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At least 127 records · Page 7

Characterization of build parameters and microstructure in low heat input WAAM of Ni-based superalloy Haynes 282

Conference paper for 2024 10th International Conference on Advances in Materials, Manufacturing & Repair for Power Plants. Ni-based superalloy Haynes 282 is a prime candidate for advanced power generation systems due to its superior fabricability, weldability, and high-temperature performance. Additive manufacturing offers potential cost and time savings for gas turbine components. Wire-arc direct energy deposition can create large components but often requires post-processing treatments, such as hot isostatic pressing (HIP), to address porosity. This study explores a low heat-input, high deposition rate GMAW process to achieve fully dense Haynes 282 without HIP. Twenty-one blocks were deposited, varying travel and wire feed speeds. Initial analysis (visual inspection, microstructural examination, and CT) revealed the impact of build parameters on internal porosity and defects. Scanning electron microscopy provided insights into structural heterogeneity and microstructural properties. Related journal article can be found at https://doi.org/10.31399/asm.cp.am-epri-2024p0001.

Adam, Benjamin↗

Elucidating the corrosion mechanism of commercial Ni-based superalloys in UCl3 containing-chloride molten salt systems

Elucidating the role of UCl3 in the corrosion mechanism of Ni-based superalloys exposed to chloride molten salts Trishelle Copeland-Johnson1, Michael Woods1, Ruchi Gakhar1, Daniel J. Murray1, Guoping Cao1, Lingfeng He1 1Idaho National Laboratory, Idaho Falls, ID, United States The United States Department of Energy (DOE) aims to diversify the domestic energy portfolio towards more sustainable options, including implementation of molten salt reactor (MSR) technology. Chloride molten salts have been investigated as an appropriate MSR coolant and fuel because their relatively inexpensive, abundant, and exhibit favorable thermophysical properties. However, the corrosivity of chloride molten salts have not been extensively studied, especially with the inclusion of actinide products, such as UCl3. Accordingly, the development of nuclear structural materials with excellent corrosion performance is critical to the successful implementation of MSRs, particularly from a mechanistic perspective. In this investigation, we attempt to elucidate the interfacial corrosion mechanism between Ni-based structural materials, such as Inconel 617, and UCl3-containing salt systems through a multi-modal advanced characterization approach, including electron microscopy techniques. The findings from this investigation will expand the knowledgebase of chloride molten salt corrosion of MSR structural materials for strategic property-to-performance design.

36 - MATERIALS SCIENCE↗

Nickel-based superalloy single crystals fabricated via electron beam melting

Additive manufacturing technologies have emerged as potential disruptive processes whose possible impacts range from supply chain logistics, prototyping, and novel materials synthesis. Numerous works illustrate the ability to control mi- crostructure in fusion based processes and a few recent authors have even produced single crystals. However, a number of open questions remain regarding the process window which enables printing of single crystals. Furthermore, it has been observed that these additively manufactured single crystals exhibit a preferred $\langle$011$\rangle$ secondary orientation. In this work we investigate fabrication conditions which enable printing of single crystals via electron beam melting. A space filling design of experiments is utilized to efficiently explore the fabrication space. Single crystals were success- fully obtained using both commercially available powders and custom melt alloys. Microstructures obtained via these exploratory experiments exhibited a continuum of columnar structures ranging from weakly textured polycrystals, near single crystal, and fully single crystalline material. Complex geometry experiments are performed to study the grain selection mechanism. We find that the grain selection mechanism is independent of the bulk scale geometry and must therefore by driven by local heat transfer and solidification dynamics. Furthermore, grain selection is shown to be driven by competing driving forces; one which prefers epitaxial growth and another which is driven by the imposed scan pattern geometry. Finally, a mechanism is proposed for the anomalous secondary orientation preference.

36 MATERIALS SCIENCE↗

Long term oxidation of NiCoCrAlY coated Ni-based superalloys: A comparison of observed and simulated interdiffusion

Lifetimes of MCrAlY-type coatings can easily surpass 25 kh when the criteria of ß-depletion is used. To reduce experimental effort, it’s necessary to develop models capable of simulating interdiffusion and oxidation. In the present study, NiCoCrAlY coatings were high velocity oxyfuel deposited on PWA 1483, MARM247, and CMSX-4 substrates, and samples were exposed at 900 °C for 5–20 kh in air+10 vol%H 2 O to study interdiffusion rates. Here, Thermo-Calc/DICTRA was used to reproduce the observed differences, and microstructures were compared. Based on the agreement between calculated and observed rates, simulations were projected past the experimental exposures, utilizing ß-depletion as lifetime criteria.

