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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.

The effect of heat-treatment and build orientation on martensitic phase transformation in additively manufactured (AM) 304L stainless steel is studied and compared with conventionally produced wrought material. The relationships between observed martensitic transformations and material microstructures and their effects on mechanical strength are established through experimental observations. In situ high-energy X-ray powder diffraction measurements were performed to monitor the evolution of ϵ and α′ martensite during compressive loading of stainless steel. Electron backscatter diffraction (EBSD) was used to provide insight on initial grain morphology, crystallographic misorientation within grains, and crystallographic texture. Heat treatment alters the microstructure of AM samples creating different initial conditions. This difference in starting microstructure resulted in variability in martensitic transformation during compressive deformation. The rate of martensitic transformation decreased for AM samples treated with temperatures up to 1100∘C, after which the AM microstructures recrystallized, resulting in increased rate of martensitic transformation for those samples treated at higher temperatures. It was also observed that aligning the axis of compression with the AM build direction resulted in a lower rate of strain-induced martensite formation as opposed to aligning the compression axis perpendicular to it. More favorable distribution of crystal orientations in the latter loading orientation promoted martensitic transformation. These and additional experimental observations from EBSD in terms of kernel average misorientation, mean grain orientation spread, and mean crystallite size reveal strong microstructural effects on strength of additively manufactured metallic materials.

A solid state phase transformation of Ti-6Al-4V was studied using high speed in situ x-ray diffraction measurements made during rapid cooling of a cold metal transfer arc weld bead deposited onto a water cooled substrate. Analysis of body centered cubic (BCC) and hexagonal close packed (HCP) lattices revealed an abrupt, nonlinear shift in the lattice parameters of both phases just after the HCP phase had nucleated. Postmortem transmission electron microscopy confirmed that V diffusion was mostly suppressed during cooling. Together, these results indicate that at this cooling rate of approximately 104 K/s, which is representative of cooling rates of many additive manufacturing and welding processes, kinematic coherency of the BCC–HCP interfaces gives rise to the anomalous lattice expansion and contraction behaviors of both phases during the initial nucleation and growth stages of (mostly) martensitic transformation from BCC to HCP; the role of diffusion in such lattice anomalies is shown to be minimal.

Fabricating parts using laser powder bed fusion (LPBF) is of growing interest to many fields, ranging from medical to aerospace, but this process is often plagued with residual stresses that can reach magnitudes as high as the yield strength of the material. Previous work has demonstrated the ability to reduce residual stress during LPBF by over 90% using an in situ annealing method that makes use of large area, shaped light illumination from a set of laser diodes. In this work, an in-depth analysis of the effectiveness of this in situ residual stress reduction technique is presented. A custom LPBF system was used to fabricate 316 L stainless steel parts, and the stresses of these parts were analyzed using the contour method and neutron diffraction on various planes within the samples. These spatial measurements revealed stress reductions near the edges and base of the samples in each of the three measured orthogonal stress directions, in addition to an overall reduction in stress owing to in situ application of laser diode heating. The experimental results were found to be in excellent agreement with numerical thermomechanical simulations that captured the effects of various processing parameters. Furthermore, in cases where the annealing was only performed once every 5 layers, the residual stress was similarly reduced, which indicates that further optimization might be achieved to limit additional processing time during the builds while still relieving equivalent amounts of stress.

A simple statistical analysis which yields the precision, resolution, accuracy and trueness of diffraction-based lattice strain measurements is discussed. The procedure consists of measuring the thermal expansion induced in each component of an ideal non-reacting two-component crystalline powder sample in situ. One component, with a high coefficient of thermal expansion (CTE), serves as an internal thermometer. The quantities of interest are obtained by determining the smallest statistically significant thermal lattice strain which can be detected through diffraction analysis in the second, low-CTE, component in response to controlled temperature changes. This procedure also provides a robust check of the alignment of the diffraction system and is able to reveal the presence of systematic errors. The application of this technique to a time-of-flight engineering diffractometer/strain scanner is presented.

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.

