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DOE OSTI2022

Mitigating keyhole pore formation by nanoparticles during laser powder bed fusion additive manufacturing

Keyhole pore formation is one of the most detrimental subsurface defects in the laser metal additive manufacturing process. However, effective ways to mitigate keyhole pore formation beyond tuning laser processing conditions during keyhole mode laser melting are still lacking. Here we report a novel approach to mitigate keyhole pore formation during laser powder bed fusion (LPBF) process by using stable nanoparticles. The critical keyhole depth for keyhole pore generation (i.e., the largest keyhole depth without keyhole pore formation) during LPBF of Al6061 increases from 246 µm to 454 µm (85% increase) after adding TiC nanoparticles. In-depth x-ray imaging studies and thermo-fluid dynamics simulation enable us to identify that two mechanisms work together to mitigate keyhole pore generation: (1) adding nanoparticles prevents the keyhole from collapsing by increasing the liquid viscosity to impede the protrusion development; (2) adding nanoparticles slows down the keyhole pore movement by increasing the liquid viscosity, resulting in the recapturing of the pore by the keyhole. We further demonstrate that adding TiC nanoparticles can also eliminate the keyhole fluctuation induced keyhole pore during LPBF of Al6061. Our research provides a potential way to mitigate keyhole pore formation for defect lean metal additive manufacturing.

36 MATERIALS SCIENCE↗

DOE OSTI2022

DEFECT DETECTION USING DYNAMIC ANALYSIS FOR ADDITIVE MANUFACTURED METALS

Additive manufacturing (AM) has the ability to produce parts with complex geometries and internal features, however, for demanding applications such as the automotive and aerospace industries, it is crucial that the parts can meet the demanding functional and geometric requirements. Quality control for AM parts focuses on nondestructive methods of testing, but many of the current methods are expensive and time-consuming. The research presented in this report explores various methods of nondestructive evaluation (NDE) using dynamic analysis on stainless steel parts produced with selective laser melting (SLM). Methods include, but are not limited to, frequency response functions (FRF), impedance-based measurements, and scanning laser doppler vibrometry. Additionally, mode shape analysis was performed in MATLAB and FEA simulations were used for comparison with experimental results. The results indicate that dynamic analysis has the potential to be a feasible method of defect detection and NDE in AM parts and future work should focus on refining these methods, such as optimizing test parameters to improve sensitivity to defects.

Deonarain, Gita↗

DOE OSTI2025

Assessment of critical flaw sizes and crack driving forces during additive manufacturing of metallic materials

Additive manufacturing (AM) of complex engineering components is often plagued by a high susceptibility to cracking, particularly in high-strength metallic materials. While alloy design efforts have made progress in mitigating solidification defects, there remains a need for mechanistic guidelines to predict susceptibility to solid-state cracking. To address this gap, driving forces for the growth of melt pool cracks are calculated across a wide range of alloys using an efficient computational framework. Calculations are coupled with rapid single track laser experiments to elucidate trends in cracking from laser melting. The analyses conducted here highlight the important role of material properties in susceptibility to cracking, notably fracture toughness and elastic modulus. An important finding is that residual stresses that are limited in magnitude to the yield stress of the material are likely insufficient to drive cracking during cooling. Furthermore, the implications of these results are discussed in the context of alloy design for AM and residual stress accumulation during AM.

36 MATERIALS SCIENCE↗

DOE OSTI2025

A snapshot of high-entropy alloy processing techniques and their effects on resulting mechanical properties

High-entropy alloys (HEAs) exhibit exceptional strength, corrosion resistance, and thermal stability, making them promising candidates for nuclear, aerospace, and other extreme applications. While most prior work has focused on compositional design, manufacturing techniques themselves can alter microstructure and mechanical properties as dramatically as alloy chemistry. This review compiles and compares the effects of processing routes—including arc melting, induction melting, mechanical alloying with spark plasma sintering, and additive manufacturing—on the structure and properties of HEAs. Quantitative comparisons highlight, for example, that SPS-processed alloys can achieve ∼20–45 % higher yield and tensile strength than arc-melted counterparts, while Bridgman solidification produces nearly single-crystal structures with elongation to failure exceeding 80 %. Additive manufacturing routes such as selective laser melting offer fine microstructures but also introduce anisotropy and porosity, leading to yield strengths spanning 100–600 MPa for the same composition. By synthesizing such results, this review provides actionable insight into how processing routes interact with HEA core effects (high entropy, lattice distortion, sluggish diffusion, and cocktail effect) to determine performance, thereby offering a practical guide for optimizing manufacturing strategies.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Time-Resolved Geometric Feature Tracking Elucidates Laser-Induced Keyhole Dynamics

