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All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

A Bezier Curve Informed Melt Pool Geometry to Model Additive Manufacturing Microstructures Using SPPARKS

Additive manufacturing is a transformative technology with the potential to manufacture designs which traditional subtractive machining methods cannot. Additive manufacturing offers fast builds at near final desired geometry; however, material properties and variability from part to part remain a challenge for certification and qualification of metallic components. AM induced metallic microstructures are spatially heterogeneous and highly process dependent. Engineering properties such as strength and toughness are significantly affected by microstructure morphologies resulting from the manufacturing process Linking process parameters to microstructures and ultimately to the dynamic response of AM materials is critical to certifying and qualifying AM built parts and components and improving the performance of AM materials. The AM fabrication process is characterized by building parts layer by layer using a selective laser melt process guided by a computer. A laser selectively scans and melts metal according to a designated geometry. As the laser scans, metal melts, fuses, and solidifies forming the final geometry in a layerwise fashion. As the laser heat source moves away, the metal cools and solidifies forming metallic microstructures. This work describes a microstructure modeling application implemented in the SPPARKS kinetic Monte Carlo computational framework for simulating the resulting microstructures. The application uses Bzier curves and surfaces to model the melt pool surface and spatial temperature profile induced by moving the laser heat source; it simulates the melting and fusing of metal at the laser hot spot and microstructure formation and evolution when the laser moves away. The geometry of the melt pool is quite flexible and we explore effects of variances in model parameters on simulated microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Predictive multiphase evolution in Al-containing high-entropy alloys

The ability to predict and understand phases in high-entropy alloys (HEAs) is still being debated, and primarily true predictive capabilities derive from the known thermodynamics of materials. The present work demonstrates that prior work using high-throughput first-principles calculations may be further utilized to provide direct insight into the temperature- and composition-dependent phase evolution in HEAs, particularly Al-containing HEAs with a strengthening multiphase microstructure. Using a simple model with parameters derived from first-principles calculations, we reproduce the major features associated with Al-containing phases, demonstrating a generalizable approach for exploring potential phase evolution where little experimental data exists. Neutron scattering, in situ microscopy, and calorimetry measurements suggest that our high-throughput Monte Carlo technique captures both qualitative and quantitative features for both intermetallic phase formation and microstructure evolution at lower temperatures. This study provides a simple approach to guide HEA development, including ordered multi-phase HEAs, which may prove valuable for structural applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In situ measurement of damage evolution in shocked magnesium as a function of microstructure

Accurate modeling and prediction of damage induced by dynamic loading in materials have long proved to be a difficult task. Examination of postmortem recovered samples cannot capture the time-dependent evolution of void nucleation and growth, and attempts at analytical models are hindered by the necessity to make simplifying assumptions, because of the lack of high-resolution, in situ, time-resolved experimental data. We use absorption contrast imaging to directly image the time evolution of spall damage in metals at ~1.6-μm spatial resolution. We observe a dependence of void distribution and size on time and microstructure. The insights gained from these data can be used to validate and improve dynamic damage prediction models, which have the potential to lead to the design of superior damage-resistant materials.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Anomalous Annealing Response of Directed Energy Deposited Type 304L Austenitic Stainless Steel

Directed energy deposited (DED) and forged austenitic stainless steels possess dissimilar microstructures but can exhibit similar mechanical properties. In this study, annealing was used to evolve the microstructure of both conventional wrought and DED type 304L austenitic stainless steels, and significant differences were observed. In particular, the density of geometrically necessary dislocations and hardness were used to probe the evolution of the microstructure and properties. Forged type 304L exhibited the expected decrease in measured dislocation density and hardness as a function of annealing temperature. Here, the more complex microstructure–property relationship observed in the DED type 304L material is attributed to compositional heterogeneities in the solidification microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructurally driven self-sharpening mechanism in beaver incisor enamel facilitates their capacity to fell trees