An in-situ high-pressure neutron diffraction experiment was conducted on a δ-phase stabilized plutonium alloy with isotope 242 Pu. Upon room-temperature compression, neither of the previously reported pressure-induced transformation paths, δ → α′ or δ → γ’ → α′, was observed up to 1.2 GPa. Instead, a drastic reduction in the diffraction intensity of the δ phase was observed when the pressure was above 0.8 GPa. At the highest pressure of the experiment (1.2 GPa), the diffraction data appear to be characteristic of an amorphous state, manifested by the diminishing intensities of all diffraction lines. In addition, no evidence was found to support the transformation to a body-centered tetragonal structure (δ’), which was previously inferred from the diffraction line broadening during initial compression to 0.1 GPa. The discrepancies between the present and previous experiments suggest a substantial strain-induced stabilization of the δ-phase and is presumably attributed to the different stress states in the high-pressure environments. From the pressure - volume measurements, the determined isothermal bulk modulus for the δ-phase is in the range of 31.9 ± 1.3–34.8 ± 1.8 GPa using different pressure scales, comparable to those obtained from the resonant ultrasound spectroscopy measurements of the alloys of similar composition. The pressure-induced elastic softening is neither convinced in the present work, nor can it be resolved from the diffraction experiments if it is intrinsically weak.

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.

One of the primary barriers for adoption of additive manufacturing (AM) has been the uncertainty in the performance of AM parts due to residual stresses/strains. The rapid heating and cooling rates from the thermal history of the laser melting process result in high residual stresses/strains that produce significant part distortion. Efforts to mitigate residual stresses using post-process heat treatments can significantly impact the microstructures of the AM part which may lead to further issues. Therefore, the ability to accurately predict the residual stresses in as-built AM parts is crucial, and rigorous benchmark measurements are needed to validate such predictions. To fill this need, the AM-Bench aims to provide high-fidelity residual stress and strain benchmark measurements in well-characterized AM bridge-shaped parts. The measurements reported here are part of the residual elastic strain benchmark challenge CHAL-AMB2018-01-RS. Residual strains and stresses in this work were measured using neutron diffraction, synchrotron X-ray diffraction, and the contour method. Part deflection measurements were performed using a coordinate measurement machine after the part was partially separated from the build plate. These independently measured results show a high degree of agreement between the different techniques.

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.

The build-up of residual stresses in a part during laser powder bed fusion provides a significant limitation to the adoption of this process. These residuals stresses may cause a part to fail during a build or fall outside the specified tolerances after fabrication. In the present work a thermomechanical model is used to simulate the build process and calculate the residual stress state for Ti–6Al–4V specimens built with continuous and island scan strategies. A layer agglomeration, or lumping, approach is used to speed up the computations. A material model is developed to naturally capture the strain-rate dependence and annealing behavior of Ti–6Al–4V at elevated temperatures. Results from the thermomechanical simulations showed good agreement with synchrotron X-ray diffraction measurements used to determine the residual elastic strains in these parts. However, the experimental measurements showed higher residual strains for the specimen built with an island scan strategy; a trend not fully captured by the simulations. Parameter studies were performed to fully understand the advantages and limitations of the current simulation methodology. Reasons for both the computational and experimental findings are discussed.

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 additive manufacturing of metals as compared to conventional processing, the directional track-by-track and layer-by-layer nature of the fabrication process can lead to residual stresses that locally are both directionally and spatially heterogeneous. Much of the existing literature has focused either on the macroscale residual stress inside the entire part, or on the microscale residual stresses that are created around a scan vector, thereby neglecting the intermediate length-scale of the different layers. The objective of this research is to investigate such mesoscale residual stress distributions across several layers in Ti-6Al-4V components produced by laser metal deposition process. The incremental centre hole drilling and incremental slitting methods provide measurements with excellent spatial resolution within and across the layer length scale. In this work, the two methods complemented each other to quantify both mesoscale and directional variations of residual stress that correlate with the deposition pattern. Our findings also provide strong evidence that an oscillatory residual stress variation persists even after thermal cycling that occurs during deposition of subsequent layers.

Time-of-flight neutron diffraction measurements were conducted at ambient conditions to study microstructures of the δ-phase 239Pu-2at% Ga alloy. Based on the line profile analysis of diffraction data we derived dislocation densities using a correction routine to account for the anisotropic strain broadening. Our results show that the average dislocation density in the as-received sample, previously treated at cryogenic temperatures, is five times higher than the dislocation density measured after annealing the sample, indicating that the neutron instrumentation used in this work has sufficient resolution to detect the dislocation density changes in different sample processing. These results are also in reasonably good agreement with the dislocation densities previously reported based on TEM observations and x-ray diffraction data, suggesting that the simple correction routines applied in this work have a fairly good fidelity for deriving important microstructural information such as dislocation density for elastically highly anisotropic δ-phase 239Pu-Ga alloys.