In this report, during laser melting of metals, localized metal evaporation resulting in the formation of a keyhole shaped cavity can occur if processing conditions are chosen with high power density. An unstable keyhole can have deleterious effects in certain applications (e.g., laser powder bed fusion) as it increases the likelihood of producing defects such as porosity. In this work, we propose a pipeline that enables complete segmentation and extraction of various geometric features in keyholing conditions. In situ synchrotron high-speed X-ray visualization at the Advanced Photon Source provides large datasets of experimental images with a high spatio-temporal resolution across a range of laser parameters for Ti-6Al- 4 V. Computer vision image processing techniques were used to extract time-resolved quantitative geometric features (e.g., depth, width, front wall angle) throughout keyhole evolution which were subsequently analyzed to understand the relationship between the variation of local keyhole geometry and processing conditions. This analysis is the first to employ a data-driven approach to further our understanding of the keyholing process regime.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Fabricating Graphene Oxide/h-BN Metal Insulator Semiconductor Diodes by Nanosecond Laser Irradiation

To employ graphene’s rapid conduction in 2D devices, a heterostructure with a broad bandgap dielectric that is free of traps is required. Within this paradigm, h-BN is a good candidate because of its graphene-like structure and ultrawide bandgap. We show how to make such a heterostructure by irradiating alternating layers of a-C and a-BN film with a nanosecond excimer laser, melting and zone-refining constituent layers in the process. With Raman spectroscopy and ToF-SIMS analyses, we demonstrate this localized zone-refining into phase-pure h-BN and rGO films with distinct Raman vibrational modes and SIMS profile flattening after laser irradiation. Furthermore, in comparing laser-irradiated rGO-Si MS and rGO/h-BN/Si MIS diodes, the MIS diodes exhibit an increased turn-on voltage (4.4 V) and low leakage current. The MIS diode I-V characteristics reveal direct tunneling conduction under low bias and Fowler-Nordheim tunneling in the high-voltage regime, turning the MIS diode ON with improved rectification and current flow. This study sheds light on the nonequilibrium approaches to engineering h-BN and graphene heterostructures for ultrathin field effect transistor device development.

2D materials↗

DOE OSTI2024

PRODUCTION OF GLASS-TO-METAL SEALS USING ADDITIVE MANUFACTURING TECHNIQUES

Glass-to-metal (GtM) seals are hermetic barriers between glass and metal components, often used in the electronic and vacuum industries. Creating the seals traditionally requires heating all the components to the glass melting temperature, where the glass will flow and bond to the metal. Due to the manufacturing constraints of the individual components and sealing conditions there are geometric and material restrictions. Additive manufacturing techniques were used to make GtM seals to reduce these restrictions. Hermetic, single pin seals were produced using printed metal shells, by selective laser melting (SLM), and digital light processing (DLP) printed glass preforms. Glass preforms were printed with photosensitive resin mixed with a silicate sealing glass powder in a 1:2 weight ratio. Thermal analysis, TGA/DSC, and screening experiments were used to determine an organic removal schedule. Video techniques determined a sintering schedule by producing a densification curve at different isothermal holds which were fit with a viscous sintering model. Single pin seals were also produced use a laser assisted manufacturing (LAM) process as an alternative to the conventional furnace sealing process. A Nd:YAG laser was focused on a solid glass preform, heating the glass to form the glass-metal bond. The sealing glass was doped with a transition metal oxide, Fe2O3 or CuO, to increase absorption of the laser wavelength. The interface of hermetic LAM seals were analyzed using electron microscopy, compared to conventional prepared seals, finding a reduction of interfacial morphologies.

