Far-field High-energy Diffraction Research Articles

3D in situ observations of stress redistribution in Ti-6Al-4V within rogue grain neighborhoods during monotonic and cyclic loading

Grain-scale stress redistribution events are characterized within the Ti-6Al-4V (Ti64) hexagonal close-packed α phase using far-field high-energy X-ray diffraction microscopy. Specimens were deformed in monotonic uniaxial tension and under cyclic tensile loading with approximately 7000 grains probed in each specimen. Analyses focused on the evolution of the resolved shear stresses applied to the basal 〈a〉, prismatic 〈a〉, and pyramidal 〈c+a〉 slip systems, as well as normal stresses applied to basal planes, within individual grains. Slip system softening is observed in the basal 〈a〉 and prismatic 〈a〉 slip systems across the ensemble, while hardening is observed for the pyramidal 〈c+a〉 slip systems during both monotonic and cyclic loading. In addition, discrete stress redistribution events in which increases of normal stresses in grains not favorably oriented for slip that may lead to crack initiation are analyzed. It is observed that these increases in normal stresses are correlated to crystallographic slip in multiple neighboring grains favorably oriented for slip.

Exploring the role of Type-II residual stresses in a laser powder bed fusion nickel-based superalloy using measurement and modeling

Far-field high-energy X-ray diffraction microscopy (ff-HEDM) and the crystal plasticity finite element method (CPFEM) are used to investigate the role of grain-scale (Type-II) residual stresses on the fatigue life of additively manufactured (AM) Inconel alloy 625 (IN-625). Grain-averaged orientations, centroids, and residual elastic strain tensors from ff-HEDM data are used to instantiate a crystal plasticity model to simulate the effect of residual stresses at the grain scale. Simulation results indicate that the presence of tensile residual strains increase stress localization and heterogeneity within grains, triggering an earlier onset of plasticity. A microscale fatigue indicator parameter (FIP) is computed to model the impact of these residual strains on the cycles to fatigue crack nucleation. The crack nucleation model, based on the computed FIPs, predicts a significant reduction in the number of cycles for fatigue crack nucleation for mid- and high-cycle fatigue due to the residual strain induced localization, while the residual strains have minimal impact on low-cycle fatigue life.

Mapping 3D grain and precipitate structure during in situ mechanical testing of open-cell metal foam using micro-computed tomography and high-energy X-ray diffraction microscopy

• 3D grain structure is mapped and tracked during loading of open-cell metal foam. • Challenges included sample size relative to beam size and large ligament motions. • X-ray CT and far-field HEDM measurements collected at incremental displacements. • New scanning and stitching methodology established for far-field HEDM measurements. • Ligament-tracking code used to express crystal orientation in local reference frame. Open-cell metal foams are ultra-low-density cellular metals with complex hierarchical structures that span bulk, cell, ligament, and sub-ligament scales and give rise to desirable properties such as high strength-to-weight ratio and excellent energy absorption. Although literature suggests that intrinsic material structures at sub-ligament length scales (e.g., grains and precipitates) play an important role in mechanical behavior of open-cell metal foams, there are very few experimental measurements of such structures in three dimensions and for meaningful volumes of foam. This study seeks to map and track the three-dimensional (3D) grain and precipitate structures of an intact volume of open-cell aluminum foam by advancing microstructural characterization techniques that leverage X-ray micro-computed tomography ( μ CT ) and far-field high-energy X-ray diffraction microscopy (FF-HEDM). A 6%-relative-density aluminum foam sample was mechanically tested in compression while μ CT and FF-HEDM measurements were collected at interrupted loading states at beamline 1-ID of the Advanced Photon Source. A new scanning strategy and reconstruction algorithm were established to enable characterization of a foam volume with diameter approximately four times wider than the nominal width of the X-ray beam. The result is a set of maps that detail both the 3D grain and precipitate structures throughout the foam volume at successive strain steps. A novel grain tracking procedure was developed to track individual grains within the foam volume by accounting for the large rigid-body motions that individual ligaments can undergo during mechanical loading. The ability to track grains and precipitate structures in three dimensions throughout large bulk deformation of ultra-low-density polycrystalline materials enables new possibilities for validating numerical models and investigating local failure mechanisms. Furthermore, the methods and procedures developed in this study could be applied to other ultra-low-density structures, such as additively manufactured lattices.

