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The microstructure of additively manufactured Ti-6Al-4V (Ti64) produced by a laser powder bed fusion process was studied during post-build heat treatments between 1043 K (770 °C) and just above the β transus temperature 1241 K (1008 °C) in situ using high-energy X-ray diffraction. Parallel studies on traditionally manufactured wrought and annealed Ti64 were completed as a baseline comparison. The initial and final grain structures were characterized using electron backscatter diffraction. Likewise, the initial texture, dislocation density, and final texture were determined with X-ray diffraction. The evolution of the microstructure, including the phase evolution, internal stress, qualitative dislocation density, and vanadium distribution between the constituent phases were monitored with in situ X-ray diffraction. The as-built powder bed fusion material was single-phase hexagonal close packed (to the measurement resolution) with a fine acicular grain structure and exhibited a high dislocation density and intergranular residual stress. Recovery of the high dislocation density and annealing of the internal stress were observed to initiate concurrently at a relatively low temperature of 770 K (497 °C). Transformation to the β phase initiated at roughly 913 K (640 °C), after recovery had occurred. These results are meant to be used to design post-build heat treatments resulting in specified microstructures and properties.

The evolution of the crystallographic texture and lattice strain of uranium 6-weight percent niobium alloy samples are tracked during multiple deformation and heat treating cycles in an effort to understand and control the mechanical properties of the material following thermo-mechanical processing. The heavily twinned microstructure and low-symmetry crystal structure of U-6Nb result in multiple sequential active deformation mechanisms associated with distinctive deformation textures in strain ranges from 0-0.15 true strain. It is found that heating into the high-temperature γ-phase erases much of the texture formed during deformation at room temperature in the α′′-phase and resets the active deformation mechanisms. Through a small number of deformation/heat treat cycles to moderate strains, i.e., ~ 0.13 per cycle, the flow strength of the material is recovered to its original value. However, on the fourth such cycle, a reduction of strength is observed and the sample failed.

Steels are ubiquitous due to their affordability and the landscape of useful properties that can be generated for engineering applications. But to further expand the performance envelope, one must be able to understand and control microstructure development by alloying and processing. Here we use multiscale, advanced characterization to better understand the structural and chemical evolution of AISI 4340 steel after quenching and tempering (Q&T), including the role of quench rate and short-time, isothermal tempering below 573 K (300 °C), with an emphasis on carbide formation. We compare the microstructure and/or property changes produced by conventional tempering to those produced by higher temperature, short-time “rapid” tempering. We underscore that no single characterization technique can fully capture the subtle microstructure changes like carbon redistribution, transition carbide and/or cementite formation, and retained austenite decomposition that occur during Q&T. Only the use of multiple techniques begins to unravel these complexities. After controlled fast or slow quenching, η transition carbides clearly exist in the microstructure, likely associated with autotempering of this high martensite start temperature (Ms) steel. Isothermal tempering below 598 K (325 °C) results in the relief of carbon supersaturation in the martensite, primarily by the formation of η transition carbides that exhibit a range of carbon levels, seemingly without substitutional element partitioning between the carbide and matrix phases. Hagg transition carbide is present between 300 °C and 325 °C. After conventional tempering at or above 598 K (325 °C) for 2 h, cementite is predominant, but small amounts of cementite are also present in other conditions, even after quenching. Previous work has indicated that silicon (Si) and substitutional elements partition between the cementite, which initially forms under paraequilibrium conditions, and the matrix. Phosphorous (P) may also be preferentially located at cementite/matrix interfaces after high temperature tempering. Slower quench rates result in greater amounts of retained austenite compared to those after fast quenching, which we attribute to increased austenite stability resulting from “autopartitioning”. Rapid, high temperature tempering is also found to diminish tempered martensite embrittlement (TME) believed to be associated with the extent of austenite decomposition, resulting in mechanical properties not attainable by conventional tempering, which may have important implications with respect to industrial heat treatment processes like induction tempering. Controlling the amount and stability of retained austenite is not only relevant to the properties of Q&T steels, but also next-generation advanced high strength steels (AHSS) with austenite/martensite mixtures.

Uranium-6 wt pct niobium (14 at pct niobium) displays the shape memory effect (SME), where deformation proceeds by twinning and twin rearrangement via boundary migration within the SME regime. In-situ neutron diffraction during deformation suggests that after SME strain is exhausted, deformation proceeds via another twinning mechanism that does not recover to the original parent orientation upon reheating and transformation. Here we show from in-situ tensile and compressive loading and unloading experiments that early post-SME twins partially reverse during unloading, which is evident by rapid texture evolution, and this reversion is responsible for the inelastic portion of the previously reported ~ 2 pct strain recovery.