Beavers ( Castor ) stand out among mammals for their unique capacity to fell trees using their large, ever-growing incisors. This routine consumption of resistant fodder induces prodigious wear in the lower incisors, despite this blunting effect the incisors maintain a remarkably sharp cutting edge. Notably, the enamel edges of their incisors show a highly complex two-part microstructure of which the biomechanical import is unknown. Here, using fracture analysis, nanoindentation, and wear testing on North American beaver ( C. canadensis ) incisors we test the microstructure's possible contribution to maintaining incisal sharpness. Although comparable in hardness, the inner enamel preferentially fails and readily wears at 2.5 times the rate of the outer enamel. The outer microstructure redirects all fractures in parallel, decreasing fracture coalescence. Conversely, the inner microstructure facilitates crack coalescence increasing the wear rate by isolating layers of enamel prisms that readily fragment. Together these two architectures form a microstructurally driven self-sharpening mechanism contained entirely within the thin enamel shell. Here, our results demonstrate that enamel microstructures exposed at the occlusal surface can markedly influence both enamel crest shape and surface texture in wearing dentitions. The methods introduced here open the door to exploring the biomechanical functionality and evolution of enamel microstructures throughout Mammalia.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Understanding Fission Gas Bubble Distribution and Zirconium Redistribution in Neutron-irradiated U-Zr Metallic Fuel Using Machine Learning

U-10wt.% Zr (U-10Zr) based metallic fuel is the leading candidate for next-generation sodium cooled fast reactor in United States. Currently, Idaho National Laboratory (INL) has been the leading national laboratory for research, development, and demonstration (RD&D) on metallic fuel. Advanced post-irradiation characterization will help to understand fuel microstructure and property change during irradiation, benefiting fuel qualification for commercial application. Characterization capabilities ranging from sub-nanometer to micrometer, such as scanning electron microscopy (SEM), focused ion beam (FIB) sampling, transmission electron microscopy (TEM) characterization, and local thermal conductivity microscopy (TCM), have been utilized recently on irradiated U-10Zr fuel samples to gain a better understanding of nuclear fuel microstructure and property evolution inside a reactor. The FIB/SEM coupled with energy dispersive X-ray spectroscopy (EDS) can capture the essential information to achieve better understanding of fuel behaviors. Inside a nuclear reactor, the phase and microstructure of U-10Zr is constantly changing under neutron bombardment. For example, the gaseous fission product atoms have a limited solubility inside fuel matrix and tend to precipitate out in bubble form, which not only contribute to fuel thermal conductivity degradation but also provide a shortcut for movement of fission products, i.e. lanthanides. The resultant deposition of lanthanides at the cladding inner surface will potentially trigger a chemical reaction/interaction between nuclear fuel and cladding at reactor operational conditions, threatening fuel integrity and safety. FIB/SEM coupled with EDS can provide the fission bubble information as well as probe into phase separation or Zr redistribution, which is fundamental to predict the fuel performance. With high velocity image data generating method, such as FIB/SEM, an automatic way to extract the microstructural information quantitively can better serve the needs from post irradiation characterization. A trained machine learning model, named Decision Tree, is employed to generate a bubble classifier and to categorize bubbles into three categories: isolated bubble, connected without lanthanides, and connected with lanthanides bubbles[3]. This work presents a showcase of this approach on six regions of a fuel cross-section along the radial temperature gradient. We obtained distributions of bubble categories and porosity rates along the six regions. Moreover, a secondary phase U-Zr2 was determined and found on regions 5 and 6. The secondary phase fraction was increasing from 15.61% in region 5 to 34.79% in region 6 based on this approach . This quantitative data offers insights into the lanthanide migration and potentially thermal conductivity degradation. This information from machine learning will be fed into fuel design code for better prediction of fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Genetic programming for interpretable, data-driven continuum damage models.

