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At least 127 records · Page 7

The microstructure effects on irradiation response of ferritic – martensitic steels

Microstructural optimization to achieve greater mechanical strength has been one of the focuses in ferritic–martensitic steels development. However, these optimized microstructures’ effects on the radiation response are not well known. In this work, two ferritic–martensitic steels (9Cr-NbMo and 9Cr-Ta) underwent neutron irradiation in the High Flux Isotope Reactor, and their room-temperature post-irradiation tensile properties and microstructure evolutions were investigated and compared. These two steels exhibit similar pre-irradiation tensile behavior, and their yield strengths are higher than that of other ferritic–martensitic steels by about 200–250 MPa. Microstructural characterization on pre-irradiated materials reveals a smaller grain size in 9Cr-Ta (2.8 ± 0.3 μm in 9Cr-Ta versus 4.3 ± 0.5 μm in 9Cr-NbMo) but higher dislocation density and precipitate density in 9Cr-NbMo. As is common for ferritic–martensitic steels at low irradiation temperatures (less than about 0.45T m ), irradiation-induced hardening at 400 °C was observed for both alloys. Irradiation at 490 °C causes the two alloys to exhibit different tensile behavior: 9Cr-Ta softens by 208 MPa in yield stress, whereas 9Cr-NbMo maintains strength. Additionally, microstructural characterizations were performed, including precipitate growth, dislocation, and defect formation. Using the barrier hardening model for microstructure–property correlation, the softening in irradiated 9Cr-Ta is primarily attributed to the significant dislocation recovery, while the strength lost from the slight dislocation recovery in 9Cr-NbMo was compensated by the additional strength from the irradiation-induced cavities. The microstructure effect (primarily precipitate, dislocation and boundary) on the radiation response is discussed herein.

36 MATERIALS SCIENCE↗

Harnessing structural stochasticity in the computational discovery and design of microstructures

This paper presents a deep generative model-based design methodology for tailoring the structural stochasticity of microstructures. Although numerous methods have been established for designing deterministic (periodic) or stochastic microstructures, a systematic design approach that allows the unified treatment of both deterministic and stochastic microstructure design domains has yet to be created. The proposed methodology resolves this issue by learning a unified feature space that embodies diverse structural patterns with continuously varying stochasticity levels. A highly diverse microstructure database is established to incorporate various types of deterministic and stochastic microstructure patterns. A property-aware deep generative model is proposed to learn a unified feature space of the structural characteristics, as well as the relationship between structure features and properties of interest. Autoencoder (AE), Variational Autoencoder (VAE), and Adversarial Autoencoder (AAE) are compared to understand their relative merits in the property-aware learning of the unified feature space. Microstructural designs with tailorable stochasticity and properties are obtained by searching the unified feature space. Multiple design cases are presented to demonstrate the capability of designing microstructures for structural stochasticity and properties. Furthermore, the proposed method is employed to create stochastically graded structures, which manipulate the mechanical behaviors by varying the local stochasticity of the structure.

36 MATERIALS SCIENCE↗

Clarifying the formation of equiaxed grains and microstructural refinement in the additive manufacturing of Ti-Cu

Controlling microstructural evolution in metallic additive manufacturing (AM) is difficult, especially in producing refined as-built grains instead of coarse, directional grains. Traditional solutions involve adding inoculants to AM feedstocks, but titanium (Ti) alloys cannot employ this approach without producing detrimental secondary phases. Ti-Cu (Ti-copper) alloys offer a solution through constitutional supercooling and/or solid state thermal cycling under AM conditions. This work analyzes a compositionally graded directed energy deposition (DED) Ti-Cu build, single-melt laser tracks, and dilatometric heat treatments to evaluate if, when, and by what mechanism(s) microstructural refinement occurs. Refinement by inoculation of unmelted powder particles was also considered. Constitutional supercooling produced no net microstructural refinement as any equiaxed dendrites which form are remelted with new deposition. This finding agreed with solidification modeling of powder bed fusion-laser beam (PBF-LB) and DED builds. Solid state thermal cycling refined microstructures only during ex-situ dilatometric heat treatments, suggesting build parameter optimization is needed to achieve refinement in-situ. Accidental heterogeneous nucleation on unmelted Ti powder, originating from the different thermophysical properties of Ti and Cu, provided the most significant microstructural refinement. This work systematically assesses the microstructural refinement mechanisms of Ti-Cu in AM builds and offers insights into microstructural control in eutectoid alloys.