Adoption of metal additive manufacturing (AM) components in property-critical applications requires predictable performance of fabricated metal AM parts. In-situ diagnostics coupled with material models provide a pathway for qualification of AM whereby a prime objective is to capture data that inform or validate models or theory. Part of this is to understand the solidification and cooling of the material through diagnostics in order to ensure the part is being built correctly and that microstructures and properties are predictable. We have utilized high-energy X-ray diffraction to provide a unique probe for bulk material characterization in-situ during additive manufacture. The current work is focused on presenting the opportunities and potential pitfalls associated with extracting microstructural information from diffraction data that is necessarily limited due to the dynamic nature of the process. We present diffraction measurements and Rietveld refinement of stainless steel wire-arc line depositions using 71 keV X-rays, providing information on temperature, phase evolution, and residual stress during the deposition of a single-layer of 308L stainless filler wire on a 304L stainless steel substrate. In addition to observing both the liquid/solid and solid-state phase transformations, this methodology can be used to map the extent of the melt pool, identify thermal gradients, and measure residual stresses in materials during deposition.

Combined in-situ neutron diffraction measurements during post-processing heat treatment and thermo-mechanical crystal plasticity finite element (CPFE) simulations were utilized to study the residual phase stress development in the two-phase microstructure of an additively manufactured (AM) 304L stainless steel. The steel, fabricated via the laser engineering net shaping technique, has a microstructure comprising primarily of the austenite phase, with ∼ 2.5% ferrite phase by volume fraction. The post-build material was heated to greater than 1300 K and neutron diffraction data was recorded during heating and cooling. Specifically, the evolution of lattice strains in the individual phases were measured with temperature and the corresponding coefficients of thermal expansion (CTEs) calculated. The dislocation densities, phase fractions and textures, before and after heat treatment, were also measured. CPFE simulations were performed to study the interplay of the stress-free thermal strains and the mechanical strains in inducing inter-granular residual stresses in individual phases. The simulations confirmed the presence of process induced inter-granular residual stress primarily in the ferrite phase of the as-built AM material. Comparison of the relevant simulation data with experiments indicate that model predictions of the lattice strains and CTEs in both phases, as well as the inter-granular residual phase stress and pressure in the ferrite phase are in qualitative agreement with the experimental measurements and calculations.

Three 316L stainless steel materials are studied and reported upon; wrought, as-built additively manufactured (AM), and heat-treated AM material. The AM material was produced from the laser engineered net shaping (LENS) process. Macroscopic uniaxial compression stress-strain curves were obtained for all three materials. The curves were similar for the wrought and heat-treated AM materials but the as-built AM material demonstrated approximately 1.7 times greater flow stress at any given level of strain than the other two materials. Electron-backscatter diffraction analysis of the materials also showed that the microstructures of the three materials differed; with complex grain morphology for the as-built AM material. The mean grain size of each of the three materials also differed. The initial dislocation density was also measured with neutron diffraction and line-profile analysis for both wrought and as-built AM materials with the density in the AM material approximately 2.5 times greater. A single crystal model was proposed to represent the essential features of the three FCC materials accounting for dislocation interactions and representation of grain size via a simple Hall-Petch type term. The strength of this term is evaluated through independent experimental results on traditionally manufactured materials. The model was applied to each of the three materials by simulation of the uniaxial compression experiments by direct numerical simulation of electron-backscatter diffraction images. This allowed for representation of the size of each grain in the simulations. The results suggest that the difference in initial dislocation density of the three materials is the primary factor causing the difference in stress-strain response. Although the differences in grain size contribute to a higher stress for the as-built AM material, the effect is small. Other factors such as internal stress and grain morphology could play a role in mechanical behavior difference and these two factors are also discussed.

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.

Additive manufacturing of metal components results in unique microstructures with, necessarily, mechanical properties that are distinct from conventionally produced components. In this work, four distinct microstructural features associated with directed energy deposition of 304L stainless steels, their stability, and their influences on flow strength were examined. These were (1) high dislocation density comparable with deformed materials, (2) increased ferrite content, (3) local chemical heterogeneity, and (4) tortuous grain morphology. In situ neutron diffraction measurements were used to monitor the evolution of the as-built microstructure during post-build heat treatment and relate the specific microstructural features to the strength behavior of the material following the heat treatment. The increased flow strength of the additively manufactured material relative to wrought counterparts is found to be due primarily to an increased dislocation density in the as-built material. However, the increased dislocation density does not completely account for the increased strength and it is hypothesized that some of the additional strength is related to the unique AM grain structure.