The damage mechanisms that lead to failure in engineering alloys have been studied extensively, but converting this knowledge into constitutive models that are suitable for engineering-scale analysis remains a challenge. Evolution laws for continuum damage have been developed in the past and have proven effective but suffer from many non-physical assumptions that inhibit the overall accuracy of the model. Further, the assumptions inherent in these existing models prevent them from being applicable to a broad class of materials. At the same time, computational models of fine-scale damage mechanisms continue to advance making it tractable to generate large training data sets through computer simulation. Data-driven machine learning approaches can leverage these data sets to avoid making limiting assumptions, and instead produce models directly from the results of microstructural simulations and/or experiments. Many of these machine learning approaches are rapid and accurate, but they offer little to no insight into the underlying relationships among state variables being discovered. Conversely, genetic programming symbolic regression (GPSR) is a machine learning method that produces analytic expressions relating the state variables, allowing maximal insight and interpretability. To that end, we propose using GPSR as a data-driven method of obtaining microstructurally informed continuum damage models. Data is generated using microstructural simulations of damage evolution, parameterized over microstructural statistics (i.e., pore shape) and nominally applied deformations. Analytic expressions for damage evolution are obtained from the data using GPSR, and these expressions are then utilized within a continuum constitutive model. Overall, this approach is a promising method of automatically obtaining analytic relations describing constitutive phenomena in a material.

Buche, Michael Robert↗
DOE OSTI2018

Precipitation behavior of ωo phase and texture evolution of a forged Ti-45Al-8.5Nb-(W, B, Y) alloy during creep

Highlights: • The morphology of ω{sub o} and residual β{sub o} phases depends on creep temperature and stress. • Stress can increase the tendency of the α{sub 2} to ω{sub o} phase transformation. • The strength of the texture components depend on temperature and stress. • β{sub o}(ω{sub o}) precipitation retards the growth of recrystallized γ grains. • ω{sub o} precipitation resists and deflects the crack during the crack propagation. - Abstract: Creep rupture tests of the as-forged Ti-45Al-8.5Nb-(W,B,Y) alloy with a duplex microstructure were carried out at 750–850 °C and 130–300 MPa. An investigation was performed to study the effects of temperature and stress on the microstructure and texture evolution, as well as on the creep properties of the forged high Nb-containing TiAl alloy with a duplex microstructure. The results show that the stress exponent n = 2.8–3.3, and the creep activation energy values are in the range of 300–400 kJ/mol. After creep, a regular arrangement of ω{sub o} precipitations was observed in the β{sub o} region. The un-transformed β{sub o} phase, which remained in the ω{sub o} interval, was examined using high resolution transmission electron microscope (HRTEM). It is shown that the growth of ω{sub o} precipitations and the morphology of residual β{sub o} phases are related to the creep temperature and stress. Certain β{sub o} stabilizer elements, such as Nb, segregate into α{sub 2} plates and cause ω{sub o} precipitation during dissolution of α{sub 2} plates at high temperature. The interfacial structure between the ω{sub o} and α{sub 2} phases was studied in detail using HRTEM. Meanwhile, texture evolution and dynamic recrystallization of the γ phase were studied using electron backscatter diffraction (EBSD). Observations on the deformation structure also demonstrate that ω{sub o} precipitation acts as an obstacle inhibiting crack propagation and growth of the γ phase. The corresponding formation mechanism and possible effects on creep are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Nanostructure formation during accumulative roll bonding of commercial purity titanium

In this investigation, commercial purity titanium (CP–Ti) was subjected to accumulative roll bonding (ARB) process up to 8 cycles (equivalent strain of 6.4) at the ambient temperature. Transmission electron microscopy (TEM) and X–ray diffraction line profile analysis (XRDLPA) were utilized to investigate the microstructure and grain size evolution. Both characterization techniques could clarify the non–uniform microstructure in the early stages and the uniform microstructure in the final stages of the process. The effectiveness of ARB for the fabrication of the nano–grained structure in CP–Ti was revealed. It was found that the SFE is not the only factor affecting grain refinement, as compared with other studies on ARB of FCC materials. Influence of other factors such as the melting temperature and the crystalline structure of the material was determined on the grain refinement. - Highlights: •Nano–grained commercial purity titanium was produced by accumulative roll bonding. •TEM and XRDLPA were used for the characterization of the microstructure. •Important factors affecting the grain size of ARBed materials were discussed.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Effect of undercooling on the microstructure of Ni-35 at. pct Mo (eutectic) and Ni-38 at. pct Mo (hypereutectic) alloys