36 MATERIALS SCIENCE↗

A novel physics-based and data-supported microstructure model for part-scale simulation of laser powder bed fusion of Ti-6Al-4V

The elasto-plastic material behavior, material strength and failure modes of metals fabricated by additive manufacturing technologies are significantly determined by the underlying process-specific microstructure evolution. In this work a novel physics-based and data-supported phenomenological microstructure model for Ti-6Al-4V is proposed that is suitable for the part-scale simulation of laser powder bed fusion processes. The model predicts spatially homogenized phase fractions of the most relevant microstructural species, namely the stable β-phase, the stable α s -phase as well as the metastable Martensite α m -phase, in a physically consistent manner. In particular, the modeled microstructure evolution, in form of diffusion-based and non-diffusional transformations, is a pure consequence of energy and mobility competitions among the different species, without the need for heuristic transformation criteria as often applied in existing models. The mathematically consistent formulation of the evolution equations in rate form renders the model suitable for the practically relevant scenario of temperature- or time-dependent diffusion coefficients, arbitrary temperature profiles, and multiple coexisting phases. Due to its physically motivated foundation, the proposed model requires only a minimal number of free parameters, which are determined in an inverse identification process considering a broad experimental data basis in form of time-temperature transformation diagrams. Subsequently, the predictive ability of the model is demonstrated by means of continuous cooling transformation diagrams, showing that experimentally observed characteristics such as critical cooling rates emerge naturally from the proposed microstructure model, instead of being enforced as heuristic transformation criteria. Eventually, the proposed model is exploited to predict the microstructure evolution for a realistic selective laser melting application scenario and for the cooling/quenching process of a Ti-6Al-4V cube of practically relevant size. Numerical results confirm experimental observations that Martensite is the dominating microstructure species in regimes of high cooling rates, e.g., due to highly localized heat sources or in near-surface domains, while a proper manipulation of the temperature field, e.g., by preheating the base-plate in selective laser melting, can suppress the formation of this metastable phase.

Inverse parameter identification↗

Machine-learning-based, online estimation of ceramic’s microstructure upon the laser spot brightness during laser sintering

The ceramic microstructure strongly influences its properties. During manufacturing, the online monitoring of microstructure is critical to ensure the desired material properties. So far, the microstructure on the relevant scale is usually characterized offline using scanning electron microscopy (SEM), which is time and cost-consuming. In this work, we demonstrate a cost-effective, machine learning (ML)-based approach to simulate the SEM micrographs in real-time from the laser spot brightness. We experimentally observed a strong correlation between the laser spot brightness and the corresponding microstructure at the exact locations. The brightness values obtained from thermal emission images and the corresponding SEM micrographs were used in the training datasets. The ML algorithm was a style-based conditional generative adversarial network (CGAN). After training, the ML model could generate high-fidelity microstructure images within 0.1 seconds based on in-situ captured brightness at the laser sintering spot. We used the average grain sizes as the metric to evaluate the accuracy of the ML-predicted micrographs. Here, the ML-predicted microstructures were in good agreement, with less than 5% in difference from the real SEM images. In conclusion, we demonstrate the cost-effective, online microstructure estimation during laser sintering with a simple setup (a camera, a regular computer, and the ML model).

08 HYDROGEN↗

Automated, high-accuracy classification of textured microstructures using a convolutional neural network

Crystallographic texture is an important descriptor of material properties but requires time-intensive electron backscatter diffraction (EBSD) for identifying grain orientations. While some metrics such as grain size or grain aspect ratio can distinguish textured microstructures from untextured microstructures after significant grain growth, such morphological differences are not always visually observable. This paper explores the use of deep learning to classify experimentally measured textured microstructures without knowledge of crystallographic orientation. A deep convolutional neural network is used to extract high-order morphological features from binary images to distinguish textured microstructures from untextured microstructures. The convolutional neural network results are compared with a statistical Kolmogorov–Smirnov tests with traditional morphological metrics for describing microstructures. Results show that the convolutional neural network achieves a significantly improved classification accuracy, particularly at early stages of grain growth, highlighting the capability of deep learning to identify the subtle morphological patterns resulting from texture. The results demonstrate the potential of a convolutional neural network as a tool for reliable and automated microstructure classification with minimal preprocessing.