In situ time-resolved synchrotron X-ray diffraction experiments were conducted to study the fine-scale phase evolution of U-6Nb. Upon rapid heating from 125 °C to 400 °C, a reverse martensitic transformation sequence, α″ → γo → γs, was observed in less than 4 seconds, which represents the first direct observation of the γo → γs transformation in diffraction-based measurements. Consistent with previous ex situ metallography experiments, our isothermal hold experiments at 526 °C, 530 °C and 565 °C reveal two distinct reactions for the phase separation, γs → α-U + γ1 (general precipitation) followed by (α-U + γ1) → α-U + γ1-2 (discontinuous precipitation). For the first-stage precipitation, the incubation time is determined to be ~ 50 and 100 seconds, respectively, for the isothermal aging at 526-530 °C and 565 °C. At this stage, the phase transformation is characterized by the simultaneous growth of α-U and γ1 at the expense of γs. As expected from the Arrhenius equation for the reaction rate, the determined times (~ 23 minutes) for the completion of the first-stage reaction at 526 ± 3 °C and 530 ± 3 °C are nearly twice longer than that at 565 ± 4 °C (~ 13 minutes). Over these periods of time, the Nb contents derived from a Vegard’s-type relationship for γ1 are in the 30.2 to 32.1 and 29.2 to 30.6 at. pct ranges, and the kinetics of the precipitation at 565 ± 4 °C can be described by the classic Avrami rate equation and one-dimensional growth of a surface or grain-boundary nucleation. During the second-stage precipitation, the γ1 phase continues to enrich in Nb as it gradually evolves toward the α + γ1-2 metastable state (up to 47 at. pct over a period of 172 minutes at 530 °C). These new and time-resolved measurements can be used to better constrain the time–temperature–transformation diagram, solute (Nb) redistribution, and transformation kinetics during the early stages of the diffusional phase transformation.

In situ high-energy X-ray diffraction measurements were completed during deposition of 308L stainless steel wire onto a 304L stainless steel substrate. Attempts were made to extract microstructural features such as phase fraction and internal stress, as well as temperature evolution immediately following the deposition. The limited data that could be collected during deposition and rapid solidification are critically examined. High-energy X-rays coupled with relatively slow detectors were utilized to enable determination of orientation-dependent lattice parameters accurately enough to comment on phase strain evolution between austenite and ferrite. Information about the hydrostatic and deviatoric stress states of the constituent phases was determined on time scales that are relevant to their development. However, the time resolution of the technique was insufficient to monitor phase evolution during the solid–solid phase transformation and, more so, during solidification. Moreover, the accurate and absolute determination of inherently statistical parameters, such as phase fraction, depends critically on the ability to sample a statistically significant numbers of grains in the microstructure.

The production of metallic parts via laser-powder bed fusion (L-PBF) additive manufacturing is rapidly growing. To use components produced via L-PBF in safety-critical applications, a high degree of confidence is required in their quality. This qualification can be supported by means of a validated thermomechanical model capable of predicting the final residual stress state and subsequent performance. In this work, we use high-energy X-ray diffraction to determine a three-dimensional residual strain and stress state in a Ti-6Al-4V L-PBF component. The experimental results are used to provide validation of simulations, showing strong quantitative agreement.

A series of measurements were designed to gain confidence in the interpretation of the peak breadth in diffraction patterns collected from additively manufactured material, which has a novel microstructure in comparison to the well understood microstructure of wrought materials. Stainless steels made with two additive manufacturing techniques were compared to wrought material. Similar patterns observed in the scattering vector dependence for additively manufactured and deformed wrought materials suggested that the broadening in both materials was related to dislocations. This was confirmed by heat-treatment, during which both materials exhibited recovery due to the annealing of dislocations at the same temperature.

We present a comprehensive study of the effects of internal boundaries on the accuracy of residual stress values obtained from the eigenstrain method. In the experimental part of this effort, a composite specimen, consisting of an aluminum cylinder sandwiched between steel cylinders of the same diameter, was uniformly heated under axial displacement constraint. During the experiment, the sample temperature and the reaction stresses in the load frame in response to changes in sample temperature were monitored. In addition, the local (elastic) lattice strain distribution within the specimen was measured using neutron diffraction. The eigenstrain method, utilizing finite element modeling, was then used to predict the stress field existing within the sample in response to the constraint imposed by the load frame against axial thermal expansion. Our comparison of the computed and measured stress distributions showed that, while the eigenstrain method predicted acceptable stress values away from the cylinder interfaces, its predictions did not match experimentally measured values near them. These observations indicate that the eigenstrain method is not valid for sample geometries with this type of internal boundaries.

In situ neutron diffraction measurements were completed during tensile and compressive deformation of stainless steel 304L additively manufactured (AM) using a high power directed energy deposition process. Traditionally produced wrought 304L material was also studied for comparison. The AM material exhibited roughly 200 MPa higher flow stress relative to the wrought material. Crystallite size, crystallographic texture, dislocation density, and lattice strains were all characterized to understand the differences in the macroscopic mechanical behavior. The AM material’s initial dislocation density was about 10 times that of the wrought material, and the flow strength of both materials obeyed the Taylor equation, indicating that the AM material’s increased yield strength was primarily due to greater dislocation density. Also, a ~50 MPa flow strength tension/compression asymmetry was observed in the AM material, and several potential causes were examined.

In-situ neutron diffraction measurements were performed during heat-treating and uniaxial loading of additively manufactured (AM) GP1 material. Although the measured chemical composition of the GP1 powder falls within the composition specifications of 17-4 PH steel, a fully martensitic alloy in the wrought condition, the crystal structure of the as-built GP1 material is fully austenitic. Chemical analysis of the as-built material shows high oxygen and nitrogen content, which then significantly decreased after heat-treating in a vacuum furnace at 650 °C for one hour. Significant austenite-to-martensite phase transformation is observed during compressive and tensile loading of the as-built and heat-treated material with accompanied strengthening as martensite volume fraction increases. During loading, the initial average phase stress state in the martensite is hydrostatic compression independent of the loading direction. Preferred orientation transformation in austenite and applied load accommodation by variant selection in martensite are observed via measurements of the texture development.