Ni-35 at. pct Mo and Ni-38 at. pct Mo alloy specimens have been solidified from various levels of undercooling in the differential thermal analysis and the electromagnetic levitation units in a pyrex/vycor bed. The evolution of the microstructure in the solified specimens has been examined in terms of the degree of undercooling, the nature of the first phase to nucleate from the melt, and the specimen cooling rate. The melt has been observed to undercool more in the presence of intermetallic NiMo (beta) phase as compared to that in the presence of nickel-rich solid solution (gamma). The 'anomalous eutectic' type of microstructure has been shown to result from the initial formation of the dendritic skeleton of either of the two phases, its segmentation due to convection and ripening, and the subsequent nucleation of the other phase in the interdendritic liquid regions. The recalescence behavior has been examined as a function of undercooling and the nature of the phase nucleating first in the melt.

Tewari, S. N.↗
DOE OSTI2019

Microstructure and Mechanical Properties of Copper Billets Fabricated by the Repetitive Extrusion and Free Forging Process

In the present study, with the aim of obtaining a weakened texture, grain refinement and improved mechanical properties, copper billets were successfully fabricated using the severe plastic deformation method of repetitive extrusion and free forging (REFF) without using any additional tools or devices. The evolution of the microstructure, texture and mechanical behavior of the ultrafine grain copper billets over an increasing number of REEF cycles was also systematically studied. Our results show that the effective strain per REFF process was ε = 2.35. After two cycles of REFF process, the sum effective strain became ε = 4.7, leading to high efficiency of grain refinement. The grain size was refined from 50 to 0.8 μm; the yield strength was increased to 462 MPa, and we obtained a weakened texture in the pure copper billets. By increasing the number of cycles, the grain refinement ability was decreased, and the texture was thus strengthened further. Therefore, two cycles of REFF were a reasonable process for producing ultrafine-grained copper billets.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Crack Initiation Behavior of Cold-Worked Alloy 690 in Simulated PWR Primary Water - Role of Starting Microstructure, Applied Stress and Cold Work on Precursor Damage Evolution

Long-term stress corrosion crack (SCC) initiation behavior in Alloy 690 is being evaluated by constant load tensile testing in simulated pressurized water reactor primary water. Seven commercial Alloy 690 heats with different starting microstructures and cold-work levels are being tested at either 90% or 100% of the material yield stress. Previous studies have revealed grain boundary (GB) cavity formation after 7,110 to 9,220 hours of exposure in certain thermally treated (TT) Alloy 690 heats in highly cold-worked (CW) conditions, serving as precursors to intergranular cracks. This paper summarizes the new characterization results for the evolution of GB cavities in four Alloy 690TT heats in 21% and 31%CW conditions loaded at yield stress after 18,400 hours of exposure. Link-up of GB cavities has led to formation of long internal creep cracks, resulting in crack initiation detected by direct current potential drop in a highly CW Alloy 690TT heat with uniform, semi-continuous distribution of small GB carbides. In comparison, highly CW materials featuring larger and more widely spaced GB carbides did not show a significant increase in GB cavity density or size. Quantitative assessments were performed on GB cavity evolution in highly CW specimens for two Alloy 690TT heats demonstrating the strong dependence of GB cavity evolution on applied stress and starting GB microstructure.

