. Density functional theory calculations were employed to predict the APB energies from structural energies of γ a ′ and L12 and were validated against estimations from supercell methods for several binary compounds. The implications of the discovery of the γ a ′ are discussed.

International audience; Fatigue crack nucleation in crystalline materials typically develops due to highly localized cyclic slip. During a fatigue cycle, reverse slip differs locally from slip in the forward direction particularly in precipitate-containing materials such as superalloys. In this paper we report the first direct measurements of irreversibility at the scale of individual slip bands by high-resolution digital image correlation (DIC) in a polycrystalline nickel-based superalloy. Quantitative measurements of the slip irreversibility are challenging for regions of material that have a size that captures the microstructure and its variability. High spatial resolution at the nanometer scale during experimental measurements is needed to observe slip localization during deformation. Moreover, large fields are also needed to obtain the material response over statistically representative populations of microstructural configurations. Recently, high resolution scanning electron microscope (SEM) digital image correlation (DIC) has been extended for quantitative analysis of discontinuities induced by slip events using the Heaviside-DIC method. This novel method provides quantitative measurements of slip localization at the specimen surface. In this paper, the Heaviside-DIC method is used to measure slip irreversibility and plastic strain accumulation in a nickel-based superalloy. The method detects bands with high levels of irreversibility early in cycling that ultimately form fatigue cracks upon further cycling. The local microstructural configurations that induce large amounts of plasticity and slip irreversibility are correlated to crack nucleation locations.

Nondestructive X-ray diffraction contrast tomography imaging was used to characterize the microstructure evolution in a polycrystalline bulk strontium titanate specimen. Simultaneous acquisition of diffraction and absorption information allows for the reconstruction of shape and orientation of more than 800 grains in the specimen as well as porosity. Three-dimensional microstructure reconstructions of two coarsening states of the same specimen are presented alongside a detailed exploration of the crystallographic, topological and morphological characteristics of the evolving microstructure. The overall analysis of the 3D structure shows a clear signature of the grain boundary anisotropy, which can be correlated to surface energy anisotropy: the grain boundary plane distribution function shows an excess of 〈100〉-oriented interfaces with respect to a random structure. The results are discussed in the context of interface property anisotropy effects.

A sample of 304L stainless steel manufactured by Laser Engineered Net Shaping (LENS) was characterized in 3D using TriBeam tomography. The crystallographic, structural, and chemical properties of the as-deposited microstructure have been studied in detail. 3D characterization reveals complex grain morphologies and large orientation gradients, in excess of 10∘, that are not easily interpreted from 2D cross-sections alone. Misorientations were calculated via a methodology that locates the initial location and orientation of grains that grow during the build process. For larger grains, misorientation increased along the direction of solidification. For grains with complex morphologies, K-means clustering in orientation space is demonstrated as a useful approach for determining the initial growth orientation. The gradients in misorientation directly tracked with gradients in chemistry predicted by a Scheil analysis. The accumulation of misorientation is linked to the solutal and thermal solidification path, offering potential design pathways for novel alloys more suited for additive manufacturing.