Uranium-niobium alloys can exist with significantly different microstructures and mechanical properties, heavily influenced by thermomechanical processing history and impurities. Here, the influence of Ti and other impurities is studied on uranium-14 at.% niobium additively manufactured using laser powder bed fusion. Two different metallic impurity levels were investigated and a Nb equivalent (Nbeq) composition is defined to represent the impurities. In-situ neutron diffraction during compression loading shows that increased Nbeq promotes the formation of γ°-tetragonal phase at the expense of α″-monoclinic phase, resulting in 2 × higher yield strength than water quenched α″ and a strain induced transformation to α″ with superelastic strains to 4.5%.

Charpy test specimens were additively manufactured (AM) on a single stainless steel plate from a 17–4 class stainless steel using a powder-bed, laser melting technique on an EOS M280 direct metal laser sintering (DMLS) machine. Cross-hatched mesh support structures for the Charpy test specimens were varied in strut width and density to parametrically study their influence on the build stability and accuracy as the DMLS process has been known to generate parts with large amounts of residual stress. Neutron diffraction was used to profile the residual stresses in several of the AM samples before and after the samples were removed from the support structure for the purpose of determining residual stresses. The residual stresses were found to depend very little on the properties of the support structure over the limited range studied here. The largest stress component was in the long direction of each of the samples studied and was roughly 2/3 of the yield stress of the material. The stress field was altered considerably when the specimen was removed from the support structure. It was noted in this study that a single Charpy specimen developed a significant tear between the growth plate and support structure. The presence of the tear in the support structure strongly affected the observed stress field: the asymmetric tear resulted in a significantly asymmetric stress field that propagated through removal of the sample from the base plate. The altered final residual stress state of the sample as well as its observed final shape indicates that the tear initiated during the build and developed without disrupting the fabrication process, suggesting a need for in-situ monitoring.

A recently modified Elasto-Plastic Self-Consistent (EPSC) model which empirically accounts for both intergranular and intragranular back stresses has been successfully used to simulate the cyclic (tension-compression) loading behaviour of an Fe-24Mn-3Al-2Si-1Ni-0.06C TWinning Induced Plasticity (TWIP) steel between strain limits of ±1%. Lattice strain measurements acquired via in-situ neutron diffraction were used to further validate the modelling results. An improved prediction of the pronounced Bauschinger effect during unloading is achieved when the reversibility of partial slip in the 〈 112 〉 direction is accounted for. This result indicates a potential contribution of the stress-induced separation of partial dislocations to the observed early yielding at the low strain levels employed in this study. It also raises the possibility that de-twinning events could be operative during load reversal.

An elasto-plastic self-consistent (EPSC) polycrystal plasticity formulation is adapted to model deformation of wrought α-uranium (α-U) accommodated by a combination of elasticity, dislocation glide, and deformation twinning. The EPSC model incorporates a strain-path, strain rate, and temperature sensitive dislocation density-based hardening law for the evolution of resistance to slip, twinning, and de-twinning and a slip system-level kinematic back-stress law to influence the driving force for activation. The model is used to interpret the complex deformation behavior of α-U as a function of strain-path and temperature. Samples of α-U with different initial orientation distributions are experimentally evaluated in simple compression, tension, and load reversal at room temperature and in compression and rolling at 573 K under a quasi-static deformation rate. Evolution of texture and twinning is characterized using electron backscattered diffraction and in-situ and ex-situ neutron diffraction during deformation. It is observed that the behavior of the material is highly anisotropic owing to its low-symmetry orthorhombic crystal structure and different activation stresses for crystallographic deformation modes. The model is calibrated and validated under these deformation conditions and predicts the stress-strain responses, amount of twinning, texture evolution, and lattice strains with one set of parameters for the hardening and back-stress evolution laws. Subsequently, the developed model is used as a constitutive law in the implicit finite element (FE) framework to simulate drawing of a hemispherical part from a rolled sheet of α-U. Here, the FE-EPSC model is a two-level homogenization scheme with EPSC relating the grain-level to the polycrystalline aggregate-level response, while the FE framework scales the polycrystalline to the part-level response. The simulation results and insights from the calculations, such as location dependent texture evolution is in good agreement with experiments.