36 MATERIALS SCIENCE↗

Transient Microstructure Evolutions and Local Properties of Dual-Phase 980 MPa Grade Steel Via Friction Stir Spot Processing

Friction stir processing is a novel solid-state process to modify microstructures and their properties by intense, localized plastic deformation. However, little research has been reported for microstructure evolutions of advanced high-strength steels during the process. The present work focuses on the study of transient microstructure changes and local mechanical properties for friction stir spot processed dual-phase (DP) 980 MPa grade steel (DP980) under different peak temperatures. A pinless silicon nitride ceramic tool was used to produce relatively simple material deformation and flow near the tool. Friction stir spot processed steel samples were characterized by optical and electron microscopies. Furthermore, Vickers microhardness and nano-indentation measurements were used to study local mechanical properties for correlation with microstructures. A swallow layer of refined grains (<0.6 µm) was obtained with a low peak temperature (under 400 °C), whereas higher peak temperatures (>Ac 1 ) led to a change in grain size with different microstructures (fine-grained DP or martensite). Electron back-scattered diffraction characterizations revealed a large deformation in the as-received microstructures (mixture of ferrite and tempered martensite) induced by friction stir spot processing, leading to recrystallization and grain refinement around the stirred zone. Also, nano-indentation measurements showed a higher hardness than the hardness of the as-received DP980. Friction stir processing with different process conditions effectively changed microstructures and local mechanical properties.

36 MATERIALS SCIENCE↗

Atom Probe Tomography for understanding microstructural and chemical changes in nuclear materials

Atom Probe Tomography (APT) is routinely employed to determine 3D microstructure and chemistry changes in structural materials used in reactor to understand irradiation effect. These findings help to correlate changes to mechanical and physical properties of nuclear materials which are subjected to extreme reactor conditions. With safety and economics of a reactor in mind, it is essential to be able to predict the changes in the fuel composition and microstructure as a function of burnup. Also, there is current need to develop advanced fuels with improved properties and performance which requires the experimental data on changes in microstructure, physical and chemical properties after irradiation for feedback process. A novel approach is presented to determine the local burnup in irradiated fuels using isotopic quantification obtained by Atom Probe Tomography (APT). Considering the volume of sample used (<100?µm3) for APT experiments using the lift-out process in a scanning electron microscope equipped with a Focused Ion Beam (FIB), the presented method determines the local burnup from a nuclear fuel, where a minimal amount of waste is produced. In this work, three samples were analyzed with different burnup conditions to quantify the isotopes of 235U, 236U, and 238U for burnup calculation in the irradiated metallic U–7Mo dispersion fuel. The calculated values were found in excellent agreement with MCNP calculations. With regard to structural materials, one of the primary factors limiting the utilization of fuel rods of Zr alloys is hydrogen pick up during oxidation. Past experimental studies have shown that the hydrogen pickup in Zirconium alloys is influenced by the alloy composition as well by irradiation temperature and neutron dose. Oftentimes, it is not feasible to carry out comprehensive studies on understanding the microstructural evolution in neutron irradiated materials since in reactor irradiation programs are extremely costly, lengthy and logistically complicated. The use of ion irradiation as a substitute has grown in recent years for several reasons including less radioactivity, faster irradiations and lower costs. In the framework of the MUZIC 3 project, samples of Zircaloy-4 have been proton and Zr2+ irradiated at the Michigan Ion Beam Lab (MIBL) facility with aim to create a microstructure that is similar to that observed after in-reactor service. The temperature of the environment is adjusted to compensate for the higher dose rate, as has been done previously. As a first step in this project the irradiated microstructures have been characterized using Transmission Electron Microscopy and Atom Probe Tomography to elucidate the microstructural changes, including precipitate amorphization and dissolution and the formation of dislocation loops. This presentation plans to highlight initial finding of this project.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