Polymorphism of garnet solid electrolytes and its implications for grain-level chemo-mechanics.

Understanding and mitigating filament formation, short-circuit and solid electrolyte fracture is necessary for advanced all-solid-state batteries. Here, we employ a coupled far-field high-energy diffraction microscopy and tomography approach for assessing the chemo-mechanical behaviour for dense, polycrystalline garnet (Li7La3Zr2O12) solid electrolytes with grain-level resolution. In situ monitoring of grain-level stress responses reveals that the failure mechanism is stochastic and affected by local microstructural heterogeneity. Coupling high-energy X-ray diffraction and far-field high-energy diffraction microscopy measurements reveals the presence of phase heterogeneity that can alter local chemo-mechanics within the bulk solid electrolyte. These local regions are proposed to be regions with the presence of a cubic polymorph of LLZO, potentially arising from local dopant concentration variation. The coupled tomography and FF-HEDM experiments are combined with transport and mechanics modelling to illustrate the degradation of polycrystalline garnet solid electrolytes. The results showcase the pathways for processing high-performing solid-state batteries.

3D In-situ Stop Action Study of Recrystallization in Additively Manufactured 316L Stainless Steel: Reconstruction Optimization and Observations

A volume of an additively manufactured 316L stainless steel sample has been tracked during its recrystallization using near- and far-field High Energy Diffraction Microscopy (HEDM) and absorption tomography at Advanced Photon Source beamline 1-ID. A near-field compatible in situ furnace allows monitoring of Bragg diffraction signals as they evolve out of a weak and diffuse background while the sample temperature is ≈ 1250° C. The sample is rapidly cooled to room temperature after observation of significant signal evolution and ∼ 0.035 mm3 is mapped by the near-field method. Four cycles of heat treatment follow the structure from a state of small, isolated grains through impingement of domains to near completion of recyrstallization. Here, the experiment and reconstructions are described, and recrystallized fractions, twin domains, and distributions of grain boundary types are discussed.

The dynamics of recrystallized grains during static recrystallization in a hot-compressed Mg-3.2Zn-0.1Ca wt.% alloy using in-situ far field high-energy diffraction microscopy

The poor formability of rolled magnesium (Mg) alloy sheet remains a barrier to its widespread commercial use and is attributed to the strong basal texture that occurs in most mechanically processed Mg alloys. Recent attempts to successfully weaken the texture have been made using Mg-Zn-Ca alloys in combination with post-deformation annealing. The motivation for this work is to understand the evolution of the mesoscale processes that occur during annealing (specifically, static recrystallization) and lead to this texture weakening. Toward this goal, more than 1,200 recrystallized grains were studied during in-situ annealing in an 80% hot-compressed Mg-3.2Zn-0.1Ca wt.% (ZX30) alloy using far-field high-energy diffraction (ff-HEDM). The relative volume, crystallographic orientation, and position of each recrystallized grain emerging within a 1 × 1 × 0.1 mm3vol were tracked throughout static recrystallization. These measurements were used to quantitatively measure the nucleation and growth statistics associated with recrystallized grains as a function of annealing time. The measurements reflected a highly heterogeneous process with individual grain dynamics varying wildly from the average, and they also point to relations between relative grain volume and growth rate (or more accurately, the rate of change of volume) with a peak average rate occurring early in recrystallization (at 22% recrystallized). We also explore whether a recrystallized grain's current state can be used to predict its future growth behaviors with implications for Monte Carlo simulations. Finally, we investigate whether recrystallized grains with specific orientations have preferential nucleation and/or growth, and we find that grains with a weak basal texture have a pronounced nucleation advantage that increases with annealing time, while other grain orientations have a slight growth advantage that diminishes with annealing time.

