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The tensile properties of additively manufactured (AM) metals and alloys are among the most important variables that impact the potential applications of these materials. Here we examine and report on the tensile properties of AM 316L stainless steels fabricated by the laser powder-bed-fusion (L-PBF) technique, via twelve sets of optimized laser processing parameters that produce materials with density >98.8 ± 0.10%. A heterogeneous microstructure is observed in all L-PBF samples, including microscopic features such as dislocations, cellular walls, elemental segregations, local misorientations, impurities, precipitates, and a large fraction of low-angle grain boundaries (2-10°, ∼40–60%). The derived average grain size defined by high-angle grain boundaries (>10°) is ∼30–50 μm. Tensile testing reveals a yield strength ranging from 552 to 635 MPa and a tensile-elongation-to-failure (TEF) of 0.09–0.42 for directly-printed samples, whereas these values are 592–690 MPa and 0.29–0.50 for samples machined from the as-built rectangular thin plates. In all samples, we observe a variation of tensile yield strength within ∼15% but not the TEF, suggesting marginal microstructural changes despite a wide range of laser processing parameters. The large scatter of TEF in directly-printed samples originates from the sensitivity of thin gauge geometry (∼2 mm2 cross-section area) to the built-in flaws. We measured a substantially higher strain rate sensitivity (m∼0.02–0.03) of L-PBF 316L compared to the coarse-grained counterparts (∼0.006), together with a small activation volume of ∼20–30b3 (where b is the Burgers vector of 316L). These deformation kinetics parameters suggest that the tensile plasticity of L-PBF 316L is controlled by a much finer microstructural length scale than the measured grain size, consistent with the high strength and juxtaposed nano- to macro-structures seen in these materials. Strategies to optimize the tensile properties of AM materials are discussed.

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 (AM) is expected to become an established manufacturing technology in the near future. The growing penetration of AM at manufacturers across the world and the dependence of this technology on computerization have already raised security concerns, some of which have been proven experimentally. In this paper, we analyze the AM Security from three awareness perspectives: exposure to an attack, evaluation of the system, and potential liability for a successful attack. For each of these perspectives, we first introduce the conceptual background and then provide the analysis of its applicability to AM, highlighting its distinctiveness from closely related subtractive manufacturing (SM). Our analysis shows that, while there is a certain overlap between AM and SM security, the AM requires a separate and unique perspective and approach undertaken by experts with relevant domain expertise.

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.

The evaluation of simple thermal model of selective laser melting (SLM) process shows that the temperature distribution in the sample is characterized by two dimensionless parameters: normalized enthalpy and the ratio of dwell time to the thermal diffusion time. We demonstrated that the melt depth data taken for different machines for different materials collapsed in one curve, making possible to rescale the optimal processing parameters between the different materials and machines. The melt pool depth, width and the length are the universal function of these two parameters. Within the operational range of parameters for SLM these functions can be interpolated by the simple algebraic expressions given the possibility to reduce the calculation of the melt pool characteristic to spreadsheet model.

Additive manufacturing (AM) is a rapidly growing, multibillion dollar industry. AM is increasingly being used to manufacture functional parts, including components of safety critical systems in aerospace, automotive, and other industries. This makes AM an attractive attack target. AM Security is a fairly new field of research that addresses this novel threat. This paper serves dual purposes: For researchers just entering AM security, we provide an in-depth introduction to this highly multi-disciplinary research field. And, for active researchers in the field, this paper provides a comprehensive, structured survey of the state of the art as well as our proposal for attack taxonomies.

Additive Manufacturing is a promising way of processing tungsten, with opportunities to create more complex parts than are possible using other powder metallurgical routes. This may lead to extended applications such as collimators, in fusion reactors, or in other structurally loaded, high temperature environments. The poor thermal shock resistance and ductile-to-brittle transition that occurs in tungsten above room temperature are challenges that hinder production of fully dense and crack free parts. This research employs high speed in-situ monitoring of Selective Laser Melting of single tracks to visualize crack initiation and propagation. The circumstances that lead to cracking are correlated with microstructural morphology and processing conditions.