SOC Synthetic Microstructure Bank

QUICK START: Start with property_library.html (can be found by typing the filename into the query box) and use the interactive table to filter, sort, and select a microstructure with the desired properties. Search for the alphabetic code to obtain the corresponding dataset. Full description: This is a bank of 1,970 unique 3-phase electrode microstructure files. When you account for reassigning phase IDs (e.g. declare that 1=Ni and 2=pore, instead of 1=pore and 2=Ni), it actually represents 5,910 unique electrode microstructures, each of which could be considered to be either an air or a fuel electrode (e.g. declare that the phase IDs correspond to pore, Ni, and YSZ; or that they correspond to pore, LSCF, and GDC; or whatever electron-conductor and ion-conductor combination is being studied). The voxel size is 50 nm and each electrode file contains a 4x4 grid of (12.5 micron)^3 sub-volumes. If placed together in a grid, they comprise a 50x50x12.5 micron electrode (note that the interfaces between sub-volumes will be sharp; this can be mitigated via simulating annealing/relaxation). The sub-volumes can also be used individually for a reasonably sized 12.5 micron cubic region-of-interest. A user can simply consider the voxel size to be a different value to rescale the volumes (and all of their morphological features, including particle size) as desired. These microstructures were generated using DREAM3D. The general procedure is outlined in https://doi.org/10.1016/j.jpowsour.2018.03.025 The file names are an alphabetic code having to do with the input parameters used in DREAM3D when they were generated. Most users would be best served by starting with the file property_library.html or property_library_subvols.html (which lists properties for each individual subvolume). These files contain a catalogue of the actual, measured properties of every microstructure in the database. Any combination of property values can be filtered and sorted until a desired electrode is found, at which point the user can find the file corresponding to that alphabetic code. The properties in the catalogue include connected TPB density, and for each phase: phase fraction, average particle size, polydispersity of particle size, tortuosity, and connected pair-wise interfacial area. They also include what fraction of each property is connected through to the interfaces of the volume. If the desired combination of properties is not found at first, remember that the phase IDs can be re-assigned arbitrarily, e.g. swapping 1s and 2s. In fact, the database was generated with this in mind so as not to generate redundant microstructures. If the database does not contain the desired property combinations, try to search for the other possible permutations of those properties with re-assigned phase IDs. Please cite https://doi.org/10.1149/10301.0909ecst for use. Please contact the maintainer, William K. Epting, for additional information or assistance.

3D microstructure↗

The effect of microstructure on the dynamic shock response of 1045 steel

Herein, the effect of microstructure on the shock response of 1045 steel is investigated via plate impact experiments and postmortem characterization. Three unique microstructures are explored: ferrite-pearlite, martensite, and ferrite with spheroidal cementite (i.e. spheroidized). Two spall recovery experiments, at approximate peak pressures of 3.2 and 3.5 GPa, are conducted to assess the Hugoniot elastic limit (HEL), spall strength, and damage morphology of the various microstructures. The ferrite-pearlite and martensite microstructures exhibit continuous yielding at both quasi-static and dynamic rates, while the spheroidized condition displays discontinuous yielding. Discontinuous yielding of the spheroidized microstructure is attributed to a combined low initial dislocation density coupled with a low dislocation nucleation rate. The spall strength of ferrite-pearlite is consistently lower than the spheroidized microstructure, attributed to elongated cementite that is more susceptible to cracking than more spherical cementite precipitates. Despite a high density of boundaries, martensite exhibits the highest spall strength. A large percentage of the boundaries within the martensite microstructure are found to be low energy (i.e. Σ3 or low angle), and are thus less susceptible to spall damage. Overall, the high spall strength of martensite is likely linked to traditional strengthening mechanisms that limit dislocation motion.

36 MATERIALS SCIENCE↗

Schmid factor crack propagation and tracking crystallographic texture markers of microstructural condition in direct energy deposition additive manufacturing of Ti-6Al-4V

Metallic additive manufacturing (AM) provides a customizable and tailorable manufacturing process for new engineering designs and technologies. The greatest challenge currently facing metallic AM is maintaining control of microstructural evolution during solidification and any solid state phase transformations during the build process. Ti-6Al-4V has been extensively surveyed in this regard, with the potential solid state and solidification microstructures explored at length. In this study, we evaluate the applicability of previously determined crystallo- graphic markers of microstructural condition observed in electron beam melting powder bed fusion (PBF-EB) builds of Ti-6Al-4V in a directed energy deposition (DED) build process. The aim of this effort is to elucidate whether or not these specific crystallographic textures are useful tools for indicating microstructural conditions in AM variants beyond PBF-EB. Parent β-Ti grain size was determined to be directly related to α-Ti textures in the DED build process, and the solid state microstructural condition could be inferred from the intensity of specific α-Ti orientations. Qualitative trends on the as-solidified β-Ti grain size were also determined to be related to the presence of a fiber texture, and proposed as a marker for as-solidified grain size in any cubic metal melted by AM. Analysis of the DED Ti-6Al-4V build also demonstrated a near complete fracture of the build volume, suspected to originate from accumulated thermal stresses in the solid state. Crack propagation was found to only appreciably occur in regions of slow cooling with large α +β colonies. Schmid factors for the basal and prismatic α-Ti systems explained the observed crack pathway, including slower bifurcation in colonies with lower Schmid factors of both slip systems. Colony morphologies and localized equiaxed β-Ti solidification were also found to originate from build pauses during production and uneven heating of the build edges during deposition. Tailoring of DED Ti-6Al-4V microstructures with the insight gained here is proposed, along with cautionary insight on preventing unplanned build pauses to maintain an informed and controlled thermal environment for microstructural control.