Additive manufacturing (AM) technology provides unique opportunities for producing net-shape geometries at the macroscale through microscale processing. This level of control presents inherent trade-offs necessitating the establishment of quality controls aimed at minimizing undesirable properties, such as porosity and residual stresses. Here, we perform a parametric study into the effects of laser scanning pattern, power, speed, and build direction in powder bed fusion AM on residual stress. In an effort to better understand the factors influencing macroscale residual stresses, a destructive surface residual stress measurement technique (digital image correlation in conjunction with build plate removal and sectioning) has been coupled with a nondestructive volumetric evaluation method (i.e., neutron diffraction). Good agreement between the two measurement techniques is observed. Furthermore, a reduction in residual stress is obtained by decreasing scan island size, increasing island to wall rotation to 45 deg, and increasing applied energy per unit length (laser power/speed). Neutron diffraction measurements reveal that, while in-plane residual stresses are affected by scan island rotation, axial residual stresses are unchanged. We attribute this in-plane behavior to misalignment between the greatest thermal stresses (scan direction) and largest part dimension.

A 7.1-Mn 0.1-C transformation-induced plasticity steel was intercritically annealed at 600 °C and 650 °C for 168 h. Ultra-fine-grained microstructures with annealing temperature dependent retained austenite fractions and tensile properties were produced. in situ neutron diffraction was used to investigate the change in tensile properties via measurement of phase fractions, elastic phase strains, and diffraction peak broadening during deformation. Austenite transformation to martensite controlled initial yielding in the 650 °C annealed steel and stress induced transformation was observed. In contrast, yielding after annealing at 600 °C was controlled by plastic deformation of ferrite, with austenite transformation initiating only after yield point elongation. The sequence of deformation between constituents was readily apparent in the lattice strain and peak width data. During deformation, compressive lattice strains were always developed in austenite, ferrite plastic deformation initiated around 700 MPa in both steels, and tensile stress was preferentially transferred to deformation-induced martensite. The development of compressive strains in austenite was related to constraint of the volume expansion during austenite transformation to martensite.

Thermomechanical cycling of a Ni49.9Ti50.1 (at.%) shape memory alloy was investigated. Combined ex situ macroscopic experiments and in situ neutron diffraction measurements were performed to relate the macroscopic evolution in behavior (e.g., dimensional instabilities) observed during thermal cycling to the responsible microscopic mechanism(s) through texture, internal strain, peak shape, and phase evolution from the neutron data. Pre-deformation in the austenite or martensite phases affected the macroscopic cyclic behavior (e.g., actuation strain), depending on the level of pre-strain and the associated microstructural changes. However, the pre-deformation did not completely stabilize the cyclic response. Subsequent thermomechanical cycling revealed that the martensite texture changed with continued thermal cycling, while the austenite texture did not. For the conditions investigated, stagnation of the martensite texture occurred around the eighth cycle, consistent with asymptotic saturation of the macroscopic transformation strains. Moreover, diffraction spectra peak shapes (broadening) were found to vary with cycling indicative of the accumulation of lattice defects, consistent with the constant increase in residual strain.

Using in situ neutron diffraction technique we investigated the temperature dependent deformation mechanisms in ultrafine grained (UFG) austenitic Fe–14Cr–16Ni alloy prepared by equal channel angular pressing. Tensile test studies show diminished ductility when testing temperature increased from 20 to 200 °C. At 200 °C, non-linear lattice strain deviation on [2 0 0] orientation proceeded plastic yielding by a large margin, accompanied by a greater distortion of crystal structure. In addition, the capability to accumulate dislocations was substantially reduced at 200 °C as evidenced by lower dislocation density than that at 20 °C. Dynamic recovery expedited at elevated temperature because of enlarged critical separation distance for annihilation of dislocation dipoles via climb. Calculations show that both high angle grain boundaries and thermal kinetic energy assisted the reduction of vacancy formation energy.

Time-of-flight neutron measurements have been made at 20, 400 and 650oC on δ-processed Inconel 718 in order to measure the load sharing between the γ-phase matrix and the orthorhombic δ-phase. The strain response parallel and perpendicular to the applied stress was measured for seven γ-phase reflections and five δ-phase reflections. The latter were about 50 times weaker than the former suggesting a 2.0% concentration of the δ-phase. At all temperatures the δ-phase strain becomes strongly tensile parallel to the loading direction but also exhibits plastic deformation. However, the nature of the three orthorhombic strains changes with temperature.

Near-field high energy x-ray diffraction microscopy (nf-HEDM) and high energy x-ray micro-tomography (μT) have been utilized to characterize the pore structure and grain morphology in sintered ceramic UO2nuclear fuel material. μT successfully images pores to 2-3μm diameters and is analyzed to produce a pore size distribution. It is apparent that the largest number of pores and pore volume in the sintered ceramic are below the current resolution of the technique, which might be more appropriate to image cracks in the same ceramics. Grain orientation maps of slices determined by nf-HEDM at 25 μm intervals are presented and analyzed in terms of grain boundary misorientation angle. The benefit of these two techniques is that they are non-destructive and thus could be performed before and after processes (such as time at temperature or in-reactor) or even in-situ.