Laser Powder-Bed Fusion (L-PBF) metal-based additive manufacturing (AM) is complex and not fully understood. Successful processing for one material, might not necessarily apply to a different material. This paper describes a workflow process that aims at creating a material data sheet standard that describes regimes where the process can be expected to be robust. The procedure consists of building a Gaussian process-based surrogate model of the L-PBF process that predicts melt pool depth in single-track experiments given a laser power, scan speed, and laser beam size combination. The predictions are then mapped onto a power versus scan speed diagram delimiting the conduction from the keyhole melting controlled regimes. This statistical framework is shown to be robust even for cases where experimental training data might be suboptimal in quality, if appropriate physics-based filters are applied. Additionally, it is demonstrated that a high-fidelity simulation model of L-PBF can equally be successfully used for building a surrogate model, which is beneficial since simulations are getting more efficient and are more practical to study the response of different materials, than to re-tool an AM machine for new material powder.

• This article focuses on reviewing modeling and simulation effort in metal additive manufacturing taking places at U.S. Department of Energy national laboratories.

The microstructures of rapidly solidified U-6wt%Nb powder particles synthesized by centrifugal atomization were characterized using scanning electron microscopy and transmission electron microscopy. Observed variations in microstructure are related to particle sizes. All of the powder particles exhibited a two-zone microstructure. The formation of this two-zone microstructure is described by a transition from solidification controlled by internal heat flow and high solidification rate during recalescence (micro-segregation-free or partitionless growth) to solidification controlled by external heat flow with slower solidification rates (dendritic growth with solute redistribution). The extent of partitionless solidification increased with decreasing particle size due to larger undercoolings in smaller particles prior to solidification. The metastable phases that formed are related to variations in Nb concentration across the particles. The microstructures of the powders were heavily twinned.

Additive manufacturing (AM) enables the fabrication of complex designs that are difficult to create by other means. Metal parts manufactured by laser powder bed fusion (LPBF) can incorporate intricate design features and demonstrate desirable mechanical properties. However, printing a part that is qualified for its intended application often involves reprinting and discarding many parts to eliminate defects, improve dimensional accuracy, and increase repeatability. The process of iteratively converging on the appropriate build parameters increases the time and cost of creating functional LPBF manufactured parts. This paper describes a fast, scalable method for part-scale process optimization of arbitrary geometries. The computational approach uses feature extraction to identify scan vectors in need of parameter adaptation and applies results from simulation-based feed forward control models. This method provides a framework to quickly optimize complex parts through the targeted application of models with a range of fidelity and by automating the transfer of optimization strategies to new part designs. The computational approach and algorithmic framework are described, a software package is implemented, the method is applied to parts with complex features, and parts are printed on a customized open architecture LPBF machine.

Computational models for simulating physical phenomena during laser-based powder bed fusion additive manufacturing (L-PBF AM) processes are essential for enhancing our understanding of these phenomena, enable process optimization, and accelerate qualification and certification of AM materials and parts. It is a well-known fact that such models typically involve multiple sources of uncertainty that originate from different sources such as model parameters uncertainty, or model/code inadequacy, among many others. Uncertainty quantification (UQ) is a broad field that focuses on characterizing such uncertainties in order to maximize the benefit of these models. Although UQ has been a center theme in computational models associated with diverse fields such as computational fluid dynamics and macro-economics, it has not yet been fully exploited with computational models for advanced manufacturing. The current study presents one among the first efforts to conduct uncertainty propagation (UP) analysis in the context of L-PBF AM. More specifically, we present a generalized polynomial chaos expansions (gPCE) framework to assess the distributions of melt pool dimensions due to uncertainty in input model parameters. We develop the methodology and then employ it to validate model predictions, both through benchmarking them against Monte Carlo (MC) methods and against experimental data acquired from an experimental testbed.

The metal laser powder bed fusion additive manufacturing process uses high power lasers to build parts layer upon layer by melting fine metal powders. Qualification of parts produced using this technology is broadly recognised as a significant challenge. Physics based process models have been identified as being foundational to qualification of additively manufactured metal parts. In the present article, a multiscale modelling strategy is described that will serve as the foundation upon which process control and part qualification can be built. This includes a model at the scale of the powder that simulates single track/single multilayer builds and provides powder bed and melt pool thermal data. A second model computationally builds a complete part and predicts manufactured properties (residual stress, dimensional accuracy) in three dimensions. Modelling is tied to experiment through data mining.