36 MATERIALS SCIENCE↗

Modeling lattice rotation fields from discrete crystallographic slip bands in superalloys

Here in this work, we investigate the relationship between an intense slip band (ISB) and the zone of large lattice rotations that forms ahead of the tip of the ISB. We develop a crystal plasticity finite element model of a discrete ISB lying within an oligocrystalline assembly and calculate the local crystalline stress and lattice rotation fields generated by the ISB. The calculations demonstrate that, first, a region of severe lattice rotations, commonly referred to as a microvolume, does not form without the ISB, and second, large amounts of accumulated slip in the ISB are required to enlarge the microvolume to sizes and rotation magnitudes observed experimentally. Ahead of the ISB tip, the quintessential plastic zone always forms, but the atypical microvolume forms when non-concentrated and spatially diffuse slip is activated by the ISB-induced stress field. This result suggests that the detrimental ISB/microvolume pair will likely appear in pairs of crystals in which transmission of the slip from the ISB is severely blocked by the grain boundary, a hypothesis that we verify with a few target cases.

36 MATERIALS SCIENCE↗

Four-dimensional microstructurally small fatigue crack growth in cyclically loaded nickel superalloy specimen

Here, we nondestructively image a low-solvus high refractory (LSHR) nickel base specimen microstructure during cyclic loading to characterize crack propagation during the microstructurally small crack (MSC) growth regime. Micro-computed tomography (uCT) is used to characterize the material density and identify crack interfaces, while high-energy diffraction microscopy (HEDM) provides snapshots of the microstructural orientation field changes. From these measurements, data are computationally reconstructed and coregistered to describe the specimen’s configuration before load, before crack nucleation, and throughout the crack propagation/loading process. An MSC forms at a FIB-cut notch, which was previously placed to concentrate stress at the center of the specimen gauge, and propagates along a facet parallel to the local {1 1 1} crystallographic plane. Analysis of available crystallographic slip directions and measured point-to-point disorientation axes indicate probable single and coplanar slip activity along FCC octahedral planes within this region. Similar analyses of other crack propagation facets reveal generally slower growth along directions favoring zig-zag cross and codirectional cross slip, which are often disfavored at room temperature.

36 MATERIALS SCIENCE↗

Measurement of grain boundary strength of Inconel X-750 superalloy using in-situ micro-tensile testing techniques in FIB/SEM system

Grain boundaries (GBs), known as two-dimensional defects, are omnipresent in polycrystalline metallic alloys and thus influence a wide range of mechanical properties under different environmental conditions like irradiation and corrosion. Therefore, quantifying the strength of individual GBs is critical for understanding the degradation of mechanical properties of materials under different conditions. In this study we developed an efficient approach for the fabrication of micro-tensile specimens with a GB almost perpendicular to the tensile direction, which is expected to advance the development of individual GB tensile testing at micro or nanoscale in a wide scope of materials. Further, an in-situ cantilever micro-tensile testing method was developed and used to quantify the strength of a Σ3 GB in Inconel X-750 with the combination of finite element modeling. The average ultimate tensile strength (UTS) of a non-irradiated Σ3 GB is estimated at around 1.4 GPa, comparable to that of a neutron-irradiated Σ3 GB with a dose of ~1.5 dpa (1.3 GPa). Moreover, the in-situ push-to-pull micro-tensile testing technique developed in this work provides valuable insights into the high-angle GB deformation and fracture behavior. This method generates qualitatively similar ductility behavior before and after neutron irradiation as the bulk material testing. However, the ductility and UTS values obtained from this method are different from bulk measurements due to vastly different specimen dimensions.

36 MATERIALS SCIENCE↗

Influence of intermediate carbon content on the microstructure and high-temperature mechanical properties of cast and wrought Ni-based superalloy nimonic 105

NIMONIC® 105 variants with three different carbon concentrations were manufactured. Here, the medium carbon content variant shows inferior creep properties due to a bimodal grain size distribution and non-uniform carbides repartition leading to plastic strain accumulation between the two domains. Here, this eventually facilitated facile cracking and void formation during high-temperature creep.