Read, Aaron Reece↗

DOE OSTI2021

Crystal plasticity model of residual stress in additive manufacturing using the element elimination and reactivation method

Selective laser melting is receiving increasing interest as an additive manufacturing technique. Residual stresses induced by the large temperature gradients and inhomogeneous cooling process can favour the generation of cracks. In this work, a crystal plasticity finite element model is developed to simulate the formation of residual stresses and to understand the correlation between plastic deformation, grain orientation and residual stresses in the additive manufacturing process. The temperature profile and grain structure from thermal-fluid flow and grain growth simulations are implemented into the crystal plasticity model. An element elimination and reactivation method is proposed to model the melting and solidification and to reinitialize state variables, such as the plastic deformation, in the reactivated elements. The accuracy of this method is judged against previous method based on the stiffness degradation of liquid regions by comparing the plastic deformation as a function of time induced by thermal stresses. The method is used to investigate residual stresses parallel and perpendicular to the laser scan direction, and the correlation with the maximum Schmid factor of the grains along those directions. The magnitude of the residual stress can be predicted as a function of the depth, grain orientation and position with respect to the molten pool. The simulation results are directly comparable to X-ray diffraction experiments and stress–strain curves.

316 stainless steel↗

DOE OSTI2024

Selective laser sintering and spark plasma sintering of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide ceramics

Abstract Two advanced manufacturing processes, spark plasma sintering (SPS) and selective laser sintering (SLS), have been developed for synthesis of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide (CCC) via reactive sintering of a powder mixture of constitute monocarbides. X‐ray diffraction analysis confirmed that the single‐phase CCC can be formed by both SPS and SLS. While a homogenous microstructure with uniform metal element distributions was developed during SPS, three‐layer microstructures with a thin TiC‐rich layer and two TaC‐rich layers along with a TiO 2 ‐rich surface layer containing W nanoparticles were formed during SLS. In addition, cellular structures with W, Zr, and Ti element segregation and dislocations on cell boundaries were observed in the SLS‐CCC sample, indicating the effect of nonequilibrium conditions on microstructure formation during laser melting followed by rapid cooling and solidification process. Compared to the SPS‐CCC sample, the SLS‐CCC showed enhanced hardness and reduced thermal conductivity, which may be related to their unique cellular structures.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Phase Selection During Solidification and Solid-State Phase Transformations in an Al-10Ce-8Mn (wt pct) Alloy

In multicomponent Al-Ce alloys, and especially after additive manufacturing (AM), complex and metastable solidification microstructures are frequently observed. Here, in this research, the relationship between solidification conditions and phase selection are explored for an Al-10Ce-8Mn (wt pct) alloy using a systematic study of laser melting conditions. Three solidification modes were observed: primary Al 10 Mn 2 Ce; primary Al 20 Mn 2 Ce; and eutectic FCC Al + Al 20 Mn 2 Ce. These solidification modes were correlated to specific liquid-solid interface velocities using a simple thermal model, showing the change in primary solidification phase for low (< 6.8 × 10 −4 m/s), moderate (between 8.2 × 10 −4 and 5.9 × 10 −2 m/s) and high solidification velocities (> 6.2 x 10 −2 m/s) for the above three solidification microstructures, respectively. These results were rationalized by using interface response function (IRF) theory to describe the solidification undercooling for the possible primary intermetallic phases. The implication of the local phase selection from differing solidification conditions is summarized by a comparison of hardness which demonstrates the potential variance of Vickers hardness from 101 to 242 (VHV) by changing the laser velocity from 1 to 83 mm/s. Interestingly, on heat treatment at 400°C, the decomposition pathways of the solidification microstructure and hardness were also found to be different, thereby opening multiple pathways for spatial microstructure and property control within AM components.

Sisco, Kevin↗

DOE OSTI2021

A High-Throughput Method to Define Additive Manufacturing Process Parameters: Application to Haynes 282

This paper demonstrates how an analytical and experimental method can be used to rapidly define the 45 additive manufacturing settings for a new alloy where the process parameters were previously unknown. A nickel-based superalloy, Haynes 282, was chosen for the analysis. An experimental matrix of focused processing parameters was predicted with a dimensionless number and 100 samples were printed using the Selective Laser Melting technique. High-throughput measurements validated the predicted process conditions needed to achieve desired density and hardness. The whole process was completed in 16 hours. The new technique was confirmed with analytical processing maps adopted by the metal additive manufacturing community. With the predicted set of process parameters, microstructural characterizations and tensile testing were used to confirm the predictions. The resultant as-fabricated microstructures have refined length scales of both microsegregation and secondary phase distributions. As a result, the mechanical properties were comparable within the predicted processing window and exhibited high strength and high ductility.