Repeatability and sensitivity characterization of the far-field high-energy diffraction microscopy instrument at the Advanced Photon Source.

In the last two decades, far-field high-energy diffraction microscopy (FF-HEDM) and similar non-destructive techniques have been actively developed at synchrotron light sources around the world. As these techniques (and associated analysis tools) are becoming more available for the general users of these light sources, it is important and timely to characterize their performance and capabilities. In this work, the FF-HEDM instrument implemented at the 1-ID-E endstation of the Advanced Photon Source (APS) is summarized. The set of measurements conducted to characterize the instrument's repeatability and sensitivity to changes in grain orientation and position are also described. When an appropriate grain matching method is used, the FF-HEDM instrument's repeatability is approximately 5 µm in translation, 0.02° in rotation, and 2 × 10-4 in strain; the instrument sensitivity is approximately 5 µm in translation and 0.05° in rotation.

Discrepancy Between Crystal Plasticity Simulations and Far-Field High-Energy X-ray Diffraction Microscopy Measurements

Discrepancy Between Crystal Plasticity Simulations and Far-Field High-Energy X-ray Diffraction Microscopy Measurements

Void coalescence and ductile failure in IN718 investigated via high-energy synchrotron X-ray tomography and diffraction

Ductile failure through the growth and coalescence of voids is of particular relevance for many engineering materials. Yet, the lack of experimental measurements of the mechanical state of the material at an appropriate length scale has limited further understanding of the regime of ductile failure. In this study, local grain-scale experimental measurements are used to determine their relevance for describing and predicting ductile failure. Additive manufactured materials, due to the presence of inherent porosity, as well as the ability to tailor internal porosity, provides a promising avenue to study ductile failure. Selective laser melting is used to manufacture a specially designed specimen with two large, internal voids, in addition to the natural porosity, which is characteristic to the production process. The initial porosity and its evolution upon tensile loading are characterized via micro-tomography. Several locations of void coalescence are captured in the sample, revealing activity of multiple modes of failure. Finite element simulations, with a simplified J2 plasticity model, instantiated with the initial void structure, is deployed, in which geometric localizations of stress concentration corresponded with experimentally observed sites of coalescence but was inadequate in capturing the appropriate failure mechanism. From the experimental results of the far-field high-energy diffraction microscopy, the heterogeneous micromechanical state is identified and tracked around voids due to the local grain interactions. These experiments determine narrow bands of low stress triaxiality, at the onset of failure, which highlight the path of coalescence through intervoid shearing. Diffraction spot spreading analysis aided characterization of intragranular plasticity and strain heterogeneity, which can be coupled with high triaxiality to form the conditions inducive for coalescence through intervoid necking. In this study, the experimentally determined grain-scale description of the micromechanical state provides a physical basis that can accurately capture both the sites and the mechanism of void coalescence at the onset of ductile failure.

High-Energy Coherent X-Ray Diffraction Microscopy of Polycrystal Grains: Steps Toward a Multiscale Approach

We present proof-of-concept imaging measurements of a polycrystalline material that integrate the elements of conventional high-energy X-ray diffraction microscopy with coherent diffraction imaging techniques, and that can enable in-situ strain-sensitive imaging of lattice structure in ensembles of deeply embedded crystals over five decades of length scale upon full realization. Such multi-scale imaging capabilities are critical to addressing important questions in a variety of research areas such as materials science and engineering, chemistry, and solid state physics. Towards this eventual goal, the following key aspects are demonstrated: 1) high-energy Bragg coherent diffraction imaging (HE-BCDI) of sub-micron-scale crystallites at 52 keV at current third-generation synchrotron light sources, 2) HE-BCDI performed in conjunction with far-field high-energy diffraction microscopy (ff-HEDM) on the grains of a polycrystalline sample in an smoothly integrated manner, and 3) the orientation information of an ensemble of grains obtained via ff-HEDM used to perform complementary HE-BCDI on multiple Bragg reflections of a single targeted grain. These steps lay the foundation for integration of HE-BCDI, which typically provides a spatial resolution tens of nanometers, into a broad suite of well-established HEDM methods, extending HEDM beyond the few-micrometer resolution bound and into the nanoscale, and positioning the approach to take full advantage of the orders-of-magnitude improvement of X-ray coherence expected at fourth generation light sources presently being built and commissioned worldwide.

