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Additively manufactured (AM) components offer superior design flexibility compared to their conventionally manufactured counterparts and require process parameter optimization to achieve high-quality depositions with desirable and predictable mechanical properties. This study was focused on 4340 steel fabricated using laser powder bed fusion (LPBF), and 42 laser power and scan speed combinations have been systematically investigated to optimize the melt pool geometry and ensure fully dense parts. The AM material was compared with a wrought 4340 equivalent and studied in both as-fabricated and heat-treated conditions. Two heat treatments were designed and used to optimize the materials for strength and toughness, respectively. Microstructure, tensile, and fractographic studies were conducted to assess build integrity and establish processing–structure–performance relationships. Tensile properties of the AM materials in all studied conditions were equivalent or better than the comparable wrought materials. The high performance of the AM materials was attributed to the absence of both manganese sulfide inclusions and rolling-induced banding, typically found in the wrought materials. The fine cellular substructure is thought to additionally contribute to the high strength of the as-fabricated AM material. Complementary to the knowledge that has emerged from the experimental investigations, the dataset was further leveraged to make recommendations for future design of experiments to optimize AM build parameters in other material systems. A statistical Monte Carlo analysis was used to predict the interpolation error produced when using reduced datasets and to enable informed processing parameters selection. These findings are discussed to make recommendations for the use of AM materials for high-integrity structural applications.

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.

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 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.

Physics-based modeling of metal additive manufacturing (AM) processes is computationally challenging due to the very fine meshing required in both time and space. State-of-the-art numerical models that offer great insight into the process have been developed, but they require powerful computational resources and weeks of processing time. Thus, it is often more time-effective to fabricate multiple builds within the time it takes to complete one simulation prediction, further reinforcing the current trial-and-error approach to optimizing the build parameters. This study presents a simplified approach to the transient thermal modeling of the AM process. The numerical model is designed to run on a moderate laptop or desktop computer, without use of parallel processing. The method described in this study uses a unique approach to node creation which leverages the simplicity of the finite difference method to provide predictions in less time than it takes to build the part. Coarse meshing in both time and space along with simplifying assumptions about the solidification process are used in this numerical approach. Model predictions track well with experimental measurements. This approach is being developed for use in an industrial setting to inform deposition parameters based on a desired thermal profile.

A two-color pyrometer is aligned co-axially to the laser inside a Laser Engineered Net Shaping machine to gather thermal data during a single layer two-pass deposit. Several molten pool metrics are calculated from the pyrometer data, and anomalies in the data are used to flag potential defect locations. The depositions are scanned using x-ray Computed Tomography (XCT) with a 4.13 micron voxel, and void size and location are recorded. XCT void data is then compared to the thermal analysis to determine the efficacy of the anomaly detection technique. In this build, four voids > 40 microns in diameter were found with XCT. Three defects appeared in the interfacial region between the deposit and substrate and produced signatures that were detected by analyzing the in-situ pyrometer data.

Recent work in both 304L and 316L stainless steel produced by additive manufacturing (AM) has shown that in addition to the unique, characteristic microstructures formed during the process, a fine dispersion of sub-micron particles, with a chemistry different from either the powder feedstock or the expected final material, are evident in the final microstructure. Such fine-scale features can only be resolved using transmission electron microscopy (TEM) or similar techniques. The present work uses electron microscopy to study both the initial powder feedstock and microstructures in final AM parts. Special attention is paid to the chemistry and origin of these nanoscale particles in several different metal alloys, and their impact on the final build. Comparisons to traditional, wrought material will be made.

Accumulative roll bonded (ARB) Copper Niobium (Cu-Nb) nano-lamellar composite (NLC) panels were friction stir welded (FSWed) to evaluate the ability to join panels while retaining the nano-lamellar structure. During a single pass of the friction stir welding (FSW) process, the nano-lamellar structure of the parent material (PM) was retained but was observed to fragment into equiaxed grains during the second pass. FSW has been modeled as a severe deformation process in which the material is subjected to an instantaneous high shear strain rate followed by extreme shear strains. The loss of the nano-lamellar layers was attributed to the increased strain and longer time at temperature resulting from the second pass of the FSW process. Kinematic modeling was used to predict the global average shear strain and shear strain rates experienced by the ARB material during the FSW process. The results of this study indicate that through careful selection of FSW parameters, the nano-lamellar structure and its associated higher strength can be maintained using FSW to join ARB NLC panels.