36 MATERIALS SCIENCE↗

Geometry and size dependent microstructure and crack formation in Rene 41 superalloy fabricated by laser powder bed fusion

This study provides a systematic investigation into the size and geometry-dependent microstructural evolution and cracking susceptibility of LPBF-fabricated Rene 41. By coupling experimental microstructural analysis with thermal modeling, this research uniquely identifies the relationship between geometry-specific thermal histories, carbide coarsening, and liquation cracking. Four different geometries with varying thickness were fabricated with the identical process parameters. It was found that the grain size and morphology are not affected by the part size. However, the thinner parts exhibited coarser sub-grain structures compared to the thicker ones. The crack formation was observed for the parts with cross-sections smaller than 1 mm, whereas thicker parts had high density without any defects. Further, the cracks were observed in the interdendritic regions, suggesting that liquation cracking was the active micro-crack formation mechanism. The detailed microstructural analysis combined with a thermal finite element analysis proved that the heat extraction efficiency was lower for thinner parts causing a lower cooling rate and coarser carbides, making them more susceptible to constitutional liquation. Microhardness measurements were conducted for each geometry and correlated with the observed microstructural variations. The findings highlight the critical need for geometry-specific optimization of LPBF process parameters to mitigate cracking and achieve microstructural uniformity, offering valuable insights into the fabrication of complex, high-performance aerospace components.

36 MATERIALS SCIENCE↗

Elucidating the corrosion mechanism of commercial Ni-based Superalloys in UCl3 containing-chloride Molten Salt Systems

Molten salt reactors (MSRs) have gained renewed interest, providing several advantages over their predecessors, including the capability to consume spent fuels, enhancing the environmental sustainability of the uranium fuel cycle. For example, molten chloride fast reactors (MCFRs) can reach criticality with molten chloride spent fuel containing high concentrations of impurities, such as actinide products like uranium chloride (UCl3). However, the redox potential of chloride molten salt fuels may change in the presence of these impurities, dictating their corrosivity and in turn the corrosion performance of structural components, such as those constructed from nickel (Ni)-based alloys. The purpose of this investigation is to assess the extent of corrosion of Ni-based alloy, Inconel 617, when exposed to UCl3-LiCl-KCl eutectic salt. Inconel 617 one of only six structural materials that are fully qualified by the American Society for Mechanical Engineers (ASME) Boiler and Pressure Vessel Code for high-temperature nuclear reactor components, making it a technologically mature material to consider for constructing MCFRs. Inconel 617 specimens were submerged in a static LiCl-KCl-UCl3 eutectic salt mixture heated at 700 C for 1000 h under an inert atmosphere. Upon completion, the extent of corrosion was analyzed through a multi-modal characterization approach spanning the engineering to nanoscale, employing computed tomography, focused-ion beam, and transmission electron microscopy techniques. Results from this investigation will enhance our understanding of property-to-performance relationships of candidate structural materials for MSRs with respect to corrosion resistance and interactions between the salt and alloy interface.

36 MATERIALS SCIENCE↗

Ex-situ Heat Treatment of TEM Foils in a Custom Titanium Fixture: A Case Study on Ni-based Superalloy

The advancement of microstructural characterization at the nanoscale is critical to understanding the microstructural evolution and performance of engineering materials. Transmission electron microscopy (TEM) plays a vital role in such investigations, particularly when coupled with controlled ex- and in-situ experiments. In this study, we introduce a novel method for ex-situ heat treatment (HT) of TEM foils using a custom-designed fixture, made from pure titanium, and vacuum furnace to inhibit oxidation. This approach ensures precise temperature control and minimal sample contamination during HT, critical for substructural characterization and analysis of metallic materials. The fixture consists of a titanium base with three slits, for three sample foils, and a titanium cap for closure. The entire assembly is placed in a vacuum heat treatment furnace with high vacuum capability to prevent oxidation. To validate the effectiveness of the setup, precipitation behavior and microstructural changes were studied in an IN725 variant heat-treated at 500°C for 1 hour and 282 variant heat-treated at 700°C for 1 hour, as case studies.

electron microscopy↗

Inhomogeneous Distribution and Coarsening of y″ Precipitates in a Ni-Based Superalloy and Their Effect on Creep

It has been reported that the addition of Nb or Ta in the high Ti/Al ratio alloys promotes the formation of y″ precipitates solely and greatly contributes to the elevated temperature strength and resistance to creep deformation. In this study, the y''-dominant INCONEL alloy 725 (IN725) variants (named M725-Nb/Ta) modified with a high level of Nb/Ta additions and high Ti/Al ratio was chosen as a model alloy for microstructural observation of y'' variants upon creep. Following the high temperature aging (HTA), y'' was found to be the main strengthening precipitate with no detectable y’ in both M725 alloys. After creep, the grip/gage sections of the crept M725-Nb/Ta exhibited preferential coarsening and inhomogeneous distribution of y''. That is, one or two of the variants were preferentially coarsened at the expense of another variant, and sandwich-like structures, comprising of cubic y′ precipitates with small y″ discs on each face, were formed. This variant selection behavior taking place in the grip section with no stress applied was different from the typical stress-induced variant selection in previous literature. However, the sample with prior high temperature exposure (700 °C for 500 hours) with varying y″ characteristics demonstrated a similar trend of creep when compared with those in the HTA sample, suggesting that the coarsening and the inhomogeneous distribution of y'' was not the determinant of creep life in bulk M725-Nb/Ta alloys.