Non-destructive evaluation of plastically deformed metals is particularly valuable both for assessing dislocation microstructures and validating constitutive models. Among other methods, diffraction line profile analysis has been widely used to extract dislocation densities in deformed bulk single crystals and polycrystals. To date, the interpretation of whole line diffraction profiles relies on the use of semi-analytical models such as the extended convolutional multiple whole profile (eCMWP) method. This study proposes and assesses the prospects of a data-driven approach to extract dislocation densities from experimentally gathered whole line diffraction profiles. A database of virtual diffraction whole line profiles of Ta single crystals containing varying dislocation densities is generated. The dislocation microstructures are synthesized using discrete dislocation dynamics, and two distinct strain-based virtual diffraction algorithms are used to generate diffraction profiles. Instrumental broadening is applied to the synthetic profiles. The databases inform two Gaussian process regression-based surrogate models, allowing dislocation densities to be extracted from experimental profiles. The method is applied to 11 experimentally obtained whole line diffraction profiles gathered from plastically deformed Ta polycrystals. Upon applying both surrogate models to the experimental data and using eCMWP as a point of comparison, it is found that data-driven predictions of dislocation density can clearly capture the evolution of dislocation density with applied strain. Finally, the data-driven model is used to explore the effect of heterogeneous dislocation densities in microstructures containing grains, which may lead to more accurate data-driven predictions of dislocation density in plastically deformed polycrystals.

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.

The effect of heat-treatment and build orientation on martensitic phase transformation in additively manufactured (AM) 304L stainless steel is studied and compared with conventionally produced wrought material. The relationships between observed martensitic transformations and material microstructures and their effects on mechanical strength are established through experimental observations. In situ high-energy X-ray powder diffraction measurements were performed to monitor the evolution of e and α' martensite during compressive loading of stainless steel. Electron backscatter diffraction (EBSD) was used to provide insight on initial grain morphology, crystallographic misorientation within grains, and crystallographic texture. Heat treatment alters the microstructure of AM samples creating different initial conditions. This difference in starting microstructure resulted in variability in martensitic transformation during compressive deformation. The rate of martensitic transformation decreased for samples treated with temperatures up to 1100oC, after which the AM microstructures recrystallized, resulting in increased rate of martensitic transformation for those samples treated at higher temperatures. It was also observed that aligning the axis of compression with the AM build direction resulted in a lower rate of strain-induced martensite formation as opposed to aligning the compression axis perpendicular to it. More favorable distribution of crystal orientations in the latter loading orientation promoted martensitic transformation. These and additional experimental observations from EBSD in terms of kernel average misorientation, mean grain orientation spread, and mean crystallite size reveal strong microstructural effects on strength of additively manufactured metallic materials.

During the laser-powder bed fusion ( L -PBF) process, high laser intensities, short interaction times and highly localized heat input drive large thermal gradients that result in a state of high residual stresses. Generally, the residual stresses that develop during the L -PBF process can compromise the performance of the component. Up to now, the literature has indicated that the magnitude of the residual stresses can be affected by various process parameters. In this study, all process parameters such as laser power and speed are held fixed and the focus is solely on the effect of the laser scan strategy on the three-dimensional residual stress state of L -PBF metallic components. Four Ti-6Al-4V bridge shaped components were built using island and continuous scanning patterns parallel and offset 45° from the sample axes. High-energy X-ray diffraction was used to determine the residual stress field in each of the components. Two of them were re-measured after being partially removed from the build plate. The assumptions implicit in diffraction measurements of stress are reviewed and discussed in depth because the unique microstructure associated with L-PBF Ti-6Al-4V renders the validity of those assumptions uncertain. Specifically, additional data was collected and analyzed to evaluate the relationship between grain scale and macroscopic scale stresses. The observed residual stresses were large, ½ to ¾ of the yield strength, particularly the build direction stresses near the lateral edges of the bridges. In this work, the higher stresses were observed in the bridges built via the island scan strategies, chiefly near the edges of the parts.

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.

The mechanical properties of uranium-niobium alloys evolve with aging at relatively low temperatures due to subtle microstructural changes. In-situ neutron diffraction measurements during aging of a monoclinic U-6Nb alloy at temperatures to 573 K were performed to monitor these changes. Further, in-situ neutron diffraction studies during deformation of U-6Nb in the as-quenched state and after aging for two and eight hours at 473 K were completed to assess the influence of microstructural evolution on mechanical properties. With heating, large anisotropic changes in lattice parameter were observed followed by relaxation with time at the aging temperature. The lattice parameters return to nearly their initial values with cooling. The active plastic deformation mechanisms including, in order of occurrence, shape-memory de-twinning, mechanical twinning, and slip-mediated deformation do not change with prior aging. However, the resistance to motion of the as-quenched martensitic twin boundaries increases following aging, resulting in the observed increase in initial yield strength.