Laser Material Processing↗

DOE OSTI2020

Influence of defect characteristics on tensile deformation of an additively manufactured stainless steel: Evolutions of texture and intergranular strain

The micromechanics of plastic deformation behavior of a selective laser melt processed austenitic stainless steel were studied by investigating the evolutions of texture and intergranular strain using in situ high-energy synchrotron x-ray diffraction (sXRD). The effects of defect characteristics on tensile behavior were studied using three different samples: a near full-density sample with elliptical closed voids and two samples with lack-of-fusion (LOF) defects tensile loaded either perpendicular or parallel to their major axes. The evolutions of pole figures and inverse pole figures show that the full-density specimen develops a strong (111)/(200) fiber texture along the loading direction. For both LOF specimens, the evolution of texture is qualitatively similar to the full-density counterpart, but the development of the fiber texture was much slower, indicating a limited plasticity at a given macroscopic strain. The intergranular strain evolution in the full-density specimen is similar to that of a wrought 316L stainless steel. Conversely, a significantly different intergranular strain development was observed in a LOF specimen, where tensile strain development was observed in both the axial and transverse directions. Finally, the influence of defect type, density, and orientation on the local stress states in the steel matrix and the evolutions of intergranular strains is discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Pulsed Laser Annealed Ga Hyperdoped Poly‐Si / SiO x Passivating Contacts for High‐Efficiency Monocrystalline Si Solar Cells

Polycrystalline Si ( poly ‐Si)‐based passivating contacts are promising candidates for high‐efficiency crystalline Si solar cells. We show that nanosecond‐scale pulsed laser melting (PLM) is an industrially viable technique to fabricate such contacts with precisely controlled dopant concentration profiles that exceed the solid solubility limit. We demonstrate that conventionally doped, hole‐selective poly ‐Si/SiO x contacts that provide poor surface passivation of c ‐Si can be replaced with Ga‐ or B‐doped contacts based on non‐equilibrium doping. We overcome the solid solubility limit for both dopants in poly ‐Si by rapid cooling and recrystallization over a timescale of ∼25 ns. We show an active Ga dopant concentration of ∼3 × 10 20 cm −3 in poly ‐Si which is six times higher than its solubility limit in c ‐Si, and a B dopant concentration as high as ∼10 21 cm −3 . We measure an implied open‐circuit voltage of 735 mV for Ga‐doped poly ‐Si/SiO x contacts on Czochralski Si with a low contact resistivity of 35.5 ± 2.4 mΩ cm 2 . Scanning spreading resistance microscopy and Kelvin probe force microscopy show large diffusion and drift current in the p ‐ n junction that contributes to the low contact resistivity. Our results suggest that PLM can be extended for hyperdoping of other semiconductors with low solubility atoms to enable high‐efficiency devices.

14 SOLAR ENERGY↗

DOE OSTI2024

Refining Microstructures in Additively Manufactured Al/Cu Gradients Through TiB 2 Inclusions

Here, the additive manufacture of compositionally graded Al/Cu parts by laser engineered net shaping (LENS) is demonstrated. The use of a blue light build laser enabled deposition on a Cu substrate. The thermal gradient and rapid solidification inherent to selective laser melting enabled mass transport of Cu up to 4 mm from a Cu substrate through a pure Al deposition, providing a means of producing gradients with finer step sizes than the printed layer thicknesses. Divorcing gradient continuity from layer or particle size makes LENS a potentially enabling technology for the manufacture of graded density impactors for ramp compression experiments. Printing graded structures with pure Al, however, was prevented by the growth of Al 2 Cu 3 dendrites and acicular grains amid a matrix of Al 2 Cu. A combination of adding TiB 2 grain refining powder and actively varying print layer composition suppressed the dendritic growth mode and produced an equiaxed microstructure in a compositionally graded part. Material phase was characterized for crystal structure and nanoindentation hardness to enable a discussion of phase evolution in the rapidly solidifying melt pool of a LENS print.