Hung, Chang-Yu↗

Microstructural Development in Inconel 718 Nickel-Based Superalloy Additively Manufactured by Laser Powder Bed Fusion

Excellent weldability and high temperature stability make Inconel 718 (IN718) one of the most popular alloys to be produced by additive manufacturing. Here in this study, we investigated the effects of laser powder bed fusion (LPBF) parameters on the microstructure and relative density of IN718. The samples were fabricated with independently varied laser power (125 - 350W), laser scan speed (200 - 2200 mm/s), and laser scan rotation (0° - 90°). Archimedes’ method, optical microscopy, and scanning electron microscopy were employed to assess the influence of LPBF parameters on the relative density and microstructure. Optimal processing windows were identified for a wide range of processing parameters and relative density greater than 99.5% was achieved using volumetric energy density between 50 and 100 J/mm3. Microstructural features including melt pool geometry, lack of fusion defect, keyhole porosity, and sub-grain cellular microstructure were examined and quantified to correlate to LPBF parameters. A simple empirical model was postulated to relate relative sample density and LPBF volumetric energy density. Melt pool dimensions were quantitatively measured and compared to estimations based on Rosenthal solution, which yielded a good agreement with the width, but underestimated the depth, particularly at high energy input, due to lack of consideration for keyhole mode. In addition, the sub-grain cellular-dendritic microstructure in the as-built samples was observed to decrease with increasing laser scan speed. Quantification of the sub-micron cellular-dendritic microstructure yielded estimated cooling rate in the order of 10 5 – 10 7 K/s.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The combined effects of hydrogen and aging condition on the deformation and fracture behavior of a precipitation-hardened nickel-base superalloy

The effect of hydrogen (H) on the deformation behavior of Monel K-500 in various isothermal heat treatment conditions (non-aged, under-aged, peak-aged, and over-aged) was assessed via uniaxial mechanical testing. H-charged and non-charged specimens were strained to failure to facilitate a comparison of ductility, fracture surface morphology, strength, and work hardening behavior. For all examined heat treatment conditions, H charging leads to a significant reduction in ductility, which is accompanied by a consistent change in fracture surface morphology from ductile microvoid coalescence to brittle intergranular fracture. While H charging led to a systematic enhancement in the yield strength of all heat treatments, the three age-hardened conditions exhibited a more than 2-fold increase relative to the non-aged heat treatment. This suggests that H modifies the dislocation–precipitate interactions, which also manifest themselves through changes in work hardening metrics related to the dislocation storage and recovery rates. In particular, the H-charged peak-aged specimen exhibited a significant increase in initial hardening (dislocation storage) rate relative to the H-charged under-aged specimen. Transmission electron microscopy of these samples revealed the onset of widespread dislocation looping in the H-charged peak-aged sample, in addition to the planar slip bands characteristic of the non-charged condition. This result suggests that hydrogen induces the particle shearing-to-looping transition at smaller particle sizes. Possible mechanistic explanations for this observed behavior are presented.

36 MATERIALS SCIENCE↗

Effect of laser melt schedule on the microstructure of additively manufactured IN718 Superalloy

Laser powder bed fusion (L-PBF) has enabled the fabrication of geometrically complex metallic structures and components that are challenging to producing using conventional manufacturing approaches. The site-specific and far from equilibrium thermal conditions of L-PBF offer the potential to facilitate multi-length scale design of structure and properties across the atomic-through macro-levels. However, L-PBF systems face scalability challenges due to throughput constraints. Laser rotary powder bed fusion (L-RPBF) systems are being investigated as a solution to enhance the deposition rates compared to conventional L-PBF. Rotary systems also offer additional flexibility for controlling the time structure of melting through laser interleaving on alternating layers. Here, in this study, IN718 test samples were printed using single-laser or interleaved dual-laser configuration in a L-RPBF system to investigates the effect of process settings and melt-interleaving on as-fabricated microstructure. The microstructural evolution, such as grain size and crystallographic texture, was assessed by determining variations in the melt-pool shapes. Laser interleaving leads to a reduction in average grain size compared to single laser by ∼ 40 % at high power (400 W) and by ∼36 % at medium power (370 W). Results presented here identify key challenge for obtaining uniform microstructures and barriers for the broader adoption of high-deposition rate L-RPBF.

Dual-laser↗