The evolution of lattice strains in a fully recrystallised Fe–24Mn–3Al–2Si–1Ni–0.06C TWinning Induced Plasticity (TWIP) steel subjected to uniaxial tensile loading up to a true strain of ~35% was investigated via in-situ neutron diffraction. Typical of fcc elastic and plastic anisotropy, the {111} and {200} grain families record the lowest and highest lattice strains, respectively. Using modelling cases with and without latent hardening, the recently extended Elasto-Plastic Self-Consistent model successfully predicted the macroscopic stress–strain response, the evolution of lattice strains and the development of crystallographic texture. Compared to the isotropic hardening case, latent hardening did not have a significant effect on lattice strains and returned a relatively faster development of a stronger 〈111〉 and a weaker 〈100〉 double fibre parallel to the tensile axis. Close correspondence between the experimental lattice strains and those predicted using particular orientations embedded within a random aggregate was obtained. The result suggests that the exact orientations of the surrounding aggregate have a weak influence on the lattice strain evolution.

In situ neutron diffraction data was collected during elastic loading of rolled foils of uranium–10 wt.% molybdenum bonded to a thin layer of zirconium. Lattice parameters were ascertained from the diffraction patterns to determine the elastic strain and, subsequently, the elastic moduli and Poisson’s ratio in the rolling and transverse directions. The foil was found to be elastically isotropic in the rolling plane with an effective modulus of 86 ± 3 GPa and a Poisson’s ratio 0.39 ± 0.04.

We draw upon existing knowledge of twinning and slip mechanics to develop a diffraction analysis model that allows for empirical quantification of individual deformation mechanisms to the macroscopic behaviors of low symmetry and phase transforming crystalline solids. These methods are applied in studying elasticity, accommodation twinning, deformation twinning, and slip through neutron diffraction data of tensile and compressive deformations of monoclinic NiTi to ~18% true strain. A deeper understanding of tension–compression asymmetry in NiTi is gained by connecting crystallographic calculations of polycrystalline twinning strains with in situ diffraction measurements. Our analyses culminate in empirical, micromechanical quantification of individual elastic, accommodation twinning, deformation twinning, and slip contributions to the total macroscopic stress–strain response of a monoclinic material subjected to large deformations. From these results, we find that 20–40% of the total plastic response at high strains is due to deformation twinning and 60–80% due to slip.

Lattice strains induced by cooling textured, depleted U, from 500 °C to ambient temperature are measured using in situ neutron diffraction and simulated using an elastoplastic self-consistent polycrystal model. The results show that the high anisotropy of the single-crystal thermoelastic response induces thermal stresses sufficient to cause plastic relaxation. Incorporation of ½ 〈 1 1 ¯ 0 〉 { 1 1 0 } slip enables modeling of the observed internal strain evolution, although diffusional effects may also contribute to the observed relaxation.

The recovery of deformed beryllium was studied with mechanical testing and in situ neutron diffraction measurements. The initial texture of the material and the deformation rate were manipulated to produce four distinct deformation microstructures. The dislocation density was determined from line profile analysis of the neutron diffraction data collected as a function of temperature during annealing to a maximum homologous temperature of 0.53 following deformation. Mechanical testing was completed after the in situ annealing to determine the extent of the recovery of the flow stress. Both the dislocation density and flow stress recovered significantly by a relatively low homologous temperature of 0.3. A comparison with model calculations using a dislocation-based hardening law indicates that it is forest-type dislocations that annihilate during the relatively low temperature anneal; the dislocation substructure was stable at these temperatures. Finally, the motion of the dislocations during annealing prevented the development of intergranular thermal stresses due to the crystallographically anisotropic thermal expansion of beryllium.

The high-resolution neutron diffraction and acoustic emission (AE) techniques have been used for in-situ investigation of deformation twinning and microstructure evolution in cast polycrystalline magnesium. The combination of these two techniques results in obtaining complementary information about the twinning mechanism and evolution of the dislocation structure during the straining. The dependence of the mechanisms of the plastic deformation on loading mode is discussed in detail. The microscopy investigations revealed a difference in twin number and size after tension and compression, respectively.

Rolled beryllium samples in the form of rectangular parallelepipeds were deformed at strain rates of 0.001/s and 5/s through multiple strain paths. Samples were initially deformed in-plane nominally −0.22 in compression at a rate of 5/s to populate the microstructure with twins and then reoriented and deformed a second time either in the through-thickness direction or the other in-plane direction. The microstructure (texture and internal strain) were monitored through in-situ and ex-situ diffraction measurements using neutron diffraction on the HIPPO diffractometer at LANSCE, and high energy X-ray diffraction on the 1-ID-C beamline at the APS. Twin reversal is observed when the sample is reoriented and deformed a second time in the TT direction. The twin reversal is strain rate independent in contrast to the strong strain rate dependence observed during twinning in beryllium. Deformation twinning is also observed during secondary compression in the second in-plane direction, but from the current data set we cannot determine with certainty if these twins originate from the parent orientation or the twins formed during primary in-plane compression. As a whole, this data set creates a very demanding test for the development of polycrystalline plasticity models of deformation in hexagonal metals.

We report results from neutron diffraction experiments where partitioning of applied tensile load between the inner and outer wires of seven-wire parallel and quasi-parallel wire strands were measured while 1-all wires were undergoing elastic deformation, 2-where one wire within the bundle was undergoing plastic flow and, 3-when one or more wires fractured under load. The results indicate that mechanical interference and friction mechanisms have similar contributions to the load transferred to fractured wires, and both mechanisms should be included in analytical or numerical formulations of strain partitioning in quasi-parallel wire cables.