Laser powder-bed fusion additive manufacturing of metals employs high-power focused laser beams. Typically, the depth of the molten pool is controlled by conduction of heat in the underlying solid material. But, under certain conditions, the mechanism of melting can change from conduction to so-called “keyhole-mode” laser melting. In this mode, the depth of the molten pool is controlled by evaporation of the metal. Keyhole-mode laser melting results in melt pool depths that can be much deeper than observed in conduction mode. In addition, the collapse of the vapor cavity that is formed by the evaporation of the metal can result in a trail of voids in the wake of the laser beam. In this paper, the experimental observation of keyhole-mode laser melting in a laser powder-bed fusion additive manufacturing setting for 316L stainless steel is presented. The conditions required to transition from conduction controlled melting to keyhole-mode melting are identified.

Additive Manufacturing, a.k.a. 3D Printing, is increasingly used to manufacture functional parts, including components of safety critical systems. Therefore, assuring part quality has become of paramount importance. In-situ infrared (IR) imaging systems are a promising solution to increase final build quality and minimize time-consuming and costly post processing and characterization. However, it also raises novel security concerns. We argue that, if compromised, the same in-situ quality control can be abused to sabotage manufactured parts. As a basis for our discussion, we first detail how IR thermography is used in open-loop and, experimentally, in closed-loop quality control for powder bed fusion (PBF) systems. We then identify malicious manipulations that an adversary can perform. We discuss the consequences of the manipulations on the manufactured part's quality. For selected attacks, we also provide experimental proof of the identified manipulations and their consequences.

Additive manufacturing involves a new class of cyber-physical systems that manufacture 3D objects incrementally by depositing and fusing together thin layers of source material. In 2015, the global additive manufacturing industry had $5.165 billion in revenue, with 32.5% of all manufactured objects used as functional parts. Because of their reliance on computerization, additive manufacturing devices (or 3D printers) are susceptible to a broad range of attacks. The rapid adoption of additive manufacturing in aerospace, automotive and other industries makes it an attractive attack target and a critical asset to be protected.

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.

Effective integration of nonproliferation management into the design process is key to the broad deployment of advanced nuclear energy systems, and is an explicit goal of the Laser Inertial Fusion Energy (LIFE) project at Lawrence Livermore National Laboratory. The nuclear explosives utility of a nuclear material to a state (proliferator) or sub-state (terrorist) is a critical factor to be assessed and is one aspect of material attractiveness. In this work, we approached nuclear explosives utility through the calculation of a “figure of merit” (FOM) that has recently been developed to capture the relative viability and difficulty of constructing nuclear explosives starting from various nuclear material forms and compositions. We discuss the integration of the figure of merit into an assessment of a nuclear material theft scenario and its use in the assessment. This paper demonstrates that material attractiveness is a multidimensional concept that embodies more than the FOM. It also seeks to propose that other attributes may be able to be quantified through analogous FOMs (e.g., transformation) and that, with quantification, aggregation may be possible using concepts from the risk community.

The microstructure and properties of a material depend on dynamic processes such as defect motion, nucleation and growth, and phase transitions. Transmission electron microscopy (TEM) can spatially resolve these nanoscale phenomena but lacks the time resolution for direct observation. We used a photoemitted electron pulse to probe dynamic events with “snapshot” diffraction and imaging at 15-nanosecond resolution inside of a dynamic TEM. With the use of this capability, the moving reaction front of reactive nanolaminates is observed in situ. Time-resolved images and diffraction show a transient cellular morphology in a dynamically mixing, self-propagating reaction front, revealing brief phase separation during cooling, and thus provide insights into the mechanisms driving the self-propagating high-temperature synthesis.

Using the unique capabilities and high time resolution of dynamic transmission electron microscopy (DTEM), the fast kinetics of α → β-phase transformation in nanocrystalline Ti films were investigated using single-shot electron diffraction and bright-field TEM images. From quantitative analysis of the diffraction patterns, the transformation rates were determined for temperatures between transition start (1155 K) and melt temperature (1943 K). The experimental data were summarized in a time–temperature-transformation (TTT) curve with nanosecond time resolution. Theoretical TTT curves were calculated using analytical models for isothermal martensite and available thermodynamic data. Above 1300 K, there is excellent agreement between the experiment and the discrete–obstacle interaction model, suggesting that the nucleation rate and thermally assisted motion of the martensite interface are controlled by interface–solute atom interactions. However, theory predicts much slower transformation rates near the transition temperature than experiment. Experimental data fits using the Pati–Cohen model suggests that an increase in autocatalytic nucleation may partially account for the fast transformation rates at lower temperatures.