36 MATERIALS SCIENCE↗

Deep Neural Network Algorithm for CMC Microstructure Characterization and Variability Quantification

Microstructure characterization and variability quantification are crucial for understanding ceramic matrix composites (CMCs) mechanical behavior and deformation mechanisms across length scales. Traditionally, analyses of the micrographs obtained from microscopy are labor-intensive. However, with the vast improvement in computer vision (CV) and deep learning (DL), an automated algorithm can be designed to extract essential microstructure variability from micrographs which can then be used to construct a statistically representative volume element (SRVE). The DL-based algorithm spans the taxonomy of microstructure analyses, including semantic segmentation of microstructure constituents, secondary phases, matrix/fiber interface, and defects, and quantifying the microstructure variability in terms of probability distributions. In this work, C/SiNC and SiC/SiNC CMCs microstructures are semantically segmented through a deep convolutional neural network, followed by variability quantification through the implementation of a fully connected regression layer, hence forming a deep regression network. The deep regression network operates in a feedforward regime, in which the neuron output signal traverses through the network in a unidirectional manner. The weight tensor associated with each layer is updated through a backpropagation stochastic gradient descent approach. The input gray-scale image obtained through in-house scanning electron microscope and confocal microscope micrographs is augmented through affine transformations to increase the training set size, which is then processed through four strided convolutional layers. This compresses the image resolution by half at each layer while increasing the image depth by applying different filters (image encoding). The class activation maps (CAMs) corresponding to the applied filters highlight the key architectural features and assist with the semantic segmentation of the microstructure.

Hamza, Mohamed H.↗

Carbide Particle Redistribution in U-10Mo Alloy during Hot and Cold Rolling Processes: Synthetic Microstructure-Based Finite-Element Approach

The influence of initial carbide particle distribution features on particle fracture and the evolution of stringer distribution within an alloy of uranium with 10 weight percent molybdenum during cold rolling was investigated in this study. This work will provide guidance to casting optimization work and identify actionable process changes to eliminate the surface features directly attributed to carbides. In a previous study, various synthetic microstructure-based finite-element (FE) models were generated with consideration of different parameters (i.e., particle shape, particle volume fraction, and particle distribution), and used to examine the effects of hot rolling on the microstructure evolution. In this study, microstructures after ~80% hot rolling were used as the initial microstructures for the subsequent cold rolling simulation. Plane-strain compression loading was employed in the FE models to simulate cold rolling with reductions from ~80% to ~94%. Stringer analyses with the consideration of particle fracture were then performed with the simulated cold rolling results. The results of void evolution analyses show that microstructures with elliptical particles incorporate a much larger (almost double) void volume fraction than those with circular particles, indicating that the elliptical particles are fractured more easily than the circular ones. The results from the fracture mode analyses show that, under the adopted simple compression loading assumption, almost all the particles (i.e., >99%) were fractured by tensile separation. The results of stringer analyses show that, during cold rolling, the stringer volume fractions increase substantially due to the particle fracture, especially for the microstructures with the elliptical particles, and that the stringer volume fractions from stringers comprising many particles tend to increase faster. The maximum stringer lengths for the microstructures with circular particles tend to remain constant or decrease during cold rolling, whereas those for elliptical particles tend to slightly increase after a slight decrease. The number of particles at the surface increases very rapidly due to particle fracture during cold rolling.