An experimental and theoretical investigation was carried out to study the strain rate dependent plastic response of beryllium over a wide range of applied compression strain rates, 10 −4 –10 4 /s. At each rate, the evolution of flow stress and the final texture with deformation was obtained from a non-textured hot-pressed (HP) sample and a textured rolled sheet. The rolled sheet material was compressed in both the in-plane (IP) and through-thickness (TT) direction for comparison. The twin volume fraction was determined from the change in texture. The activity of twinning was strongly dependent on strain rate in the IP and HP samples. We applied a multi-scale constitutive model for hexagonal close packed polycrystals that accounts for crystallographic slip and twinning on individual systems in each crystal, as well as twin reorientation. Rate effects enter the calculations only through thermally activated dislocation glide on the active slip modes. The importance of this study is that it points to the necessity of using a crystallographic model based on microstructure evolution to understand the role played by plastic anisotropy, slip–slip competition, and slip–twin competition, in the mechanical response of HCP aggregates. The model reproduces the observed flow curves and texture evolution for all tests with a unique single crystal set of parameters.

Elastic residual strains were measured in a laser welded commercially pure titanium ring using a non-destructive neutron diffraction technique in order to determine the resolution of this method for the characterization of small laser welds. In addition, these measurements were used to validate calculations made using residual strain data obtained from simulation of the residual stress near the weld. The measured strains were in good agreement with the simulated results.

The large strain deformation of polycrystalline uranium 6 wt pct niobium (U6Nb) was studied in situ during uniaxial tensile and compressive loading by time-of-flight neutron diffraction. Diffraction patterns were recorded at incremental strains to a maximum of approximately 0.13 tensile and 0.15 compressive true strain. A discrete reorientation of the crystallographic texture under tensile straining between 0.04 and 0.08 true strain is consistent with a previously unobserved mechanical deformation twinning mechanism, identified as either a (100) or (010) mechanical twin system. Beyond this, a continuous texture reorientation towards an (010) crystal orientations indicates that a slip mechanism is likely predominant. An analogous mechanical twin system was not observed in compression at large strain.

Precipitate strengthening effects toward the improved creep behavior have been investigated in a ferritic superalloy with B2-type (Ni,Fe)Al precipitates. In situ neutron diffraction has been employed to study the evolution of the average phase strains, (hkl) plane-specific lattice strains, interphase lattice misfit, and grain-orientation texture during creep deformation of the ferritic superalloy at 973 K (700 °C). The creep mechanisms and particle-dislocation interactions have been studied from the macroscopic creep behavior. At a low stress level of 107 MPa, the dislocation-climb-controlled power-law creep is dominant in the matrix phase, and the load partition between the matrix and the precipitate phases remains constant. However, intergranular stresses develop progressively during the primary creep regime with the load transferred to 200 and 310 oriented grains along the axial loading direction. At a high stress level of 150 MPa, deformation is governed by the thermally activated dislocation glide (power-law breakdown) accompanied by the accelerated texture evolution. Furthermore, an increase in stress level also leads to load transfer from the plastically deformed matrix to the elastically deformed precipitates in the axial direction, along with an increase in the lattice misfit between the matrix and the precipitate phases.

In this paper we report in situ neutron diffraction results of fine-grained (8 μm) polycrystalline titanium sulfocarbide samples loaded to 700 MPa. The overall strains, and those on individual planes, are modeled via the elastoplastic self-consistent approach using elastic constants derived from ab initio calculations. Based on the results, we conclude that the response at stresses below 1 GPa, is, for the most part linear elastic and that when the theoretical elastic constants are combined with the elastoplastic self-consistent method, accurate predictions can be obtained of both the overall stress–strain curves and, more importantly, the 0 0 01, 1 0 1 ¯ , and 1 0 1 ¯ 0 reflections.

The strain-induced face-centered cubic (FCC) → hexagonal-close packed (HCP) phase transformation in a cobalt-based superalloy was investigated with four in situ loading neutron-diffraction experiments: monotonic tension, monotonic compression, high-cycle fatigue, and low-cycle fatigue. The transformation onsets for the four respective cases were 685 MPa, 698 MPa, 1 cycle, and 3 cycles, respectively. The HCP phase accumulated at rates of 0.1 wt.%-MPa −1 and 0.05 wt.%-MPa −1 for the tension and compression cases, respectively. For the cyclic-loading cases, the accumulation rates were found to be inversely proportional to the number of fatigue cycles. The results under the different loading modes suggest that the phase transformation occurs according to a tensile plastic-work criterion.