Zhai, Ziqing↗
DOE OSTI2022

Friction stir welding and self-ion irradiation effects on microstructure and mechanical properties changes within oxide dispersion strengthened steel $\mathrm{MA956}$

We report the joining process for oxide dispersion strengthened (ODS) alloys remains a key challenge facing the nuclear community. The microstructure and mechanical properties were characterized in the base material and friction stir welded ODS MA956 irradiated with 5 MeV Fe 2+ ions from 400 to 500°C up to 25 dpa. Nanoindentation was performed to assess changes in hardness and yield stress, and the dispersed barrier hardening (DBH) model was applied to described results. A combination of scanning transmission electron microscopy (STEM) and atom probe tomography (APT) were used to assess evolution of the microstructure including dispersoids, network dislocations and dislocation loops, nanoclusters, and solid solution concentrations. Overall, softening was observed as a result of increased dose, which was exacerbated at 500°C. The formation and coarsening of new dispersoids was noted while nanoclusters tended to dissolve in the base material, and were not observed in the stir zone. Solute nanocluster evolution was identified as a primary driver of the changes in mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Scan strategies in EBM-printed IN718 and the physics of bulk 3D microstructure development

Three-dimensional (3D) characterization provides opportunities for understanding processing-structure relationships in additively manufactured (AM) materials. Bulk samples of Inconel 718 were fabricated via electron beam melting (EBM) in order to study microstructural development as a function of energy input and beam scan strategy. TriBeam tomography of bulk Inconel 718 microstructures built under steady-state growth conditions reveals the sensitivity of microstructure formation and evolution to machine process parameters. Here, samples manufactured using a narrow range of energy input per unit build area result in varied grain morphologies and crystallographic textures. Using TRUCHAS, a thermal simulation software, the thermal history of bulk scan strategies was predicted, and combined with a calibrated microstructure-processing map to accurately predict bulk grain morphologies. The solidification parameters and the 3D measured nucleation density are used to predict the transition between columnar and equiaxed grain morphologies, providing a process map to guide AM parameter choices to locally control as-printed microstructure. A two-dimensional metric for characterizing bulk grain morphology was also found to agree well with predictions from the process map calibrated by 3D data. Combined with 3D tomography and thermal modelling, the physics of structure development were understood at a new level of detail with respect to the competing processes of grain nucleation and epitaxial growth.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Viscous Shear Banding in Cutting of Metals

Shear banding is a type of plastic flow instability with often adverse implications for cutting and deformation processing of metals. Here, we study the mechanics of plastic flow evolution within single shear bands in Ti- and Ni-based alloy systems. The local shear band displacement profiles are quantitatively mapped at high resolution using a special micromarker technique. The results show that shear bands, once nucleated, evolve by a universal viscous sliding mechanism that is independent of microstructural details. The evolution of local deformation around the band is accurately captured by a momentum diffusion equation based on a Bingham-type flow rule. The predicted band viscosity is very small, compared to those of liquid metals. A plausible explanation for this small viscosity and fluid-like behavior at the band, based on phonon drag, is presented.

Engineering↗
DOE OSTI2016

Neutron irradiation effects on the corrosion of Zircaloy-4 in a pressurized water reactor environment - 2016-0085

Long-time Advanced Test Reactor (ATR) corrosion weight-gain data from non-fueled α-processed Zircaloy-4 cladding coupons are presented herein. The data were generated in pressurized loops that simulated pressurized water reactor (PWR) chemistry, temperature, and neutron flux conditions. High neutron flux and high-fluence post-transition corrosion rates were accelerated over out-of-flux post-transition corrosion rates by more than 40 times at 270 deg. C and more than 30 times at 310 deg. C We conclude in large part that the acceleration was caused by irradiation-induced changes to the base metal. The effect that irradiation has on the base metal and its effect on corrosion has been shown in the past to be carried over into post-irradiation tests in autoclave environments, but its impact was shown in this study to be accentuated in the in-reactor environment, in which sustained corrosion accelerations were much greater than observed in the postirradiation tests (in non-irradiation environments). This suggests some aspect of the radiation environment potentially acts synergistically with the corrosion film formed from the irradiation-damaged base metal to further accelerate in-reactor corrosion rates. We also present results from detailed microstructural examinations of thick (more than 25 μm) oxide films formed on α-processed Zircaloy-4 grown in a 360 deg. C autoclave and in the reactor. The examinations consisted of optical microscopy, field emission gun scanning electron microscopy, focused ion beam microscopy, analytical electron microscopy, and X-ray diffraction, with a focus on the evolution of the microstructure of the intermetallic precipitates in the oxide films during exposure to autoclave water or to the corroding environment under neutron irradiation. The film microstructure suggests that the water environment was closer to the oxide-metal interface in the films grown in the reactor than in the autoclave-grown corrosion films examined, but it was not obvious from the microstructural examinations how the radiation environment facilitated that effect. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2025