Al clad U-10Mo fuel plates are being considered for conversion of several research reactors from high-enriched to low-enriched U fuel. Neutron diffraction measurements of the textures, residual phase stresses, and dislocation densities in the individual phases of the mini-foils throughout several processing steps and following hot-isostatic pressing to the Al cladding, have been completed. Recovery and recrystallization of the bare U-10Mo fuel foil, as indicated by the dislocation density and texture, are observed depending on the state of the material prior to annealing and the duration and temperature of the annealing process. In general, the cladding procedure significantly reduces the dislocation density, but the final state of the clad plate, both texture and dislocation density, depends strongly on the final processing step of the fuel foil. In contrast, the residual stress state of the final plate is dominated by the thermal expansion mismatch of the constituent materials.

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.

Samples harvested from an HT-9 fuel test assembly (ACO-3) irradiated for six years in the Fast Flux Test Facility (FFTF) reaching 2–147 dpa at 382–504 °C were deformed in-situ while collecting high-energy X-ray diffraction data to monitor microstructure evolution. With the initiation of plastic deformation, all samples exhibited a clear load transfer from the ferrite matrix to carbide particulate. This behavior was confirmed by modeling of the control material. The evolution of dislocation density in the material as a result of deformation was characterized through full pattern line profile analysis. The dislocation densities increased substantially after deformation, the level of dislocation evolution observed was highly dependent upon the irradiation temperature of the sample. Differences in both the yield and hardening behavior between samples irradiated at higher and lower temperatures suggest the existence of a transition in tensile behavior at an irradiation temperature near 420 °C dividing regions of distinct damage effects.

Neutron diffraction was used to determine residual stress in monolithic two Al-clad U 10 weight percent Mo mini-fuel plates and a full sized fuel plate. One mini-plate was cooled following hot isostatic pressing at a rate of 6.75 °C/min, the second at 0.675 °C/min. A non-traditional method of calibrating the neutron diffractometer at each measurement point was necessitated by the thin nature of the sample. The in-plane stresses in the U–10Mo foils are relatively large, −250 MPa in the U–10Mo foil of the fast cooled mini-plate,-150 MPa in the slow cooled mini-plate and −275 MPa in the full-sized plate. Likewise, the in-plane stresses in the Al-cladding of the fast-cooled mini-plate and full-sized plate were determined to reach ∼50 MPa, while in the slow-cooled sample the stresses in the Al cladding were on the level of the measurement uncertainty. The in-plane stresses in the Zr diffusion barrier were estimated to be as large as −300 MPa.

We study the thermally activated, slow conversion of the hysteretically retained ω phase into stable α phase in recovered samples of shocked zirconium. The ω-phase decays in time following an algebraic law, unlike the predictions of the nucleation-growth framework for first order transitions, and residual volume fractions of phases and dislocation densities are related by a power law. We propose an explanation for the annealing mechanism through coupled dynamics of dislocations and phase change. We find that the long-time behavior is controlled by the interplay of dislocations, shear fluctuations, and remnant volume fractions of phases, which lead to an algebraic decay in time. For late time, thermally activated quantities such as the dislocation mobility and nucleation rate set the timescale and control the algebraic behavior, respectively. At high enough temperatures this behavior is effectively indistinguishable from standard Avrami kinetics.

Additively-manufactured Ti-6Al-4V (Ti64) exhibits high strength but in some cases inferior elongation to those of conventionally manufactured materials. Post-processing of additively manufactured Ti64 components is investigated to modify the mechanical properties for specific applications while still utilizing the benefits of the additive manufacturing process. The mechanical properties and fatigue resistance of Ti64 samples made by electron beam melting were tested in the as-built state. Several heat treatments (up to 1000 °C) were performed to study their effect on the microstructure and mechanical properties. Phase content during heating was tested with high reliability by neutron diffraction at Los Alamos National Laboratory. Two different hot isostatic pressings (HIP) cycles were tested, one at low temperature (780 °C), the other is at the standard temperature (920 °C). The results show that lowering the HIP holding temperature retains the fine microstructure (~1% β phase) and the 0.2% proof stress of the as-built samples (1038 MPa), but gives rise to higher elongation (~14%) and better fatigue life. The material subjected to a higher HIP temperature had a coarser microstructure, more residual β phase (~2% difference), displayed slightly lower Vickers hardness (~15 HV10N), 0.2% proof stress (~60 MPa) and ultimate stresses (~40 MPa) than the material HIP’ed at 780 °C, but had superior elongation (~6%) and fatigue resistance. Heat treatment at 1000 °C entirely altered the microstructure (~7% β phase), yield elongation of 13.7% but decrease the 0.2% proof-stress to 927 MPa. The results of the HIP at 780 °C imply it would be beneficial to lower the standard ASTM HIP temperature for Ti6Al4V additively manufactured by electron beam melting.