The damping behavior of a model ferroelastic-reinforced–metal matrix composite (FR-MMC) system was examined through the incorporation of barium titanate (BaTiO3) particles into a Cu-10 wt pct Sn (bearing bronze) matrix. The damping properties of the resulting FR-MMC were investigated vs frequency, temperature (above and below the Curie temperature of the ferroelastic reinforcement), and number of strain cycles. Dynamic mechanical analysis (DMA) indicates that the incorporation of the ferroelastic-capable reinforcement significantly augments the damping capability relative to the matrix alone, and also with respect to the damping that would result from the presence of passive composite reinforcements. Neutron diffraction data demonstrate a strong correlation of domain reorientation activity to imposed stress level and demonstrate a degree of reversibility important to the potential practical application of this mechanism of damping.

A complimentary set of experiments, in situ neutron diffraction and ex situ synchrotron X-ray diffraction, were used to study the phase-transformation and subgrain-deformation characteristics of a cobalt-based superalloy. The neutron diffraction indicated a strain-induced phase transformation in the cobalt-based superalloy under uniaxial tension and compression. The synchrotron X-ray diffraction revealed stacking-fault accumulation and twinning under the same loading conditions. The extent of transformation was found to be greater under tension than under compression. Tensile plastic strains below 2% were accommodated by the stacking-fault creation, while those greater than 2% were accommodated by the phase transformation. Twinning was found to be more active under compressive loading than under tensile loading.

The effect of texture on the low-cycle fatigue behavior of a rolled magnesium alloy, AZ31B, was studied at room temperature. It is shown that the Coffin–Manson and Basquin relationships can be used to describe the fatigue resistance of the alloy. The alloy loaded along the rolling direction exhibits only slightly better low-cycle fatigue resistance than that loaded along the transverse direction, due to the in-plane texture symmetry. The in-plane cases exhibit better fatigue behavior than the through-thickness loading. Neutron diffraction and synchrotron diffraction were employed to assist in making mechanistic understandings for the findings. The fundamental difference in the low-cycle fatigue behaviors between the in-plane and through-thickness loadings is attributed to the different activation sequences of twinning and detwinning mechanisms involved and, particularly, the greater requirement for c-axis compression of the grains during the through-thickness tests. The different activation sequences are essentially determined by the initial crystallographic texture, such that the inverted hysteresis-loop shapes are observed.

Following a preceding work on cordierite thermal expansion, high temperature neutron diffraction has allowed observation of lattice strain with temperature in extruded porous cordierite in the form of a rod. The temperature dependence of the grain microstress in the rod was determined from neutron diffraction data (by comparison with powder data) and from the macroscopic thermal expansion (by the integrity factor model). The two methods are in good agreement.

The hydride-phase formation and its influence on the fatigue behavior of a Zircaloy-4 alloy charged with hydrogen gas are investigated. First, the microstructure and fatigue crack propagation rate of the alloy in the as-received condition are studied. Second, the formation and homogeneous distribution of the delta zirconium hydride in the bulk and its effect on the fatigue crack propagation rate are presented. The results show that in the presence of hydrides, the zirconium alloy exhibits reduced toughness and enhanced crack growth rates. Finally, the influence of a preexisting fatigue crack in the specimen and the subsequent hydride formation are examined. The residual lattice strain profile around the fatigue crack tip is measured using neutron diffraction. It is observed that the combined effects of residual strains and hydride precipitation on the fatigue behavior are more severe leading to propagation of the crack under near threshold loading.

Recently cobalt was classified as a kinking nonlinear elastic, KNE, solid. Fully reversible incipient kink bands, IKBs, were invoked to explain both its microyielding and hysteretic stress–strain curves. Herein we present further evidence and insights in the KNE nature of cobalt by measuring its mechanical hysteresis as a function of grain size, pre-strain and testing temperature. Unlike previous work, in coarse-grained cobalt, something other than grain boundaries determine the domain size. The hysteresis loops were only obtained at temperatures where cobalt was hexagonal-close packed. In situ neutron diffraction strains could only account for ≈1/3 of the total strain measured and ruled out dislocation pileups as the source of the remaining strain suggesting that it is due to IKBs. The totality of our results can be successfully explained and quantified by our microscale IKB-based model, based on which we estimate the critical resolved shear stress of basal plane dislocations to be 13 ± 3 MPa and the reversible dislocation density to be 1.5–6 × 10 13 m −2 in the ≈200–400 MPa stress range.

Plastic deformation of hexagonal metals such as beryllium occurs by a mix of dislocation slip and deformation twinning mechanisms. Slip and twinning are controlled by different mechanisms at the atomic scale, and thus respond differently to variations in strain rate. In general, deformation twinning is expected to be favored by high strain rate conditions. Both textured and randomly textured polycrystalline beryllium samples were deformed at strain rates from 0.0001/s to 5000/s. The yield point was found to be strain rate insensitive over the 7+ orders of magnitude of strain rate. The hardening, however, is strongly rate dependent for some of the initial textures, depending on loading direction relative to the basal poles. Optical microscopy and neutron diffraction measurements of the crystallographic texture were carried out to monitor the evolution of the microstructure and, specifically, the activity of deformation twinning as a function of strain rate. The relative roles of the active slip and twin deformation mechanisms are linked to the observed rate dependence of the flow stress.