Although recent years have seen significant advances in the spatial resolution possible in the transmission electron microscope (TEM), the temporal resolution of most microscopes is limited to video rate at best. This lack of temporal resolution means that our understanding of dynamic processes in materials is extremely limited. High temporal resolution in the TEM can be achieved, however, by replacing the normal thermionic or field emission source with a photoemission source. In this case the temporal resolution is limited only by the ability to create a short pulse of photoexcited electrons in the source, and this can be as short as a few femtoseconds. The operation of the photo-emission source and the control of the subsequent pulse of electrons (containing as many as 5 x 10(7) electrons) create significant challenges for a standard microscope column that is designed to operate with a single electron in the column at any one time. In this paper, the generation and control of electron pulses in the TEM to obtain a temporal resolution10(-6)s will be described and the effect of the pulse duration and current density on the spatial resolution of the instrument will be examined. The potential of these levels of temporal and spatial resolution for the study of dynamic materials processes will also be discussed.

The transient events of the α–β martensitic transformation in nanocrystalline Ti films were explored via single-shot electron diffraction patterns with 1.5 ns temporal resolution. The diffraction patterns were acquired with a newly constructed dynamic transmission electron microscope (DTEM), which combines nanosecond pulsed laser systems and pump-probe techniques with a conventional TEM. With the DTEM, the transient events of fundamental material processes can be captured in the form of electron diffraction patterns or images with nanosecond temporal resolution. The transient phenomena of the martensitic transformations in nanocrystalline Ti is ideally suited for study in the DTEM, with their rapid nucleation, characteristic interface velocities ∼1 km/s, and significant irreversible microstructural changes. Free-standing 40-nm-thick Ti films were laser-heated at a rate of ∼1010 K/s to a temperature above the 1155 K transition point, then probed at various time intervals with a 1.5-ns-long, intense electron pulse. Diffraction patterns show an almost complete transition to the β phase within 500 ns. Post-mortem analysis (after the sample is allowed to cool) shows a reversion to the α phase coupled with substantial grain growth, lath formation, and texture modification. The cooled material also shows a complete lack of apparent dislocations, suggesting the possible importance of a “massive” short-range diffusion transformation mechanism.

Grain boundary character distributions and triple junction distributions have been determined for 70 experimental microstructures, comprising aluminum-, copper-, austenitic iron- and nickel-based alloys in a wide variety of processed states. In these FCC metals, the fraction of coincidence site lattice (CSL) boundaries ranges from about 12% (as for a random Mackenzie distribution) to values as high as 75%. Despite wide variations in composition, processing, and grain size, we find that the grain boundary character distribution and triple junction distributions of these materials have striking similarities, and can be described by just a few parameters. This universality arises due to the highly non-random laws that govern the assembly of the grain boundary network, and due to the kinematic limitation that CSL boundaries arise primarily through twinning.

The goal of grain boundary engineering is to increase the fraction of so-called special grain boundaries, while decreasing the contiguity of the remaining random boundaries which are susceptible to intergranular degradation such as cracking, cavitation, corrosion and rapid self-diffusion. In the present work, we describe a technique for the quantitative experimental study of grain boundary network topology, with an emphasis on the connectivity of special and random grain boundaries. Interconnected grain boundary networks, or “clusters”, of either entirely random or entirely special boundaries are extracted from electron backscatter diffraction data on a Ni-base alloy, and characterized according to their total normalized length (their “mass”), as well as their characteristic linear dimensions. The process of grain boundary engineering, involving cycles of straining and annealing, is found to substantially reduce the mass and size of random boundary clusters. Furthermore, quantitative assessment of the boundary network topology shows that the special grain boundary fraction is a poor predictor of network topology, but that the higher-order correlation derived from triple junction distributions can successfully describe the length scales of random boundary clusters.