36 MATERIALS SCIENCE↗

DOE OSTI2022

On the Prediction of Uniaxial Tensile Behavior Beyond the Yield Point of Wrought and Additively Manufactured Ti-6Al-4V

In this paper, phenomenological relationships are presented that permit the prediction of the plastic regime of stress–strain curves using a limited number of parameters. These relationships were obtained from both conventional (wrought + β annealed) and additively manufactured (i.e., “3D printed”) Ti-6Al-4V. Three different methods of additive manufacturing have been exploited to produce the materials, including large-volume electron beam additive manufacturing, large-volume laser hot wire additive manufacturing, and small-volume selective laser melting. The general fundamental expressions are independent not only of the additive manufacturing process, but also of a wide variety of post-deposition heat treatments, however the coefficients are specific to material states. Thus, this work demonstrates that it is possible to predict not only the ultimate tensile strength, but also the full true stress, true strain curves, if certain parameters of the material are known. In general, the prediction of ultimate tensile strength are within 5% of the experimentally measured values across all additive manufacturing variants and subsequent heat treatments. The absolute values of ultimate tensile strength range from ~ 910 MPa to ~ 1170 MPa for the single alloy Ti-6Al-4V. Data representing 113 explicit samples are included in this work.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Origin of dislocation structures in an additively manufactured austenitic stainless steel 316L

In this experiment, the origin of dislocation structures in AM stainless steels was systematically investigated by controlling the effect of thermal stress through geometric constraints for the first time. Stainless steel 316L parts were produced in the form of “1D” rods, “2D” walls, and "3D" rectangular prisms to evaluate the effect of constraints to thermal expansion/shrinkage on the development of defect microstructures and to elucidate the origin of additively manufactured (AM) dislocation microstructures. Dislocation density, organization, chemical micro-segregation, precipitate structures, and misorientations were analyzed as a function of increasing constraints around solidifying material in 1D, 2D, and 3D components built using both directed energy deposition (DED) and powder-bed selective laser melting (SLM). In DED parts, the dislocation density was not dependent on local misorientations or micro-segregation patterns, but evolved from approximately ρ ⊥ = 10 12 m -2 in 1D parts to ρ ⊥ = 10 14 m -2 in 3D parts, indicating that it is primarily thermal distortions that produce AM dislocation structures. In DED 3D parts and SLM parts, dislocation densities were highest (ρ ⊥ ≈ 10 14 m -2 ) and corresponded to the formation of dislocation cells approximately 300-450 nm in diameter. Dislocation cells overlapped with dendrite micro-segregation in some but not all cases. The results illustrate that dendritic micro-segregation, precipitates, or local misorientations influence how the dislocations organize during processing, but are not responsible for producing the organized cell structures. Furthermore, this work shows that AM dislocation structures originate due to thermal distortions during printing, which are primarily dictated by constraints surrounding the melt pool and thermal cycling.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Massively parallel phase-field simulations targeting exascale

The interface thickness in the phase-field (PF) method limits its simulation scales. Consequently, large-scale PF simulations become prohibitively expensive for resolving the extremely fine microstructures that typically form during rapid solidification processing. This challenge is significant in predicting microstructure evolution in metal additive manufacturing and has been identified by the United States Department of Energy’s Exascale Computing Project. Here, to address this, we develop a multi-GPU and MPI-based massively parallel simulation code, utilizing state-of-the-art algorithms, software, and libraries, for large-scale three-dimensional (3D) PF simulations. We report the first GPU-parallel PF simulations on Frontier (currently the second TOP500 exascale cluster) and Summit machines, taking dendritic growth as an example problem. We evaluate the parallel performance of our implementation using scaling studies with more than 24 000 GPUs (among the largest known computations to date) and the acceleration performance using large-scale simulations of dendritic growth in 3D. Finally, massively parallel GPUs in these supercomputers enabled the first coupled multiscale simulations of laser melting and subsequent dendritic solidification on the scale of a full melt-pool, demonstrating the feasibility of performing PF simulations with a point total over 2 billion grid points within an acceptable time.

Exascale↗

DOE OSTI2021

Hydrogen embrittlement of additively manufactured austenitic stainless steel 316 L

Additive manufacturing (AM) is a promising means of production of austenitic stainless steel (SS) parts for hydrogen service. The hydrogen embrittlement resistance of SS 316 L parts manufactured by powder-bed-fed selective laser melting (SLM) and directed energy deposition (DED) was examined using slow strain rate tensile testing. The influence of the hierarchical AM microstructures on mechanical response, microstructural evolution, and void formation were analyzed using multiscale electron microscopy. Furthermore, the presence of hydrogen reduced ductility in as-built DED materials, but did not significantly influence the response in as-built SLM material or heat-treated materials. Microstructural features driving these different responses are discussed.

36 MATERIALS SCIENCE↗