36 MATERIALS SCIENCE↗

Update on Activities Related to the Library of Graphite Microstructures

This report provides an overview and update of the ongoing efforts to create a comprehensive library of microstructures for nuclear graphite and carbon-based materials under consideration for nuclear applications. The library includes data on microstructural characterization of unirradiated graphite materials, a guide to the techniques used to analyze graphite (which complements the ASME guidelines and ASTM standards), a summary of characterization data for neutron-irradiated or oxidized material, and a compendium of microstructural information for carbon-based materials. These efforts are being conducted at various length scales for the filler and binder phases in graphite to better understand graphite’s local structure and property relationships. This report is a follow-up to the previous milestone report titled Report on initial development of a database of nuclear graphite characteristics based on microstructural characterization, ORNL/TM/-2023/2992, published in July 2023.The effort to develop the library of microstructures supports the US Department of Energy Office of Advanced Reactor Technologies program objectives of aiding the material selection, licensing, management, and core assessments of a graphite core by documenting the unirradiated microstructure of relevant grades or characterizing the microstructure’s evolution under the reactor environment. Additionally, this project aims to provide (1) information and guidelines for the characterizing of graphite and (2) a protocol to assess a nuclear graphite grade.

36 MATERIALS SCIENCE↗

Role of Dynamic Nucleation at Moving Boundaries in Phase and Microstructure Selection

Solidification microstructures that form under steady-state growth conditions (cells, dendrites, regular eutectics, etc.) are reasonably well understood in comparison to other, more complex microstructures, which form under intrinsically non-steady-state growth conditions due to the competition between the nucleation and growth of several phases. Some important practical examples in this latter class include microstructures forming in peritectic systems in highly undercooled droplets, and in strip cast stainless steels. Prediction of phase and microstructure selection in these systems has been traditionally based on (1) heterogeneous nucleation on a static interface, and (2) comparing the relative growth rate of different phase/microstructures under steady-state growth conditions. The formation of new phases, however, occurs via nucleation on, or ahead of, a moving boundary. In addition, the actual selection process is controlled by a complex interaction between the nucleation process and the growth competition between the nuclei and the pre-existing phase under non-steady-state conditions. As a result, it is often difficult to predict which microstructure will form and which phases will be selected under prescribed processing conditions. This research addresses this critical role of nucleation at moving boundaries in the selection of phases and solidification microstructures through quantitative experiments and numerical modeling in peritectic systems. In order to create a well characterized system in which to study this problem, we focus on the directional solidification of hypo- and hyper-peritectic alloys in the two-phase region, imposing a large enough ratio of temperature gradient/growth rate (G/V(sub p)) to suppress the morphological instability of both the parent (alpha) and peritectic (Beta) phases, i.e. each phase alone would grow as a planar front. Our combined experimental and theoretical results show that, already in this simplified case, the growth competition of these two phases leads to a rich variety of microstructures that depend sensitively upon the relative importance of nucleation, diffusion, and convection.

Karma, Alain↗

Microstructure, Mechanical Properties, Hot-Die Forming, and Joining of 47XD Gamma TiAl Rolled Sheets

The microstructure and mechanical properties, along with the hot-die forming and joining of Ti-47Al-2Nb-2Mn-0.8 vol% TiB, sheets (known as 47XD), produced by a low-cost rolling process, were evaluated. A near-gamma microstructure was obtained in the as-rolled condition. The microstructures of heat-treated sheets ranged from a recrystallized equiaxed near-gamma microstructure at 1,200 to 1,310 C, to a duplex microstructure at 1,350 C, to a fully lamellar microstructure at 1,376 C. Tensile behavior was determined for unidirectionally rolled and cross-rolled sheets for room temperature (RT) to 816 C. Yield stress decreased gradually with increasing deformation temperature up to 704 C; above 704 C, it declined rapidly. Ultimate tensile strength exhibited a gradual decrease up to 537 C before peaking at 704 C, followed by a rapid decline at 816 C. The modulus showed a gradual decrease with temperature, reaching approximately 72% of the RT value at 816 C. Strain to failure increased slowly from RT to 537 C; between 537 C and 704 C it exhibited a phenomenal increase, suggesting that the ductile-brittle transition temperature was below 704 C. Fracture mode changed from transgranular fracture at low temperature, to a mixture of transgranular and intergranular fracture at intermediate temperature, to ductile fracture at 816 C, coupled with dynamic recrystallization at large strains. Creep rupture response was evaluated between 649 and 816 C over the stress range of 69 to 276 MPa. Deformation parameters for steady-state creep rate and time-to-rupture were similar: activation energies of approximately 350 kJ/mol and stress exponents of approximately 4.5. Hot-die forming of sheets into corrugations was done at elevated temperatures in vacuum. The process parameters to join sheets by diffusion bonding and brazing with TiCuNi 70 filler alloy were optimized for test coupons and successfully used to fabricate large truss-core and honeycomb structures. Nondestructive evaluation methods, e.g., ultrasonic C-scans and thermography along with metallography, were used to characterize bond quality. Microstructural evaluation during heat treatment, identification of phases at the braze/matrix interface, determination of shear strengths of brazed joints, and deformation mechanisms during tensile and creep processes will be discussed.