Grain boundary engineering comprises processes by which the relative fractions of so-called special and random grain boundaries in microstructures are manipulated with the objective of improving materials properties such as corrosion, creep resistance, and weldability. One such process also referred to as sequential thermomechanical processing (TMP), consists of moderate strains followed by annealing at relatively high temperatures for short periods of time. These thermomechanical treatments on fcc metals and alloys with low to medium stacking fault energies result in microstructures with high fractions of Σ3n and other special boundaries, as defined by the coincidence site lattice (CSL) model. More importantly, the interconnected networks of random boundaries are significantly modified as a consequence of the processing. The modifications in the grain boundary network have been correlated with post-mortem electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) observations of the deformed and annealed states of the material. The evolution of the microstructure to a high fraction of Σ3n boundaries is correlated with the decomposition or dissociation of immobile boundaries during annealing. This is evidenced by TEM observations of the decomposition of relatively immobile boundaries into two components, one with very low energy and thus immobile, and the other a highly mobile boundary that migrates into neighboring areas of higher strain levels. The formation of low-energy grain boundaries through this mechanism and its effect on boundary network topology is discussed within the context of grain boundary engineering and linked to known microstructural evolution mechanisms.

The evolution of the deformed microstructure as a function of imposed plastic strain is of interest as it provides information on the material hardening characteristics and mechanism(s) by which cold work energy is stored. This has been extensively studied using transmission electron microscopy (TEM), where the high spatial and orientational resolution of the technique is used in advantage to study local phenomenon, such as dislocation core structures and interactions of dislocations. With the recent emergence of scanning electron microscope (SEM)-based automated electron backscatter diffraction (EBSD) techniques, it has now become possible to make mesoscale observations that are statistical in nature and complement the detailed TEM observations. Correlations of such observations will be demonstrated for the case of Ni-base alloys, which are typically non-cell forming solid solution alloys when deformed at ambient temperatures. For instance, planar slip is dominant at low-strain levels but evolves into a microstructure where distinct crystallographic dislocation-rich walls form as a function of strain and grain orientation. Observations recorded using both TEM and EBSD techniques are presented and analyzed for their implication on subsequent annealing characteristics.

Selective laser melting is a powder-based, additive-manufacturing process where a three-dimensional part is produced, layer by layer, by using a high-energy laser beam to fuse the metallic powder particles. A particular challenge in this process is the selection of appropriate process parameters that result in parts with desired properties. In this study, we describe an approach to selecting parameters for high-density (>99 %) parts using 316L stainless steel. Though there has been significant success in achieving near-full density for 316L parts, this work has been limited to laser powers 99 %, with the density reducing rapidly at high speeds due to insufficient melting, and less rapidly at low speeds due to the effect of voids created as the process enters keyhole mode.

Recently, there has been increased attention toward determination of the grain boundary character distribution (GBCD) and manipulation of the relative fractions of “special” and “random” boundaries in the microstructure through thermomechanical processing techniques in order to improve materials properties like corrosion, creep resistance, and weldability. Most of the “optimization” treatments reported in the literature have been performed on f.c.c. metals and alloys with medium to low stacking fault energies, and have resulted in microstructures with high fractions of Σ3, Σ9, and Σ27 boundaries, or Σ3n boundaries. Experiments to modify the GBCD of oxygen-free electronic Cu and Inconel 600 through sequential thermomechanical processing are presented and the efficacy of these processing routes is assessed in terms of microstructural descriptors like the random grain boundary network and the distribution of triple junctions. This analysis has shown that Σ3n reactions, which occur as a consequence of multiple twinning, not only improve the GBCD but are also critical for disrupting the connectivity of the random boundary network.

Reported here is a study of the pattern of lattice curvature near the interface of deformed high-purity aluminium (99.9999%) bicrystals of specified crystallographic character (large-angle random). Curvature data are obtained from electron back-scattering diffraction pattern observations using orientation imaging microscopy. The concept of geometrically necessary dislocations (GNDs) is used as the central tool in the description of the observations. The samples studied were channel-die compressed perpendicular to the interface to plastic strain levels of 0.1 and 0.3. At a strain level of 0.1 the primary observation is the development of a pile-up of GNDs (i.e. lattice curvature) near the interface. At the higher strain level of 0.3, however, a dramatic change in the distribution is observed. The nature of this change suggests that the interface has absorbed (or emitted) some components of the nearby GND field. with an accompanying change in the local character of the interface towards a broader d...