Micromechanical Response of Crystalline Phases in Alternate Cementitious Materials using 3-Dimensional X-ray Techniques

Cementitious materials are complex composites that exhibit significant spatial heterogeneity in their chemical composition and micromechanical response. Modern 3-dimensional characterization techniques using X-rays from synchrotron light sources, such as micro-computed tomography (μCT) and far-field high-energy diffraction microscopy (ff-HEDM), are now capable of probing this micromechanical heterogeneity. In this work, the above mentioned techniques are used to understand the varying micromechanical response of crystalline phases (cubic iron oxide and α-quartz) inherently present within an alkali-activated fly ash (AAF) during in-situ confined compression. A subset of the crystals probed using ff-HEDM are registered with the tomographic reconstructions and tracked through the applied loads, highlighting the combination of μCT and ff-HEDM as a means to examine both elastic strain in the crystalline particles (and by extension local stress response) and plastic strain in the matrix. In this study, significant differences in the load carrying behaviors of the crystalline phases were observed wherein the cubic iron oxide crystals laterally expanded during the confined compression test, while the α-quartz particles laterally contracted and at the final load step, shed load likely due to failure in the surrounding matrix. Finally, the two characterization techniques are discussed in terms of both advantages and associated challenges for analysis of multi-phase cementitious materials.

ICME Approach to Determining Critical Pore Size of IN718 Produced by Selective Laser Melting

A degree of porosity is expected in additively manufactured (AM) materials. To aid in the qualification of AM materials, the smallest pore size that results in a debit in the fatigue performance is quantified. In the work presented herein, crystal plasticity simulations are used to identify the stress concentration around pores of various sizes, revealing that a single 20-μm pore or two 10-μm pores (with centers spaced 15 μm apart) localize stress at the pore, as opposed to elsewhere in the microstructure. In situ microtomography and far-field high-energy x-ray diffraction microscopy were used to identify crack formation and the evolution of the grain-level micromechanical fields during cyclic loading. Eighteen cracks were observed (15 at pores, 3 at the surface) at highly stressed grains in a sample, although most did not propagate. The dominant crack was seen to originate from the free surface, which is rationalized by fracture mechanics.

A Planar Biaxial Experiment Platform for In Situ High-Energy Diffraction Studies

An experimental platform for multiscale studies of materials subjected to plane stress loads is presented. Coupling with far-field high-energy diffraction microscopy for grain-by-grain measurements of elastic strains and rotations provides an additional benefit; it enables the direct assessment of elastic vs. inelastic deformation of the gauge sections of cruciform specimens subjected to plane stress loadings, without any a priori assumptions of the form of constitutive relationships, resolving a long-outstanding challenge of multiaxial mechanical testing. Specifically, a planar biaxial mechanical load frame with four independent hydraulic actuators capable of applying arbitrary loading paths and ratios of tension and compression was designed and built for in situ diffraction experimentation. The load frame is integrated for use at the Argonne National Laboratory Advanced Photon Source (APS) synchrotron, Sector 1, 1-ID-E endstation and the Los Alamos Neutron Science Center (LANSCE) spallation neutron source, Spectrometer for Materials Research at Temperature and Stress (SMARTS) instrument. Cruciform specimen geometries were designed to experience loading ratios in the gauges commensurate with those applied at the grips, and to minimize interference with diffracted X-rays and neutrons. The finite element models used to design the cruciform specimen geometries were experimentally validated using stereo digital image correlation measurements. This complete planar biaxial in situ diffraction platform provides a new capability for studying multiaxial micromechanics of crystalline materials (e.g., elastic, slip, twinning, phase transformation) and their dependencies on grain size, location, texture, and neighborhood characteristics.