Das, G.↗

Dual Microstructure Heat Treatment of a Nickel-Base Disk Alloy Assessed

Gas turbine engines for future subsonic aircraft will require nickel-base disk alloys that can be used at temperatures in excess of 1300 F. Smaller turbine engines, with higher rotational speeds, also require disk alloys with high strength. To address these challenges, NASA funded a series of disk programs in the 1990's. Under these initiatives, Honeywell and Allison focused their attention on Alloy 10, a high-strength, nickel-base disk alloy developed by Honeywell for application in the small turbine engines used in regional jet aircraft. Since tensile, creep, and fatigue properties are strongly influenced by alloy grain size, the effect of heat treatment on grain size and the attendant properties were studied in detail. It was observed that a fine grain microstructure offered the best tensile and fatigue properties, whereas a coarse grain microstructure offered the best creep resistance at high temperatures. Therefore, a disk with a dual microstructure, consisting of a fine-grained bore and a coarse-grained rim, should have a high potential for optimal performance. Under NASA's Ultra-Safe Propulsion Project and Ultra-Efficient Engine Technology (UEET) Program, a disk program was initiated at the NASA Glenn Research Center to assess the feasibility of using Alloy 10 to produce a dual-microstructure disk. The objectives of this program were twofold. First, existing dual-microstructure heat treatment (DMHT) technology would be applied and refined as necessary for Alloy 10 to yield the desired grain structure in full-scale forgings appropriate for use in regional gas turbine engines. Second, key mechanical properties from the bore and rim of a DMHT Alloy 10 disk would be measured and compared with conventional heat treatments to assess the benefits of DMHT technology. At Wyman Gordon and Honeywell, an active-cooling DMHT process was used to convert four full-scale Alloy 10 disks to a dual-grain microstructure. The resulting microstructures are illustrated in the photomicrographs. The fine grain size in the bore can be contrasted with the coarse grain size in the rim. Testing (at NASA Glenn) of coupons machined from these disks showed that the DMHT approach did indeed produce a high-strength, fatigue resistant bore and a creep-resistant rim. This combination of properties was previously unobtainable using conventional heat treatments, which produced disks with a uniform grain size. Future plans are in place to spin test a DMHT disk under the Ultra Safe Propulsion Project to assess the viability of this technology at the component level. This testing will include measurements of disk growth at a high temperature as well as the determination of burst speed at an intermediate temperature.

Gayda, John↗

Microstructure Modeling of Third Generation Disk Alloys

The objective of this program was to model, validate, and predict the precipitation microstructure evolution, using PrecipiCalc (QuesTek Innovations LLC) software, for 3rd generation Ni-based gas turbine disc superalloys during processing and service, with a set of logical and consistent experiments and characterizations. Furthermore, within this program, the originally research-oriented microstructure simulation tool was to be further improved and implemented to be a useful and user-friendly engineering tool. In this report, the key accomplishments achieved during the third year (2009) of the program are summarized. The activities of this year included: Further development of multistep precipitation simulation framework for gamma prime microstructure evolution during heat treatment; Calibration and validation of gamma prime microstructure modeling with supersolvus heat treated LSHR; Modeling of the microstructure evolution of the minor phases, particularly carbides, during isothermal aging, representing the long term microstructure stability during thermal exposure; and the implementation of software tools. During the research and development efforts to extend the precipitation microstructure modeling and prediction capability in this 3-year program, we identified a hurdle, related to slow gamma prime coarsening rate, with no satisfactory scientific explanation currently available. It is desirable to raise this issue to the Ni-based superalloys research community, with hope that in future there will be a mechanistic understanding and physics-based treatment to overcome the hurdle. In the mean time, an empirical correction factor was developed in this modeling effort to capture the experimental observations.

Jou, Herng-Jeng↗