A finite element implementation is reported of the Fleck–Hutchinson phenomenological strain gradient theory. This theory fits within the Toupin–Mindlin framework and deals with first-order strain gradients and the associated work-conjugate higher-order stresses. In conventional displacement-based approaches, the interpolation of displacement requires C1-continuity in order to ensure convergence of the finite element procedure for higher-order theories. Mixed-type finite elements are developed herein for the Fleck–Hutchinson theory; these elements use standard C0-continuous shape functions and can achieve the same convergence as C1 elements. These C0 elements use displacements and displacement gradients as nodal degrees of freedom. Kinematic constraints between displacement gradients are enforced via the Lagrange multiplier method. The elements developed all pass a patch test. The resulting finite element scheme is used to solve some representative linear elastic boundary value problems and the comparative accuracy of various types of element is evaluated. Copyright © 1999 John Wiley & Sons, Ltd.

Analysis of Experimental Error in High Resolution Electron Micrographs

A method is described to prepare a high-resolution electron micrograph for quantitative comparison with a simulated high-resolution image. The experimental data are converted from the darkening of film used to acquire the image to units of electrons per incident electron, the same units used in the simulation. Also, distortions in the image arising from distortions in the image-forming lenses of the electron microscope are removed to improve the quality of the data. Finally, an alignment procedure is described which gives precise, pixel-by-pixel alignment of the experimental image with the simulated image. Examples of the procedure are shown to illustrate how actual data are prepared for quantitative analysis.

There is a need for predictive material “aging” models in the nuclear energy industry, where applications include life extension of existing reactors, the development of high burnup fuels, and dry cask storage of used nuclear fuel. These problems require extrapolating from the validation domain, where there is available experimental data, to the application domain, where there is little or no experimental data. The need for predictive material aging models will drive the need for associated assessments of the uncertainties in the predictions. Methods to quantify uncertainties in model predictions, using experimental data that is only distantly related to the application domain, are discussed in this paper.

The production of metal parts via laser powder bed fusion additive manufacturing is growing exponentially. However, the transition of this technology from production of prototypes to production of critical parts is hindered by a lack of confidence in the quality of the part. Confidence can be established via a fundamental understanding of the physics of the process. It is generally accepted that this understanding will be increasingly achieved through modeling and simulation. However, there are significant physics, computational, and materials challenges stemming from the broad range of length and time scales and temperature ranges associated with the process. In this paper, we review the current state of the art and describe the challenges that need to be met to achieve the desired fundamental understanding of the physics of the process.

New insight into the atomic segregation of copper to an aluminum grain boundary has been obtained using atomic resolution electron microscopy techniques coupled with ab-initio electronic structure calculations. We find the copper segregation to be site specific, changing the structure of the boundary by unexpectedly occupying interstitial sites. The calculated energy for segregation was found to be sufficient for essentially all of the interstitial sites to be filled. Minor elemental constituents in materials can have profound effects on their engineering performance, often through segregation to grain boundaries in the host material. One important example is the great resistance to electromigration damage in microelectronics imparted by small additions of copper to aluminum interconnects.

Classical plasticity theories generally assume that the stress at a point is a function of strain at that point only. However, when gradients in strain become significant, this localization assumption is no longer valid. These conventional models fail to display a ‘size effect’. This effect is seen experimentally when the scale of the phenomenon of interest is on the order of several microns. Under these conditions, strain gradients are of a significant magnitude as compared to the overall strain and must be considered for models to accurately capture observed phenomena.The mechanics community has been actively involved in the development of strain gradient theories for many years. Recently, interest in this area has been rekindled and several new approaches have appeared in the literature. Two different approaches are currently being evaluated. One approach considers strain gradients as internal variables that do not introduce work conjugate higher order stresses. Another approach considers the strain gradients as internal degrees of freedom that requires work conjugate higher order stresses. Experiments are being performed to determine which approach models material behavior accurately with the least amount of complexity. A key difference between the two models considered here is the nature of the assumed boundary conditions at material interfaces. Therefore, we are investigating the deformation behavior of aluminum/sapphire interfaces loaded under simple shear. Samples are fabricated using ultra-high vacuum diffusion bonding. To determine the lattice rotations near the boundary, we are examining the samples with both electron backscatter diffraction methods (EBSD) in the scanning electron microscope and with a variety of diffraction techniques in the transmission electron microscope. The experimentally found boundary conditions shall be subsequently used to determine whether the simpler internal variable model is adequately descriptive or if the greater complexity associated with the internal degree of freedom approach is warranted.