In-situ study of planar slip in a commercial aluminum-lithium alloy using high energy X-ray diffraction microscopy

Aluminum-lithium alloys offer high specific-strength and -stiffness which makes them attractive for aerospace applications. However, several material related challenges have limited the use of these alloys including a tendency for grain boundary cracking due to localized damage known as delamination. Prior studies of these alloys have found evidence of a relationship between delamination and the occurrence of intense planar slip due to the shearing of the δ' (Al3Li) precipitate phase. In this study, far-field high-energy X-ray diffraction microscopy is used to quantify the effects of slip activity and subsequent stress response of the Al-Cu-Li alloy (AA2099) in both individual grains and various grain populations. Results show that grains with high Schmid factors, interpreted as an indicator of propensity for single slip at the elastic-plastic transition, are most likely to undergo grain softening consistent with precipitate-shear-driven planar slip. Conversely, grains with low Schmid factors are less prone to this deformation mode. A corresponding rise in triaxiality is found in grains which soften. The implications of pairings of grains exhibiting dissimilar micromechanical behaviors for delamination are discussed.

Three-dimensional in situ characterization of phase transformation induced austenite grain refinement in nickel-titanium

Near-field and far-field high-energy diffraction microscopy and microcomputed tomography X-ray techniques were used to study a bulk single crystal nickel‑titanium shape memory alloy sample subjected to thermal cycling under a constant applied load. Three-dimensional in situ reconstructions of the austenite microstructure are presented, including the structure and distribution of emergent grain boundaries. After 1 cycle, the subgrain structure is significantly refined, and heterogeneous Σ3 and Σ9 grain boundaries emerge. The low volume and uneven dispersion of the emergent Σ boundaries across the volume show why previous transmission electron microscopy investigations of Σ grain boundary formation were inconsistent.

Intermittent plasticity in individual grains: A study using high energy x-ray diffraction.

Long-standing evidence suggests that plasticity in metals may proceed in an intermittent fashion. While the documentation of intermittency in plastically deforming materials has been achieved in several experimental settings, efforts to draw connections from dislocation motion and structure development to stress relaxation have been limited, especially in the bulk of deforming polycrystals. This work uses high energy x-ray diffraction measurements to build these links by characterizing plastic deformation events inside individual deforming grains in both the titanium alloy, Ti-7Al, and the magnesium alloy, AZ31. This analysis is performed by combining macroscopic stress relaxation data, complete grain stress states found using far-field high energy diffraction microscopy, and rapid x-ray diffraction spot measurements made using a Mixed-Mode Pixel Array Detector. Changes in the dislocation content within the deforming grains are monitored using the evolution of the full 3-D shapes of the diffraction spot intensity distributions in reciprocal space. The results for the Ti-7Al alloy show the presence of large stress fluctuations in contrast to AZ31, which shows a lesser degree of intermittent plastic flow.

Measuring stress-induced martensite microstructures using far-field high-energy diffraction microscopy.

Modern X-ray diffraction techniques are now allowing researchers to collect long-desired experimental verification data sets that are in situ, three-dimensional, on the same length scales as critical microstructures, and using bulk samples. These techniques need to be adapted for advanced material systems that undergo combinations of phase transformation, twinning and plasticity. One particular challenge addressed in this article is direct analysis of martensite phases in far-field high-energy diffraction microscopy experiments. Specifically, an algorithmic forward model approach is presented to analyze phase transformation and twinning data sets of shape memory alloys. In the present implementation of the algorithm, the crystallographic theory of martensite (CTM) is used to predict possible martensite microstructures (i.e. martensite orientations, twin mode, habit plane, twin plane and twin phase fractions) that could form from the parent austenite structure. This approach is successfully demonstrated on three single- and near-single-crystal NiTi samples where the fundamental assumptions of the CTM are not upheld. That is, the samples have elastically strained lattices, inclusions, precipitates, subgrains, R-phase transformation and/or are not an infinite plate. The results indicate that the CTM still provides structural solutions that match the experiments. However, the widely accepted maximum work criterion for predicting which solution of the CTM should be preferred by the material does not work in these cases. Hence, a more accurate model that can simulate these additional structural complexities can be used within the algorithm in the future to improve its performance for non-ideal materials.