Bulk nanocrystalline Al–Mg–Y alloys with amorphous grain boundary complexions display high strength and compressive plasticity

Although nanocrystalline alloys regularly exhibit high strengths, their use in structural applications often face challenges due to sample size limitations, unstable microstructures, and the limited ability to plastically deform. The incorporation of amorphous grain boundary complexions has been proposed to address these issues, by simultaneously stabilizing nanocrystalline grain structures for scale-up processing and improving alloy toughness. In the present study, the mechanical behavior of bulk nanocrystalline Al–Mg–Y is examined with macroscale compression testing, probing a length scale that is relevant to real-world structural applications. Bulk samples were fabricated via a simple powder metallurgy approach, with different hot-pressing temperatures and durations employed for consolidation in order to investigate microstructural and property evolution. All of the specimens contained primary face-centered cubic Al and secondary Al 4 C 3 and Al 3 Y phases, with the Al 3 Y particles exhibiting two populations of small equiaxed and larger elongated particles. Appreciable plasticity was measured along with high ultimate stresses over 800 MPa due to the presence of amorphous grain boundary complexions. Microstructural characterization of fracture surfaces revealed that the area fraction of dimpled regions increased with longer hot-pressing time. Most importantly, the elongated Al 3 Y particles formed regular cellular patterns with increasing hot-pressing time, delaying shear localization and significantly enhancing plasticity. The hierarchy present in the microstructure of the Al–Mg–Y alloy, from amorphous grain boundary complexions to secondary phases, gives rise to excellent bulk mechanical properties, which are attractive for structural applications.

Bulk nanocrystalline alloy↗
DOE OSTI2016

Defect evolution in single crystalline tungsten following low temperature and low dose neutron irradiation

The tungsten plasma-facing components of fusion reactors will experience an extreme environment including high temperature, intense particle fluxes of gas atoms, high-energy neutron irradiation, and significant cyclic stress loading. Irradiation-induced defect accumulation resulting in severe thermo-mechanical property degradation is expected. For this reason, and because of the lack of relevant fusion neutron sources, the fundamentals of tungsten radiation damage must be understood through coordinated mixed-spectrum fission reactor irradiation experiments and modeling. In this study, high-purity (110) single-crystal tungsten was examined by positron annihilation spectroscopy and transmission electron microscopy following low-temperature (~90 °C) and low-dose (0.006 and 0.03 dpa) mixed-spectrum neutron irradiation and subsequent isochronal annealing at 400, 500, 650, 800, 1000, 1150, and 1300 °C. The results provide insights into microstructural and defect evolution, thus identifying the mechanisms of different annealing behavior. Following 1 h annealing, ex situ characterization of vacancy defects using positron lifetime spectroscopy and coincidence Doppler broadening was performed. The vacancy cluster size distributions indicated intense vacancy clustering at 400 °C with significant damage recovery around 1000 °C. Coincidence Doppler broadening measurements confirm the trend of the vacancy defect evolution, and the S–W plots indicate that only a single type of vacancy cluster is present. Furthermore, transmission electron microscopy observations at selected annealing conditions provide supplemental information on dislocation loop populations and visible void formation. This microstructural information is consistent with the measured irradiation-induced hardening at each annealing stage. This provides insight into tungsten hardening and embrittlement due to irradiation-induced matrix defects.

Hu, Xunxiang↗