The dominant factor in determining the atomic structure of grain boundaries is the crystal structure of the material, e.g. FCC vs. BCC. However, for a given crystal structure, the structure of grain boundaries can be influenced by electronic effects, i.e. by the element comprising the crystal. Understanding and modeling the influence of electronic structure on defect structures is a key ingredient for successful atomistic simulations of materials with more complicated crystal structures than FCC. We have found that grain boundary structure is a critical test for interatomic potentials. To that end, we have fabricated the identical {Sigma}5 (3l0)/[001] symmetric tilt grain boundary in three different BCC metals (Nb, MO, and Ta) by diffusion bonding precisely oriented single crystals. The structure of these boundaries have been determined by high resolution transmission electron microscopy. The boundaries have been found to have different atomic structures. The structures of these boundaries have been modeled with atomistic simulations using interatomic potentials incorporating angularly dependent interactions, such as those developed within Model Generalized Pseudopotential Theory. The differing structures of these boundaries can be understood in terms of the strength of the angular dependence of the interatomic interaction. We report here the results for Ta.

We present a method for assessing the relative vulnerabilites of distinct classes of grain boundaries to localized corrosion. Orientation imaging microscopy provides a spatial map which identifies and classifies grain boundaries at a metal surface. Once the microstructure of a region of a sample surface has been characterized, a sample can be exposed to repeated cycles of exposure to a corrosive environment alternating with topographic measurement by an atomic force microscope in the same region in which the microstructure had been mapped. When this procedure is applied to Ni and Ni-based alloys, we observe enhanced attack at random grain boundaries relative to special boundaries and twins in a variety of environments.

There exists a growing body of literature that correlates the fraction of “special” boundaries in a microstructure, as described by the Coincident Site Lattice Model, to properties such as corrosion resistance, intergranular stress corrosion cracking, creep, etc. Several studies suggest that the grain boundary character distribution (GBCD), which is defined in terms of the relative fractions of “special” and “random” grain boundaries, can be manipulated through thermomechanical processing. This investigation evaluates the influence of specific thermomechanical processing methods on the resulting GBCD in FCC materials such as oxygenfree electronic (ofe) copper and Inconel 600. We also demonstrate that the primary effect of thermomechanical processing is to reduce or break the connectivity of the random grain boundary network. Samples of ofe Cu were subjected to a minimum of three different deformation paths to evaluate the influence of deformation path on the resulting GBCD. These include: rolling to 82% reduction in thickness, compression to 82% strain, repeated compression to 20% strain followed by annealing. In addition, the influence of annealing temperature was probed by applying, for each of the processes, three different annealing temperatures of 400, 560, and 800°C. The observations obtained from automated electron backscatter diffraction (EBSD) characterization of the microstructure are discussed in terms of deformation path, annealing temperature, and processing method. Results are compared to previous reports on strainannealed ofe Cu and sequential processed Inconel 600. These results demonstrate that among the processes considered, sequential processing is the most effective method to disrupt the random grain boundary network and improve the GBCD.

Extended abstract of a paper presented at Microscopy and Microanalysis 2008 in Albuquerque, New Mexico, USA, August 3 – August 7, 2008

High-purity tantalum single crystal cylinders oriented with [011] parallel to the cylinder axis were deformed 10, 20, and 30 percent in compression. The engineering stress-strain curve exhibited an up-turn at strains greater than ∼20% while the samples took on an ellipsoidal shape during testing, elongated along the [100] direction with almost no dimensional change along [011]. Two orthogonal planes were selected for characterization using Orientation Imaging Microscopy (OIM): one plane containing [100] and [011] (longitudinal) and the other in the plane containing [011] and [011] (transverse). OIM revealed patterns of alternating crystal rotations that develop as a function of strain and exhibit evolving length scales. The spacing and magnitude of these alternating misorientations increases in number density and decreases in spacing with increasing strain. Classical crystal plasticity calculations were performed to simulate the effects of compression deformation with and without the presence of friction. The calculated stressstrain response, local lattice reorientations, and specimen shape are compared with experiment.

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005