High-energy x-ray diffraction microscopy study of deformation microstructures in neutron-irradiated polycrystalline Fe-9%Cr

In this study, we used far-field high-energy x-ray diffraction microscopy (FF-HEDM) to measure in 3D the spatial distributions of the sizes, orientations, and residual strains of grains and subgrains formed by room-temperature tensile deformation in a neutron-irradiated (450 °C, 0.01dpa) Fe-9Cr specimen and its unirradiated counterpart. We found that neutron irradiation under this condition alone had no effect on the grain size distribution. After deformation, grains fragmented into subgrains in both unirradiated and irradiated specimens: the irradiated specimen contained a few large subgrains which co-existed with many smaller subgrains, while the unirradiated specimen contained small subgrains with a relatively uniform size distribution. Prior to deformation, the irradiated specimen had higher residual strain spread compared to its unirradiated counterpart, while after deformation to the maximum uniform elongation, the strain distributions among subgrains were similar between the unirradiated and irradiated specimens. The FF-HEDM measurements provide new insight into the effects of neutron irradiation on the mechanical response of Fe-Cr ferritic alloys.

Analyzing shear band formation with high resolution X-ray diffraction

Localization of crystallographic slip into shear bands during uniaxial compression of a copper single crystal is studied using very far-field high-energy diffraction microscopy (vff-HEDM). Diffracted intensity was collected in-situ as the crystal deformed using a unique mobile detector stage that provided access to multiple diffraction peaks with high-angular resolution. From the diffraction data, single crystal orientation pole figures (SCPFs) were generated and are used to track the evolution of the distribution of lattice orientation that develops as slip localizes. To aid the identification of ‘signatures’ of shear band formation and analyze the SCPF data, a model of slip-driven lattice reorientation within shear bands is introduced. Confidence is built in conclusions drawn from the SCPF data about the character of internal slip localization through comparisons with strain fields on the sample surface measured simultaneously using digital image correlation. From the diffraction data, we find that the active slip direction and slip plane are not directly aligned with the orientation of the shear bands that formed. In fact, by extracting the underlying slip system activity from the SCPF data, we show that intersecting shear bands measured on the surface of the sample arise from slip primarily on the same underlying single slip system. These new vff-HEDM results raise significant questions on the use of surface measurements for slip system activity estimation.

In situ, 3D characterization of the deformation mechanics of a superelastic NiTi shape memory alloy single crystal under multiscale constraint

Microstructural elements in NiTi shape memory alloys (SMAs) – precipitates, phase boundaries, inclusions, grain boundaries – can be viewed as sources of multiscale constraint that influence their deformation response. We characterized in situ, and in 3D, the deformation and the evolution of microstructure during a tension test in a superelastic NiTi specimen containing some of these sources of constraint. The method used was far-field high-energy X-ray diffraction microscopy (ff-HEDM), complemented by electron microscopy. We simulated the local stress state in the specimen using a microstructural model informed by the experimental data. Using these combined microstructure, deformation, and stress data, we report three phenomena, and relate them to specific sources of constraint. During initial elastic loading, axial lattice strain in austenite increased monotonically. On partial stress-induced phase transformation to martensite, the stress redistributed to both phases leading to a stress relaxation in austenite. The specimen contained a dense distribution of inclusions, which led to the activation of martensite habit plane variants that produce less than theoretical maximum transformation strain. Large Ni4Ti3 precipitates potentially contributed to the poor transformation response. Under load, proportional gradients in local rotation and elastic stretch developed in the martensite phase, because of the constraint at phase interfaces. This combined ff-HEDM, electron microscopy, microstructural simulation toolbox provides a versatile method to understand the effect of constraint on inelastic deformation in other alloys with hierarchical microstructure.