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.

For additive manufacturing (AM) of metallic materials, the certification and qualification paradigm needs to evolve as there is currently no broadly accepted “ASTM- or DIN-type” additive manufacturing certification process or AM-produced material specifications. Accordingly, design, manufacture, and subsequent implementation and insertion of AM materials to meet engineering applications requires detailed quantification of the constitutive (strength and damage) properties of these evolving materials, across the spectrum of metallic AM methods, in comparison/contrast to conventionally-manufactured metals and alloys. For this study, cylindrical samples of 316L SS were produced using a LENS MR-7 laser additive manufacturing system from Optomec (Albuquerque, NM) equipped with a 1 kW Yb-fiber laser. The microstructure of the AM-316L SS was characterized in both the “as-built” AM state and following a heat-treatment designed to obtain full recrystallization to facilitate comparison with annealed wrought 316L SS. The constitutive behavior as a function of strain rate and temperature was characterized and is compared to that of annealed wrought 316L SS plate material. The dynamic shock-loading-induced damage evolution and failure response of all three 316L SS materials was quantified using flyer-plate impact driven spallation experiments at peak stresses of 4.7 and 6.5 GPa. The spall strength of AM-produced 316L SS and the recrystallized-AM-316L SS were found to decrease with increasing peak shock stress while the annealed wrought 316L SS spall strength remained essentially constant. The damage evolution, characterized using optical metallography and electron-backscatter diffraction (EBSD), was found to vary significantly across the three 316L SS microstructures while the three samples loaded to a peak shock stress of 6.5 GPa displayed only ∼12% differences in spall strength.

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.

This work presents the effects of input processing parameters and strut thickness (in square struts) on microstructure and properties in laser powder bed fusion additively manufactured stainless steel 316L lattice-emulating structures. Lattice-emulating X-structures with square cross-sections of 1.5, 1.0, and 0.5 mm were fabricated using three different parameter sets with varying power, speed, and therefore, linear energy density. Grain size and morphology were shown to be dictated by epitaxial growth, which was dependent on weld pool morphology. Additionally, grain size and morphology were shown to change across the thickness direction of the struts (from the bottom inclined surface to the top inclined surface). The spatial variation in grain size was reflected by changes in hardness through the thickness of each strut. The 0.5 mm struts exhibited more significant grain elongation in the strut direction and larger sub-grain solidification cell diameters than their thicker counterparts. The larger sub-grain solidification cell diameters in the 0.5 mm samples resulted in correspondingly lower hardness values when compared to samples of higher thicknesses.

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 ability of additive manufacturing to directly fabricate complex shapes provides characterization challenges for part qualification. The orientation of the microstructures produced by these processes will change relative to the surface normal of a complex part. In this work, the microscopy and x-ray tomography of an AlSi10Mg alloy hemispherical shell fabricated using powder bed metal additive manufacturing are used to illustrate some of these challenges. The shell was manufactured using an EOS M280 system in combination with EOS-specified powder and process parameters. The layer-by-layer process of building the shell with the powder bed additive manufacturing approach results in a position-dependent microstructure that continuously changes its orientation relative to the shell surface normal. X-ray tomography was utilized to examine the position-dependent size and distribution of porosity and surface roughness in the 98.6% dense part. Optical and electron microscopy were used to identify global and local position-dependent structures, grain morphologies, chemistry, and precipitate sizes and distributions. The rapid solidification processes within the fusion zone (FZ) after the laser transit results in a small dendrite size. Cell spacings taken from the structure in the middle of the FZ were used with published relationships to estimate a cooling rate of ~9 × 105 K/s. Uniformly-distributed, nanoscale Si precipitates were found within the primary α-Al grains. A thin, distinct boundary layer containing larger α-Al grains and extended regions of the nanocrystalline divorced eutectic material surrounds the FZ. Subtle differences in the composition between the latter layer and the interior of the FZ were noted with scanning transmission electron microscopy (STEM) spectral imaging.

International audience; It was recently shown that the crystals in an already nanocrystalline alloy (Pd-10% Au) became highly oriented under extreme shearing. No such self-ordering is seen in the coarse-grained counterpart under the same conditions. Here we use phase field dislocation dynamics and polycrystalline plasticity modeling to explore the possible causes that enabled this unusual crystallographic alignment. The results suggest that full-dislocation slip and preservation of grain boundary misorientation with at least one neighbor grain can cause the highly oriented texture observed experimentally.